<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 9th June 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies, Shimadzu </strong>and <strong>Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies: Analysis of Oligonucleotides Using Ion-Pairing Alternatives on the Agilent Pro iQ Plus</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/an_oligonucleotide_analysis_pro_iq_plus_5994_8337en_agilent_87863ea5c1.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Oligonucleotides are an emerging therapeutic modality that target and modulate gene expression through the silencing or degradation of mRNA. Once an mRNA target is identified, the antisense sequence must be optimized with strategically incorporated chemical modifications to improve pharmacokinetics<sup>1</sup> , affinity, and minimize off-targeting or mismatching.<sup>2</sup>&nbsp;</p><p>Ion-pair reversed-phase LC/MS is commonly used to confirm the molecular weights of target oligo sequences to ensure proper synthesis. However, using alkylamines as ion-pairing agents often requires dedicated instrumentation. Furthermore, toxic and cost-prohibitive perfluorinated alcohols such as HFIP (hexafluoroisopropanol) are required for optimal chromatographic separation and MS sensitivity.&nbsp;</p><p>In this application, an alternative reversed-phase approach was used for molecular confirmation of oligonucleotides. The method used ammonium bicarbonate instead of ion pairing, while still providing sufficient chromatographic retention and MS sensitivity. Twenty replicate injections of three different antisense oligonucleotides and five replicates of a single siRNA were performed to ensure the applicability and reproducibility of the method.</p><h4><strong>Experimental&nbsp;</strong></h4><h5><strong>Instrument configuration&nbsp;</strong></h5><p>This experiment was conducted using the following instrument configuration:</p><ul><li>Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=InfinityLab+Pro+iQ+Plus+LC%2FMS"><strong>InfinityLab Pro iQ Plus LC/MS</strong></a> system (G6170A)&nbsp;</li><li>Agilent Infinity II 1290 bio binary pump (G7120A)&nbsp;</li><li>Agilent Infinity II 1290 bio multisampler (G7167B)&nbsp;</li><li>Agilent Infinity II 1290 bio column compartment (G7116B)&nbsp;</li><li>Agilent Infinity II 1260 diode array detector HS (G7117C)&nbsp;</li></ul><p>Although this analysis used an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=Infinity+II+LC"><strong>Infinity II LC</strong></a> configuration, comparable results can be achieved on the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=Infinity+III+LC"><strong>Infinity III LC</strong></a> system with no changes to method parameters.</p><h4><strong>Results and discussion</strong></h4><p>Established in 1997, an alkylamine ion pair with perfluorinated alcohol as the acidic modifier is the preferred mobile phase for LC/MS analysis of oligonucleotides.<sup>3</sup> This is due to its chromatographic performance and electrospray efficiency, especially when compared to mobile phases using acetate as the counter ion. Extensive work has further demonstrated a wide experimental design space when using this powerful ion-pairing system.<sup>4</sup>&nbsp;</p><p>However, there are consequences when using alkylamine and HFIP for LC/MS methods. First, optimization of buffer components is necessary since oligo modifications and sequence affect electrospray desorption and chromatography.<sup>5</sup> Second, alkylamine may contaminate ionization sources and LC systems, leading to background peaks if polarity is switched back to positive mode. Consequently, this requires extensive cleaning/passivation of LC components and ion source surfaces. Even then, some labs may dedicate systems to negative mode due to the adsorption of alkylamines onto the LC/MS system. Finally, alkylamine-containing mobile phases have a short shelf life if not kept sealed under argon gas, and thus, mobile phases must be made fresh, sometimes daily, to ensure consistent method performance.&nbsp;</p><p>For labs performing molecular weight confirmation workflows where many oligos are analyzed, optimizing mobile phase conditions may not be feasible. Additionally, LC/MS downtime due to instrument maintenance and daily preparation of buffers may lead to sample backlogs, which for many labs can be a considerable challenge. A more practical approach would be to use a non-ion-pairing, reversed-phase methodology.&nbsp;</p><p>Recent work provides a more practical and cost-effective alternative to ion pairs, using an ammonium bicarbonate (NH<sub>4</sub> HCO<sub>3</sub>) buffer and methanol as the strong solvent.<sup>6</sup> This is an advantageous method for molecular weight confirmation, as ESI sensitivity and chromatographic performance are sufficient, even with minimal optimization of the mobile phase and gradient. Further, this referenced work postulates that carbon dioxide outgassing facilitates droplet formation, while ammonia evaporation contributes to proton adduction, thus allowing for positive mode analysis. This, therefore, eliminates the need to dedicate a system for negative mode analysis.</p><h4><strong>Conclusion</strong></h4><p>The method described in this application note provides a practical approach for medium- to high-throughput molecular confirmation of synthetic oligonucleotides. The Agilent Pro iQ Plus demonstrates excellent resolution and sensitivity for a unit mass detector, even at high m/z ranges that exceed the capabilities of many single quadrupole detectors. The method uses a novel ammonium bicarbonate mobile phase, providing sufficient LC/MS performance for labs analyzing many types of oligos, including antisense oligonucleotides and siRNAs. LC and MS results described in this application note are reproducible. Data analysis workflows are simplified using Agilent OpenLab CDS MS spectral deconvolution, which is automated by unattended processing methods that require minimal optimization.</p><h3><strong>2. Shimadzu: One System, Multiple Solutions: Analysis of PFAS &amp; Cyanotoxins in Water Adhering to EPA 537.1, 544, and 545&nbsp;</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/an_02_ssi_176_en_792c78f426.pdf"><strong>Full PDF for download</strong></a></li></ul><p><strong>User Benefits</strong></p><ul><li>A single Shimadzu LCMS-8060RX triple quadrupole mass spectrometer can successfully quantitate both PFAS and cyanotoxins in water with automatic method switching.</li><li>With only a five-minute rinsing time between methods, the system maintains high accuracy and sensitivity over an extended run time, even with multiple injections and method changes.</li><li>This single system approach allows laboratories to respond swiftly to emergencies, like Harmful Algae Blooms, while minimizing disruption to routine PFAS testing and eliminating the need to invest in multiple instruments.</li></ul><p>Per- and Polyfluoroalkyl Substances (PFAS) are a group of synthetic chemicals extensively used in consumer products (e.g., food packaging materials and non-stick coatings) and industrial applications such as firefighting foams and polymer/plastics manufacturing. Their remarkable properties, including high stability and resistance to degradation, coupled with widespread usage, have led to their persistent accumulation in the environment. Consequently, regulatory and governmental organizations, including the US Environmental Protection Agency (EPA) and the European Chemicals Agency (ECHA)<sup>1</sup>, are working to restrict their presence in the environment.&nbsp;</p><p>In the United States, EPA Method 537.1 is one of the approved methods by EPA for the analysis of PFAS in drinking water. It targets 18 compounds, utilizing solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) for detection at low ng/L concentrations<sup>2</sup>. EPA Method 533 is the only other EPAapproved method for PFAS analysis in drinking water. It follows a workflow similar to that of EPA Method 537.1 but expands the target list to include 25 PFAS compounds<sup>3</sup>.&nbsp;</p><p>PFAS is not the only concern—other contaminants in drinking water can also pose significant health risks. Cyanobacteria, also referred to as blue-green algae, are photosynthetic organisms that thrive in both freshwater and marine ecosystems. The frequency and occurrence of Harmful Algae Blooms (HABs) have risen substantially over the years, primarily due to human-induced inputs of phosphorus and nitrogen into aquatic systems, fueling the global increase in harmful algal blooms. These organisms can significantly affect water quality by producing cyanotoxins such as cylindrospermopsin, anatoxin-a and microcystins. Exposure to these cyanotoxins can cause a range of adverse health effects in humans and animals, from mild skin irritations to severe illnesses<sup>4</sup>.&nbsp;</p><p>The US EPA has established Methods 544 and 545 as analytical protocols for detecting cyanotoxins in drinking water and freshwater. EPA Method 544 is designed to detect microcystins and nodularin<sup>5</sup>, while EPA Method 545 targets cylindrospermopsin and anatoxin-a <sup>6</sup>. Both methods employ liquid chromatography-tandem mass spectrometry (LCMS/MS) for precise analysis.</p><p>Ideally, separate instruments should be dedicated to analyzing PFAS and cyanotoxins to minimize the risk of contamination and interference. However, with the growing demand for water testing and rapid turn-around-times during emergencies that may alter routine testing, a single system capable of handling multiple methods offers a more costeffective solution. This application demonstrates the accurate and robust quantification of PFAS and cyanotoxins, performed in accordance with EPA Methods 537.1, 545, and 544, using a single Shimadzu LCMS-8060RX triple quadrupole mass spectrometer with automatic method switching.</p><h4><strong>Method</strong></h4><p><strong>System configuration:</strong> A Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=LCMS-8060RX"><strong>LCMS-8060RX</strong></a> triple quadrupole mass spectrometer (Figure 1) was used to quantify the PFAS and cyanotoxins in water. The front-end liquid chromatography (LC) system was configured with the Shimadzu LC-40 series, ensuring seamless automation, method switching, and high efficiency. Key modules include three degassers (one 3-channel and two 5-channel), two LC40 solvent pumps equipped with low-pressure gradient (LPGE) modules, an autosampler, a system controller, a column oven with two column switching valves (one 6-port, 2-position valve and one 7-port, 6-position valve).</p><p>PFAS contamination can originate from solvent containers and consumables used in the LC system. To minimize background interference, a delay column is implemented before the autosampler to separate background PFAS from target analytes.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This study demonstrates the successful quantification of PFAS (EPA 537.1) and cyanotoxins, including microcystins and nodularin (EPA 544) as well as cylindrospermopsin and anatoxin-a (EPA 545), using a single triple quadrupole mass spectrometer with automatic method switching. By leveraging this streamlined approach, we achieved precise and reliable measurements while maintaining high accuracy and sensitivity across extended analytical runs, even with multiple injections and frequent method transitions.&nbsp;</p><p>A key advantage of this approach is the efficient switching between analytical methods with only a five-minute rinse between methods. This ensures complete removal of residual analytes and prevents mobile phase contamination, allowing smooth transitions between PFAS and cyanotoxin analysis without compromising data quality. The rapid automatic rinsing process eliminates the need for extensive manual intervention, reducing instrument downtime and increasing overall laboratory productivity.&nbsp;</p><p>By consolidating multiple analytical methods into a single instrument, this approach minimizes the need for separate systems, thereby reducing both capital investment and maintenance costs. This single system enables laboratories with the capability to respond quickly to emergencies, such as HABs, without major disruption of their routine testing, for PFAS and potentially other organic contaminants. Furthermore, automation significantly enhances operational efficiency by minimizing manual labor requirements, improving reproducibility, and optimizing high-throughput sample analysis. This method provides a cost-effective and reliable solution for laboratories performing environmental monitoring and regulatory compliance testing.</p><h3><strong>3. Thermo Fisher Scientific: Comprehensive screening of per- and polyfluoroalkyl substances (PFAS) in textiles: Utilizing combustion ion chromatography for total organic fluorine (TOF) analysis</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/an_003571_ic_Integrion_fluoride_textiles_an003571_na_en_8643b1e42a.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Per- and polyfluoroalkyl substances (PFAS) are used globally across various industries and comprise thousands of individual compounds. These amphipathic substances are extensively incorporated into textile-based products, such as clothing, carpets, and other household items to provide waterproofing, oil, dirt, and heat protection, as well as increased durability. PFAS can be released from functional textiles according to an outdoor aging study.<sup>1</sup> The Department of Toxic Substances Control (DTSC) has found that treated textiles and leathers are major sources of PFAS exposure for people and the environment, particularly through inhalation when using these products. PFAS also contribute to widespread environmental contamination, similar to other consumer products like food packaging and cosmetics.<sup>2</sup></p><p>Traditionally, PFAS testing has been conducted using liquid chromatography coupled with triple quadrupole mass spectrometry (LC-QQQ). While LC-QQQ is a targeted analytical technique, its results are limited to compounds for which standards are available. Consequently, these targeted studies do not necessarily provide a comprehensive measurement of the total PFAS in samples. Recently, laboratories have focused on developing and validating lower-cost alternatives that offer a more comprehensive measure of total PFAS content. This has led to the development of several methods for measuring total fluorine (TF) as a proxy for total PFAS contamination in textiles. Technologies employed in these methods include combustion ion chromatography (CIC)<sup>5</sup> and particle-induced γ-ray emission spectroscopy (PIGE).6 However, measuring only TF is not a reliable proxy for PFAS, as it includes both organic and inorganic fluorine, the latter of which is not considered PFAS. Using TF as a measure of PFAS may result in overestimating the amount of PFAS in samples.&nbsp;</p><p>California AB 1817 introduces a new methodology for testing PFAS contamination or intentional use of PFAS in fabrics based on the amount of TOF in the sample. This is a significant change from previous approaches, employing a non-specific untargeted method to PFAS detection and quantification. In this study, we developed a method to determine TOF in textiles using CIC. CIC offers excellent sensitivity and versatility, independent of sample thickness, and the capability for direct ion chromatography (IC) analysis to determine inorganic fluorine (IF).</p><h4><strong>Experimental&nbsp;</strong></h4><h5><strong>Equipment&nbsp;</strong></h5><p><strong>A </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/408"><strong>Thermo Scientific™ Dionex™ Integrion™ HPIC™ System</strong></a><strong> (P/N 22153-60306) including:&nbsp;</strong></p><ul><li>Eluent generator&nbsp;</li><li>Pump&nbsp;</li><li>Degasser&nbsp;</li><li>Conductivity detector&nbsp;</li><li>Column oven temperature control&nbsp;</li><li>Detector-suppressor compartment temperature control&nbsp;</li></ul><p><strong>Nittoseiko Automatic Combustion Unit Model AQF–2100H system* including</strong>:&nbsp;</p><ul><li>Automatic Sample Changer ASC-270LS&nbsp;</li><li>Horizontal Furnace Model HF-210&nbsp;</li><li>Gas Absorption Unit GA-211&nbsp;</li><li>External Solution Selector ES-210&nbsp;</li><li><strong>*</strong>Any combustion oven with equivalent performance will work.</li></ul><h5><strong>Software&nbsp;</strong></h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/76"><strong>Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)</strong></a> Version 7.3 1 with DDK driver to control the combustion system</li></ul><h4><strong>Results and discussion</strong></h4><h5><strong>TOF in textile samples by CIC</strong></h5><p>The TF in a sample is defined as the sum of TIF and TOF. In this study, TOF was determined by subtraction of TIF from TF. After combusting the solid sample, TF was measured using IC. High concentrations of TF (&gt;100 ppm) were observed in five of the six samples tested (Table 2).&nbsp;</p><p>TIF was measured using IC after extracting the ground textile samples with DI water. The contribution of TIF to TF was found to be very small (&lt;1 ppm) as shown in Table 2. Even after subtracting TIF, the TOF remained above 100 ppm for five of the samples. Therefore, the five samples did not meet the regulatory limit of 100 ppm TOF set by the state of California.<sup>3</sup></p><p>&nbsp;Figure 5 shows the IC chromatograms of TF and TIF of Sample #1. Fluoride is well separated from other anions that may be present in samples, allowing for accurate determination.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>We developed a sensitive and accurate method using CIC to determine TOF in textiles. The method offers a detection limit of 0.37 ppm, which is significantly lower than the regulatory threshold of 100 ppm, ensuring reliable detection of PFAS. Spiked recovery experiments show the method’s accuracy falls within a range of 85–105%. This TOF method is beneficial for manufacturers who want to ensure compliance with current state regulations. Moreover, the CIC workflow provides a more comprehensive understanding of the total PFAS and fluorinated content in textiles compared to LC-MS targeted approaches, offering greater clarity about the potential PFAS contamination in textiles.</p>

News from LabRulezLCMS Library - Week 24, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 16th June 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you brochure by <strong>Agilent Technologies </strong>and<strong> </strong>application notes by<strong> Shimadzu, Thermo Fisher Scientific </strong>and<strong> Waters Corporation!</strong></p><h3><strong>1. Agilent Technologies: PFAS Analysis Without Compromise</strong></h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/br_sample_prep_solutions_for_environmental_pfas_analysis_5994_8377en_agilent_f4acd7c313.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The brochure presents Agilent’s comprehensive solutions for environmental PFAS (per- and polyfluoroalkyl substances) analysis, designed to support laboratories in meeting increasingly stringent regulatory standards. Given the persistence and bioaccumulative nature of PFAS in water, soil, and biological samples, effective and contamination-free sample preparation is crucial. Agilent offers a complete range of <strong>solid phase extraction (SPE) cartridges</strong> and start-up kits specifically tailored for EPA and ISO PFAS methods, including EPA 533, 537.1, and 1633, as well as ISO 21675:2019. These tools ensure high recovery rates, method compliance, and minimal contamination risk.</p><p>At the heart of Agilent’s offering are the <strong>Bond Elut PFAS WAX </strong>and <strong>Bond Elut PFAS WAX/Carbon S dual-phase cartridges</strong>. The WAX cartridges utilize polymeric PSDVB sorbent with diamino functionality for strong retention and selectivity, making them ideal for extracting a broad range of PFAS classes, from carboxylic and sulfonic acids to fluorotelomer sulfonates and polyfluoroalkyl ethers. The dual-phase WAX/Carbon S cartridges combine high PFAS recovery with superior matrix cleanup, effectively handling complex samples like biosolids and fish tissues in compliance with EPA Method 1633.</p><p>Agilent ensures batch-to-batch consistency through rigorous quality control. Each cartridge batch comes with a Certificate of Analysis (CoA), verifying PFAS cleanliness and recovery. This level of assurance helps labs reduce verification workload while ensuring reliable, reproducible results. Additionally, the products are compatible with automated sample preparation systems, which is essential for high-throughput labs aiming to optimize workflow efficiency.</p><p>To further support labs, Agilent offers specialized <strong>PFAS Start-Up Kits</strong> and <strong>PFC-free HPLC conversion kits </strong>for ultratrace PFAS analysis. These complete workflow solutions include vials, columns, filters, and sorbents engineered to prevent PFAS contamination. Whether the application is environmental or food-related, Agilent’s portfolio equips laboratories with the tools they need to conduct PFAS testing with confidence, accuracy, and regulatory compliance.</p><h3><strong>2. Shimadzu: Chiral Amino Acid Analysis Using a Single Quadrupole Mass Spectrometer</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00870_en_19d0c986a5.pdf"><strong>Full PDF for download</strong></a></li></ul><p><strong>User Benefits</strong></p><ul><li>Separation with a chiral column enables direct analysis of chiral amino acids without pretreatment by derivatization.</li><li>By using a high-performance single quadrupole LC-MS system, even trace quantities of D-amino acids can be detected in foods and cosmetics</li></ul><p>Of the 20 types of amino acids included in proteins, optical isomers exist for all but glycine. Most naturally occurring amino acids are L-amino acids, but advancements in analytical technology have revealed the presence of D-amino acids in many organisms. It is also becoming evident that D-amino acids have different physiological functions than L-amino acids. Consequently, D-amino acids perform attracted attention in basic research related to their physiological and medical functions and for applications in the fields of food, health, and beauty.&nbsp;</p><p>This Application News article describes using a single quadrupole LC-MS system with a crown ether-type chiral column to analyze chiral amino acids, which enables rapid analysis of chiral amino acids without derivatization pretreatment. If a comprehensive analysis of all hydrophilic metabolites that includes amino acids is required, refer also to Application News No. 01-00334-EN, which describes a useful technique forsuch analysis.</p><h4><strong>Instruments and Analysis Conditions&nbsp;</strong></h4><p>Analysis was performed with a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=Nexera+series+HPLC+"><strong>Nexera series HPLC </strong></a>system that was combined with an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=LCMS-2050"><strong>LCMS-2050</strong></a> LC-MS system (Fig. 1). Although compact, the LCMS-2050 single quadrupole mass spectrometer offers easy operability and outstanding performance. Equipped with a DUIS heated ion source, which provides the benefits of both ESI and APCI, it can analyze masses ranging from m/z 2 to 2000. That makes it well suited for simultaneously analyzing all metabolites, including amino acids, as described in Application NewsNo. 01-00334-EN.&nbsp;</p><p>The analysis condition settings for HPLC and MS are shown in Table 1. The analysis conditions for LCMS-2050 was configured based on the analysis conditions in the LC/MS/MS Method Package for D/L Amino Acids. Using a crown ether-type chiral column enables the chiral separation of all amino acids except proline, which is a secondary amine.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This article describes using a chiral column and a single quadrupole LC-MS system to analyze chiral amino acids. The technique enables direct analysis of chiral amino acids without derivatization pretreatment. Although sensitivity is lower than a triple quadrupole LC-MS system, it offers equivalent or higher sensitivity than a quadrupole time-of-flight LC-MS system or a fluorescence detector. So while it is not appropriate for analyzing ultra-trace concentrations of chiral amino acids, it is well suited to analyzing foods and other samples that contain large amounts of chiral amino acids. It also offers good throughput, with the ability to analyze samples within 15 minutes, even if that involves switching between (+) and (-) columns to separate components from contaminants in the samples. This also makes it well suited for analyzing large quantities of samples. Widespread adoption of the described techniques for chiral amino acid analysis can be expected to lead to continuous advancements in the R&amp;D of foods, cosmetics, and othersamples.</p><h3><strong>3. Thermo Fisher Scientific: Enhanced screening of PFAS compounds in wastewater: Implementing U.S. EPA Method 1621 with improved combustion-ion chromatography</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003774_ic_ic_systems_combustion_environmental_an003774_na_en_db0fb51b4c.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Per- and polyfluoroalkyl substances (PFAS) is the collective name for over 14,000 synthetic fluorinated compounds. A PFAS compound is defined as a compound containing a fully fluorinated methyl group or methylene on an alkane functional group (Organisation of Economic Co-operation and Development (OECD)) or as a fluorinated compound with at least two adjacent saturated carbons with one carbon fully fluorinated and the other at least partially fluorinated (U.S. Environmental Protection Agency (EPA)).<sup>1,2</sup> Since the 1940s, PFAS have been prevalent in many polymers, surfactants, fire-suppression chemicals, industrial products, and consumer products.<sup>3-6</sup> In addition to their extensive presence, PFAS compounds are persistent and bioaccumulate. Consequently, PFAS compounds are an environmental contamination concern. Toxicological studies of several PFAS compounds, such as perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS), indicate the potential for acute to chronic effects impacting reproductive health.<sup>7-11</sup> Fewer studies have been conducted on the thousands of other compounds grouped under the EPA PFAS classification.<sup>2</sup></p><p>The U.S. EPA has defined targeted and non-targeted analysis methods for PFAS.<sup>12-18</sup> Combustion-ion chromatography (C-IC) was previously demonstrated as a screening method for PFAS; PFAS compounds are converted to HF, and the subsequent fluoride is analyzed by ion chromatography (IC) with suppressed conductivity detection.<sup>19-24</sup> This technique is incorporated into EPA Method 1621 for non-targeted determinations of PFAS as adsorbable organic fluorine (AOF).<sup>25-28</sup> Our results from the EPA Method 1621 multi-laboratory study are also published in the Thermo Scientific Application Note AN002748 with additional tips for successful implementation in the Thermo Scientific Technical Note TN003056.<sup>29,30</sup></p><p>&nbsp;In the EPA Method 1621 collaboration study, we found that reduced baseline contamination and increased sensitivity, accuracy, and precision can be achieved by minimizing sources of contamination.<sup>29,30</sup> Another approach to reduce baseline contamination is to design the adsorption and combustionabsorption systems in a way that reduces or eliminates contamination sources. In this application, EPA Method 1621 is implemented on the offline Thermo Scientific™ Cindion™ Adsorption module, a Cindion Combustion / Absorption module with liquid and solid sample handling, and a Thermo Scientific™ Dionex™ Inuvion™ Reagent-free Ion Chromatography (RFIC™) System. The adsorption module was designed to minimize contamination by eliminating contamination sources. To increase throughput, the adsorption module is designed to semiautomatically adsorb PFAS from six water samples at a time. The Thermo Scientific™ Cindion™ Combustion-Ion Chromatography (C-IC) System was optimized for increased combustion efficiency by incorporating a Z-fold combustion tube to introduce oxygen at multiple locations. As a result, the combustion tube and furnace are shorter, and combustion times are reduced. This also results in a smaller footprint, saving crowded bench space. Data processing and system management are also more efficient because the Cindion C-IC system is controlled by a single software, the Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS). Overall, this solution provides improved sensitivity due to increased signal-to-noise, improved recoveries of added standards, and comparable reproducibility to previous results in a smaller footprint.</p><h4><strong>Experimental&nbsp;</strong></h4><h5><strong>Equipment&nbsp;</strong></h5><p><strong>Cindion C-IC system&nbsp;</strong></p><ul><li>Thermo Scientific™ Cindion™ Combustion / Absorption Module (P/N B51006425) with Thermo Scientific™ Cindion™ C-IC Solids Kit (P/N B51006426)&nbsp;</li><li>Thermo Scientific™ Cindion™ Solid / Liquids Autosampler (P/N B51006429)</li><li>Thermo Scientific™ Cindion™ Adsorption Module (P/N B51006430), includes six column holders&nbsp;</li><li>Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1078"><strong>Dionex™ Inuvion™ IC System</strong></a> with RFIC (P/N 22185-60108)&nbsp;</li><li>Optional Thermo Scientific™ Dionex™ Eluent Monitor, 4 L (P/N 22185-62708)&nbsp;</li><li>Thermo Scientific™ Thermolyne™ Muffle furnace, 2 L small bench top, to clean combustion cups, recommended for EPA Method 1621 (P/N FB1415M)&nbsp;</li></ul><p><strong>Software&nbsp;</strong></p><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/76"><strong>Chromeleon CDS software</strong></a>, Chromeleon 7 version 3.2, with Cindion C-IC system and eluent monitor drivers</li></ul><h4><strong>Results and discussion&nbsp;</strong></h4><p>The official EPA Method 1621 was updated from the draft method, and therefore, some of the section enumerations have changed. In addition, this method was updated from the EPA method by initiating the gradient at 4 min instead of 6 min to ensure that all anions are fully eluted from the column. Initial demonstration of capability In EPA Method 1621, the initial demonstration of capability (IDC) is required before analyzing samples. IDC includes determining the retention time windows of fluoride and chloride, calibration with relative standard error (RSE) 1 min from the water dip (void volume) and other peaks eluting near fluoride for accurate determinations. In hydroxide eluent separations with suppressed conductivity, as shown in Figure 2, the water dip is small and isolated from fluoride. Fluoride elutes away from the water dip in a flat baseline region. The results of these retention time experiments are summarized in Table 1. Fluoride meets the retention time criteria.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This application note demonstrates U.S. EPA Method 1621 results using an improved C-IC workflow solution. The C-IC complete flow path includes the adsorption of PFAS in wastewater samples using the offline Cindion adsorption module, the combustion of the PFAS to fluoride using the Cindion combustion-absorption system, and quantitation using a Dionex Inuvion IC instrument with RFIC. The results were improved compared to previous implementation of EPA Method 1621 in Thermo Scientific Application Note AN002748. MDLs were improved (1.7 μg/L vs. 2.3 μg/L) with comparable reproducibility (4.5% RSDs vs. 4.6%) and improved accuracy (82–101% vs. 70–120%) as compared to previous results. This method showcases significant advantages of the Cindion C-IC system for measuring AOF and screening for PFAS in wastewater. In addition to ease of use, RFIC with hydroxide eluents provides more accurate reporting because fluoride easily elutes from the water dip, eliminating the need for manual integration. These data collectively highlight the power of C-IC in eliminating the sample matrix and measuring only adsorbable fluorine content in samples, successfully achieving the goals outlined in U.S. EPA Method 1621.</p><h3><strong>4. Waters Corporation: Enhanced Reliability for Long-Term PFAS Analysis with the Xevo TQ Absolute XR Mass Spectrometer</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008824_en_a91738478b.pdf"><strong>Full PDF for download</strong></a></li></ul><p><strong>Benefits</strong></p><ul><li>Xevo TQ Absolute XR provided maximal system uptime for PFAS analysis across 10 weeks and more than 7000 injections with no unscheduled downtime.</li><li>Reliable calculated concentrations were maintained for PFAS at relevant levels in extracts of river water, biosolid, and landfill leachate with %RSDs of &lt;8.4%.</li><li>Seamless batch review and long-term calibration management using waters_connect™ for Quantitation Software accelerated data validation workflows.</li></ul><p>As awareness grows around the environmental and health impacts of PFAS, regulatory pressure continues to intensify globally. The EPA Method 1633A1 has become a critical protocol for the quantitation of 40 PFAS compounds in diverse environmental matrices, including non-potable water, soils, biosolids, and tissues. Although the method describes a solid phase extraction (SPE) clean-up step for all sample types, these matrices still contain co-extractive interferents when introduced into an LC-MS/MS system, which can contaminate the system and degrade method performance over time. This application note describes how the StepWave XR Ion Guide, a novel slotted bandpass ion guide within the Xevo TQ Absolute XR Mass Spectrometer, can be integrated into a typical PFAS workflow to enhance signal robustness while preserving sensitivity and speed, thereby boosting method reliability.</p><h4><strong>Experimental</strong></h4><h5><strong>LC Conditions</strong></h5><ul><li>UPLC system: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY™ Premier System </strong></a>with Binary Solvent Manager and Flow-Through Needle&nbsp;</li></ul><h5><strong>MS Conditions</strong></h5><ul><li>MS system: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/554"><strong>Xevo TQ Absolute XR Mass Spectrometer</strong></a></li></ul><h4><strong>Results and Discussion</strong></h4><h5><strong>QC Performance&nbsp;</strong></h5><p>Method performance was evaluated every 10 sample extract injections to ensure that the weekly calibration of the method was stable. Figure 2 shows the QC plots for GenX, L-PFHxS, L-PFOS, PFBS, PFNA, and PFOA with a tolerance of ±30% set from the assigned concentration level (0.1–0.2 ng/mL) over the course of the study. Table 1 lists the %RSDs for the ion ratios for the same compounds. QC measured concentrations and ion ratios were within the set tolerances across 10 weeks and more than 7,000 injections with no unscheduled downtime. This illustrates the reliability of the Xevo TQ Absolute XR for PFAS analysis using a weekly calibration routine.</p><h4><strong>Conclusion</strong></h4><p>The StepWave XR Ion Guide within the Xevo TQ Absolute XR Mass Spectrometer was introduced into a typical PFAS workflow and shown to maintain method reliability for extended periods of time. The Xevo TQ Absolute XR provided maximal system uptime for PFAS analysis across 10 weeks and more than 7,000 injections with no unscheduled downtime. Concentrations for PFAS at relevant levels were reliably calculated in extracts of river water, biosolids, and landfill leachate with trueness in the range 70–130% and %RSDs of &lt;8.4%. These findings<br>support the Xevo TQ Absolute XR as a powerful platform for laboratories seeking to meet regulatory requirements for PFAS monitoring while minimizing system downtime and maintenance.&nbsp;</p>

News from LabRulezLCMS Library - Week 25, 2025

<p><strong>Gas Chromatography-Mass Spectrometry (GC-MS) is a workhorse in analytical laboratories, prized for its sensitivity, selectivity, and versatility. Thermo Scientific </strong><a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/mass-spectrometry/gas-chromatography-mass-spectrometry-gc-ms.html"><strong>GC-MS systems</strong></a><strong> are built to support demanding workflows with smart hardware innovations like NeverVent technology, and iConnect injectors and detectors.&nbsp;</strong></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Chromeleon_CDS_Hints_and_Tips_to_Help_Optimize_your_GC_MS_Workflows_45f2350306.jpg" alt="Thermo Fisher Scientific: Chromeleon CDS: Hints and Tips to Help Optimize your GC-MS Workflows" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Chromeleon_CDS_Hints_and_Tips_to_Help_Optimize_your_GC_MS_Workflows_45f2350306.jpg 236w," sizes="100vw" width="1024" height="678"></p><article><div><p>But even the smartest hardware can only take you so far. For many scientists and lab managers, the real bottleneck isn’t the instrument—it’s the manual, time-consuming steps required to keep workflows moving and data processing on track. That’s where Thermo Scientific Chromeleon software comes in.</p><h3><strong>Why GC-MS workflows can be a headache</strong></h3><p>Even with state-of-the-art hardware, GC-MS workflows demand attention. Routine maintenance—like column trimming, source cleaning, and inlet checks—must be tracked and managed. Meanwhile, retention time shifts can throw off compound detection, forcing analysts to manually correct and realign data.</p><p>And when it comes to data review, it’s easy to lose hours scrolling through chromatograms to check integrations and flag anomalies. It slows down decision-making and is tedious and can be prone to error.</p><h3><strong>Chromeleon software: Smarter software for GC-MS success</strong></h3><p><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Chromeleon software</strong></a> enhances and brings effortless usability to your GC-MS system by bringing efficiency, automation, and visibility into your operations. Here’s how:</p><h4><strong>✅ Retention time alignment</strong></h4><p>Automatically correct retention times across compounds with built-in tools. Save time and ensure consistent compound detection.</p><h4><strong>🛠 Integrated system suitability tests</strong></h4><p>Proactively monitor instrument performance by building automated system suitability checks directly into your sequences, enabling you to catch issues before they impact data quality.</p><h4><strong>🧠 SmartStatus intelligent software &nbsp;</strong></h4><p>Built into Thermo Scientific Chromeleon CDS, SmartStatus gives you a full view of your GC-MS system’s health. Track consumable usage, get alerts when maintenance is due, and monitor performance trends. &nbsp;</p><h4><strong>👁 Custom view settings</strong></h4><p>Streamline data review with tailored layouts that highlight exactly what you care about—whether that’s retention times, quantitation accuracy, or quality checks.</p><h4><strong>🚩 Automatic result flagging</strong></h4><p>Build in rules to flag integration errors, missing peaks, or results that fall outside of defined criteria. Zone in on issues fast—without inspecting every injection.</p><h4><strong>📄 Consistent, audit-ready reporting</strong></h4><p>Generate standardized reports with just a click—complete with full traceability. No need to carry out calculations outside of the software.</p><h3><strong>The bottom line</strong></h3><p>Your Thermo Scientific GC-MS system is built for high performance. <strong>Chromeleon software</strong> helps you <i>run it smarter</i>—by catching issues early, simplifying data review, and reducing the manual work that slows you down.</p><p><i>“Faster evaluation of data with Chromeleon on the TSQ 9610 generates a higher sample throughput with a time saving of 10% to 20% per sample run.”</i><br><i><strong>– Eurofins SOFIA GmbH</strong></i></p><p>From instrument control to streamlined data review and compliance-ready reporting, <strong>Chromeleon software </strong>helps you reclaim time, reduce errors, and drive consistency—every step of the way.</p><blockquote><p><strong>Ready to see it in action?</strong></p><p>Watch our <a target="_blank" rel="noopener noreferrer" href="https://event.on24.com/wcc/r/4940132/3DD01B56C4383C3BF8276C47E689D0F0?partnerref=E.25CMD.CH102.25762.01"><strong>GC-MS Masterclass webinar</strong></a><strong>, </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/cs_000731_gc_GC_MS_MS_TSQ_9610_food_enviro_testing_cs000731_na_en_7e59895e62/cs-000731-gc-GC-MS-MS-TSQ9610-food-enviro-testing-cs000731-na-en.pdf"><strong>hear what our customers have to say</strong></a><strong> </strong>or visit the <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/chromatography/chromatography-learning-center/chromeleon-cds-information.html"><strong>Chromeleon University</strong></a> to learn how smarter software can take your workflows to the next level.</p><p><strong>Visit us on&nbsp;</strong><a target="_blank" rel="noopener noreferrer" href="https://www.linkedin.com/showcase/72003132/admin/dashboard/"><strong>LinkedIn:</strong></a>&nbsp;#Chromeleon #GCMS</p></blockquote></div></article><section><blockquote><h4><strong>Zoe Julian</strong></h4><p>Zoe Julian is a Product Marketing Manager for Chromatography and Mass Spectrometry software at Thermo Fisher Scientific. With over 12 years' experience of working with chromatography and mass spectrometry techniques with a background in GC and GC-MS(/MS) organic environmental analysis, she has helped many laboratories and industries improve their workflows through a unique understanding of their challenges. Transitioning to a focus on Chromeleon CDS she has shown customers how software solutions can improve their productivity and support their day-to-day operations.</p></blockquote></section>

Chromeleon CDS: Hints and Tips to Help Optimize your GC-MS Workflows

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 23rd June 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application note by <strong>Shimadzu, </strong>posters by <strong>Agilent Technologies / ASMS </strong>and<strong> Thermo Fisher Scientific / ASMS </strong>and presentation by<strong> William &amp; Mary / MDCW!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Improved Determination of Polychlorinated Biphenyl Compounds by US EPA Method 1628</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_5977c_pcb_hydroinert_column_asms_2025_mp_360_en_agilent_8db06d5b24.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>Polychlorinated Biphenyl (PCBs) and the Environment&nbsp;</strong></h5><p>Polychlorinated Biphenyls (PCBs) are synthesized compounds that belong to the chlorinated hydrocarbon family of compounds. PCBs were used in a variety of industrial applications such as electrical components, plasticizers and pigments/dyes, until they were banned in 1979 by the Toxic Substances Control Act (TSCA)<sup>1</sup> . PCBs are considered to persistent organic pollutants (POPs) as they do not easily degrade in the environment. PCBs can be found in the air, water, and soil and have been known to bioaccumulate in marine life.</p><p>The EPA has recently developed a low-resolution mass spectrometry method that can calibrate 65 PCBs congeners and screens for all 209 using labeled PCB compounds for direct and indirect quantitation<sup>2</sup> . The 65 congeners are targeted for calibration and quantitation due to specific factors described in the method<sup>2</sup> . As with most EPA methods, the prescribed methodology utilizes helium as a carrier gas. The recommended column for this analysis makes adequate separation and quantitation more challenging. To achieve separation that meets the method criteria, the run time is over 40 minutes long. By using a column better suited for PCB congener separation and hydrogen as the carrier gas, superior separation can be achieved in under 20 minutes, resolving previously co-eluting analytes.</p><h4><strong>Experimental&nbsp;</strong></h4><h5><strong>System configuration using hydrogen carrier gas&nbsp;</strong></h5><p>The Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890%2F5977C+GC%2FMSD"><strong>8890/5977C GC/MSD</strong></a> equipped with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=HydroInert+Ion+source"><strong>HydroInert Ion source</strong></a> was operated in selective ion monitoring (SIM) mode for this analysis.</p><h4><strong>Conclusions</strong></h4><h5><strong>Faster Analysis, Superior Separation Achieved&nbsp;</strong></h5><ul><li>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=DB-XLB+column"><strong>DB-XLB column</strong></a> offers enhanced selectivity for PCB congeners, resulting in previously co-eluting congeners to separate.&nbsp;</li><li>Selectivity is easily achieved operating the MSD in SIM mode.&nbsp;</li><li>The method meets the 10ppb detection limit for all the quantified compounds.</li><li>The HydroInert ion source allows hydrogen carrier gas to be used for more rapid analysis.</li></ul><h3><strong>2. Shimadzu: Simultaneous Analysis of Synthetic Musk Compounds in Water Using a Triple Quadrupole GC-MS System</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_09_ssk_020_en_4ae628cef8.pdf"><strong>Full PDF for download</strong></a></li></ul><p><strong>User Benefits:</strong></p><ul><li>Using a GC-MS/MS, synthetic musk compounds in water can be accurately quantified with high sensitivity.</li><li>Supporting effective environmental monitoring in water and risk assessment using GC-MS/MS</li></ul><p>Synthetic musk compounds (SMCs) are synthetic organic substances designed as substitutes for natural musk and are widely used in various household products. During everyday activities such as showering and washing, these compounds are released into wastewater. However, current wastewater treatment processes cannot completely remove SMCs, allowing them to enter aquatic ecosystems. As highly bio-accumulative organic compounds, SMCs can cause both acute and chronic toxicity in aquatic organisms. They are also known to cause endocrine disruption when accumulated in the human body1-3) . Due to these potential risks, continuous monitoring of SMCs in water is essential. The main analytical methods for detecting SMCs in water include liquid-liquid extraction (LLE), solid-phase extraction (SPE), and solid-phase microextraction (SPME). Liquid-liquid extraction method requires a large amount of solvent and long preparation time but has the advantage of simultaneously extracting multiple organic compounds 4) . In this application news, 15 types of SMCs in water were simultaneously analyzed using the gas chromatography method with liquid-liquid extraction method.</p><h4><strong>Analytical conditions</strong></h4><p>In this newsletter, SMCs in water were analyzed using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-TQ8050+NX"><strong>GCMSTQ8050 NX</strong></a> of SHIMADZU (Figure 1). The instrumental detailed analytical conditions of instrument and the MRM conditions for each compound were shown in Table 1 and 2, respectively.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>The simultaneous analysis of 15 SMCs in water was performed using the SHIMADZU GCMS-8050 NX system. The coefficient of determination(R2) of the calibration curve for all SMCs were 0.99 or higher. The LOD and LOQ were ranged from 0.003 to 0.020 ng/mL and 0.01 to 0.07 ng/mL, respectively. The recovery test results were between 86.3 % and 106.4 %, with a relative standard deviation (RSD) of 0.7 % to 4.2 %. This analytical method, using a GC-MS/MS system, provided reliable quantitative results for 15 synthetic musk compounds in water samples and demonstrated high sensitivity and efficiency.</p><h3><strong>3. Thermo Fisher Scientific / ASMS: Performance evaluation of GC-MS/MS for Dioxin analysis with amendments to EU Regulations 644/2017 and 771/2017 for food and feed&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PO_298_ASMS_25_performance_evaluation_GC_MS_MS_dioxin_analysis_po298_na_en_8721a5f8dc.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Polychlorinated dibenzo-p-dioxins/furans (PCDD/F), or dioxins, are persistent organic pollutants (POPs) that can accumulate within food chains due to their chemical stability and high fat solubility, posing health risks to humans through food consumption<sup>1</sup> . Current regulations monitor food and feed for dioxins, with maximal allowable levels for PDCC/Fs in feedstuffs at the pg•g-1 concentration range<sup>2</sup> . However, a recent review process has proposed a reduction of up to 40% in these levels by 2024 for certain feed items, such as animal/milk/egg fats (1.0 pg•g-1), fish oil (3.5 pg•g-1), and fish feed (1.0 pg•g-1)<sup>3</sup> . Since 2014, the European Commission has permitted the use of gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) for food and feed analysis as an alternative to GC-high resolution mass spectrometry (HRMS)<sup>4,5</sup> . With the proposed reduction in maximum limits, the performance of current instrumentation to achieve these targeted limits must be assessed.</p><p>Laboratories face challenges in maintaining consistent sensitivity to detect trace levels of dioxins in complex food matrices and in reporting various regulatory requirements for PCDD/ F analysis<sup>6,7</sup> . This study used the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/485"><strong>Thermo ScientificTM TSQTM 9610 triple quadrupole GC-MS/ MS</strong></a> system with the NeverVentTM advanced electron ionization (AEI) source to demonstrate compliance with the proposed regulatory limits for PCDD/F in food and feed samples. The aim was to ensure consistency with previously determined concentrations of PCDD/F in food and feed matrices and meet current compliance with the EU regulations.</p><h4><strong>Materials and methods</strong></h4><p>Data was acquired, processed, and reported using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Thermo Scientific Chromeleon Chromatography Data System (CDS) software</strong></a>, version 7.3. Integrated instrument control ensures full automated setup of the Dioxin analytical workflow through the eWorkflow which provides optimized instrument / quantification methods, view settings for time efficient data evaluation and customizable report templates. Isotopic dilution quantification is performed automatically in real time with the incorporated custom variable and formula functionality eliminating the need for exporting to external software packages.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>The results of these comprehensive experiments demonstrate that the TSQ 9610GC-MS/MS system, configured with the NeverVent AEI source and controlled using Chromeleon CDS software together with the Dioxin eWorkflow, can deliver reliable regulatory compliant performance for the quantification and confirmation ofPCDD/Fs food and feedstuffs:&nbsp;</p><ul><li>Fentogram level sensitivity performance for ultra trace level determination of PCDD/F within food and feed samples&nbsp;</li><li>Check standard performance was within quantitation and ion ratio thresholds for regulatory method compliance at femtogram levels.&nbsp;</li><li>Accurate and precise quantitation at both current and newly adopted maximum limits for PCDD/F in food and feed.&nbsp;</li><li>Chromeleon CDS software, version 7.3, provides an integrated platform, with the ability to automatically setup, easily acquire, process and report compliant data in a fully regulated environment, eliminating the need for using external spreadsheet programs.&nbsp;</li><li>Chromeleon eWorkflows, available from Thermo Scientific also provide error-free execution of each analysis to meet standard operating procedure (SOP) requirements, further simplifying the user</li></ul><h3><strong>4. William &amp; Mary / MDCW: Method optimization of fingermark residue using comprehensive two-dimensional gas chromatography&nbsp;</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/FL_07_Macturk_MDCW_2025_Oral_Presentation_4c2c820f98.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Fingermarks—smudged or incomplete fingerprints—may lack value for direct identification but can still offer critical information through their chemical residue. This study explores the potential of nontargeted chemical analysis of fingermark residue to determine donor characteristics such as sex and age. Using comprehensive two-dimensional gas chromatography (GC×GC), the team sought to enhance analytical resolution and method efficiency.</p><h4><strong>Experimental Approach</strong></h4><p>Researchers first collected fingermark residue using cotton swab extraction, followed by centrifugation and sample preparation. A GC×GC method was optimized by adjusting parameters like modulation period, hot pulse time, oven hold times, and ramp rate. Multiple method configurations were tested for chromatographic resolution, and the optimized helium-based method was later translated for use with hydrogen carrier gas using modeling tools.</p><h4><strong>Results</strong></h4><p>Method optimization led to significant improvements in peak separation, enabling identification of various compound classes including sterols, fatty acid methyl esters, fatty alcohols, and steroids. Additionally, unexpected anthropogenic substances such as sunscreen agents and plasticizers were detected. Hydrogen-based methods were able to achieve comparable separation quality, with the “H₂ Translate” method offering the highest number of identifiable peaks.</p><h4><strong>Conclusion</strong></h4><p>This study demonstrates that nontargeted GC×GC analysis is effective for resolving both endogenous and exogenous compounds in fingermark residue. The optimized methods not only improve forensic chemical profiling but also support a successful transition from helium to hydrogen as a carrier gas—promoting sustainability without compromising analytical performance.</p>

News from LabRulezGCMS Library - Week 26, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 30th June 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you other document by <strong>Agilent Technologies </strong>and<strong> </strong>posters by<strong> Shimadzu / ASMS, Thermo Fisher Scientific / ASMS </strong>and <strong>Waters / ASMS</strong>!</p><h3><strong>1. Agilent Technologies: Understanding Solvent Focusing Gas Chromatography and How it can be Optimized for Splitless Injections&nbsp;</strong></h3><ul><li>Other document (white paper)</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/wp_solvent_focusing_gc_5994_8387en_agilent_7911ade217.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Discussions of the basic mechanism of gas chromatography (GC), samples can start as a liquid, solid, or a gas. These samples, when not in gas phase, are converted into a vapor made up of solvent and analytes that are then separated using a GC column. The type of film or stationary phase used in the column helps to separate the compounds of a sample mixture. Meanwhile, the role of the gaseous mobile phase is to move compounds through the column without chemically interacting with them.1 With splitless injections, almost the entire sample is transferred onto the column head, making it ideal for trace level analysis, but more susceptible to solvent interactions due to the large volume of solvent also introduced to the column. It is important to understand all the variables and how to optimize them to successfully perform splitless injections, including the role of the sample solvent and related solvent effects.</p><h4><strong>Sample preparation and solvent selection</strong></h4><p>Prior to efficient sample preparation methods for the analysis of pesticides, a guard column was used to help protect the analytical column from heavy matrix or nonvolatile analytes. The primary method of sample preparation used was solvent dilution in hexane or dichloromethane, which potentially passed through a filter, and then injected directly into the inlet and analyzed on a 5% phenyl phase type column. This can be referred to as the dilute and shoot method. As dichloromethane and hexane are both compatible solvents with a 5% phenyl phase, the guard column was only needed to protect the analytical column from matrix, and not from adverse&nbsp;wettability.&nbsp;</p><p>With the adoption of more involved sample preparation techniques, traditionally used in liquid chromatography, samples typically finish their preparation in the polar solvent acetonitrile. For GC analysis solvent exchange is employed, which is the process of drying down a sample in one solvent under nitrogen gas and reconstituting it in another solvent such as hexane. This procedure is performed to ensure proper interactions between solvent and column phase. Since these cleaned up samples contained less matrix, the need for a guard column was decreased.6 Gradually the requirement for solvent exchanges was decreased to decrease the overall sample preparation time, but this left the prepared samples in a final solvent of acetonitrile.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>For a gas chromatography analysis to be successful there are many factors to be considered. These factors include injection speed, solvent choice, installation of the column, and the column phase selection. Solvent selection is important in more decisions than determining which solvent will dissolve analytes. Solvent selection can impact vaporization volume in the liner, as well as impact reconcentration at the head of the GC column.&nbsp;</p><p>Splitless&nbsp;injections will be more affected by solvent selection, as there will be a greater amount of solvent introduced to the column and greater interactions between the solvent and column phase. If the solvent and column phase are mismatched, there will be an increase in the flooded zone, and a subsequent impact to the peak shape of analytes. To mitigate the problem of using a polar solvent with a nonpolar column, a guard column can be used to help refocus the solvent and analytes at the head of the analytical column and improve analyte peak shape.</p><h3><strong>2. Shimadzu / ASMS: PFAS in Bottled Water: A Simple Approach Using HS-SPME GC/MS/MS for Volatile Contaminant Analysis</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_25_TP_312_a610778a69.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Concerns about per- and polyfluoroalkyl substances (PFAS) contamination in bottled water, linked to significant health risks, are growing. The Food and Drug Administration (FDA) has published plans surveying bottled water for PFAS in 2024-2025. While Liquid Chromatography/Mass Spectrometry (LC/MS) is the primary analytical method for PFAS, it struggles to analyze certain PFAS related compounds like fluorotelomer alcohols (FTOHs), perfluoroalkyl iodides (PFIs), and (n:2) fluorotelomer iodides (FTIs). Gas Chromatography/Mass Spectrometry (GC/MS) offers a complementary approach for volatile PFAS. This study utilizes Head-Space Solid Phase Microextraction Triple Quadrupole Gas Chromatography/Mass Spectrometry (HS-SPME GC/MS/MS) to analyze PFAS in bottled water. This technique offers several advantages, including minimal sample preparation, making it a valuable tool for comprehensive PFAS analysis.</p><h4><strong>Methods</strong></h4><p>A volatile PFAS analysis method was developed on a Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-TQ8040+NX"><strong>GCMS-TQ8040 NX</strong></a> with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=AOC-6000+Plus"><strong>AOC-6000 Plus</strong></a> multifunctional autosampler equipped with a solid phase microextraction (SPME) module (Figure 1).&nbsp;</p><p>Thirteen PFAS target compounds were included in the Multiple Reaction Monitoring (MRM) method. The PFAS chemical classes were perfluoroalkyl iodides (PFIs), (n:2) fluorotelomer iodides (FTIs), (n:2) fluorotelomer acrylates (FTACs), (n:2) fluorotelomer methacrylates (FTMACs), (n:2) fluorotelomer alcohols (FTOHs) and perfluoroalkane sulfonamides (FASAs). Internal standards (IS) FTOHs, FASAs and FTAC mass-labelled compounds were added to each vial prior to extraction. Concentrations of the target compounds were calculated using isotope dilution.&nbsp;</p><p>An internal calibration curve was prepared in 10 mL of reagent water at concentrations of 2000, 1000, 500, 100, 50, 10, 2.5 and 1 ng/L. The IS were spiked at 100 ng/L to each calibrator. Sodium Chloride (NaCl) was added to each vial to achieve a final salinity concentration of 2% NaCl (w/v). These calibrators were vortex for 30 seconds and then placed on the AOC-6000 Plus autosampler rack for analysis.&nbsp;</p><p>The optimized parameters of the HS-SPME GC/MS method for the targeted PFAS are listed in table 1. Quantitative and reference ions for each PFAS target are listed in table 2. The associated internal standard used for each compound is also listed in table 2.&nbsp;</p><p>A laboratory control sample (LCS) was analyzed to determine the general performance of the method in a clean matrix. The bottled water samples were analyzed to determine the effect of matrix on method performance. The type of bottled water analyzed was purified water.</p><h4><strong>Conclusion</strong></h4><p>The PFAS family includes thousands of compounds across diverse chemical classes, making comprehensive analysis challenging and often necessitating multiple analytical techniques. LC-MS is widely used and well-established for PFAS analysis but is less effective for detecting certain compounds - particularly volatile PFAS. In contrast, GC-MS excels at analyzing volatile PFAS and serves as a valuable complement to LC-MS, offering a more complete and balanced approach to PFAS detection. By extending the range of detectable compounds, GC-MS helps overcome PFAS analysis limitations previously imposed by instrumentation constraints. This study demonstrates the strong performance of an HS-SPME GC/MS/MS method for measuring volatile PFAS in bottled water. The application presents a simple, rapid, robust, precise, and accurate workflow that significantly improves the ability to detect a broader spectrum of PFAS compounds in bottled water.</p><h3><strong>3. Thermo Fisher Scientific / ASMS: Large-scale targeted biomarker analysis of volatile organic compounds in breath by TD-GC-MS&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PO_456_ASMS_25_large_scale_targeted_biomarker_analysis_po456_na_en_910bf58c57.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Breath analysis of volatile organic compounds (VOCs) is emerging as a promising tool in non-invasive disease diagnostics. While untargeted methods dominate current workflows, they often lack reproducibility and specificity. This study introduces a fully integrated, large-scale targeted workflow for VOC biomarker quantification using TD-GC-MS, aiming to support the development of Owlstone Medical’s Breath Biopsy VOC Atlas® and broader breathomics applications.</p><h4><strong>Materials and Methods</strong></h4><p>Breath samples were collected using the ReCIVA® Breath Sampler and CASPER® air supply to reduce ambient contamination. Samples were analyzed with a <strong>Markes </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=7&amp;search=TD100xr+thermal+desorber"><strong>TD100xr thermal desorber</strong></a><strong> </strong>coupled to a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/18"><strong>Thermo Scientific Orbitrap Q Exactive GC-MS system</strong></a>, known as the Breath Biopsy OMNI® method. A total of 200 VOC targets were monitored, using 36 deuterated internal standards. All data acquisition and analysis were performed in <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Chromeleon CDS software</strong></a> in a secure, cloud-based enterprise environment.</p><h4><strong>Results</strong></h4><p>The workflow includes automated system suitability and intelligent run controls (SST/IRC) to avoid the loss of valuable patient samples. High-confidence compound identification was achieved using composite scoring, ion ratio matching, and HRAM spectral libraries. Method validation across two independent breath sample cohorts demonstrated strong precision, with over 70% of VOCs meeting the &lt;20% RSD threshold across studies and sequences.</p><h4><strong>Conclusion</strong></h4><p>This targeted TD-GC-MS workflow provides a robust, compliant, and scalable solution for high-confidence breath biomarker analysis. The integration of cloud-based Chromeleon CDS, automated QC protocols, and HRAM detection supports reproducible, high-throughput studies that are essential for advancing clinical breathomics and precision medicine.</p><h3><strong>4. Waters / ASMS: GC-APCI-MS/MS Analysis of Polychlorinated Dibenzo-p-dioxins and Furans to Revised US EPA1613 Guidelines</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008849_81ffe9aec9.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In response to the U.S. EPA’s 2024 update of Method 1613 for the analysis of PCDD/Fs in wastewater, this study evaluates the performance of an alternative workflow using tandem quadrupole mass spectrometry (MS/MS) with APCI instead of traditional high-resolution mass spectrometry (HRMS). The goal was to demonstrate that such a system can meet all critical quality control (QC) metrics required by the revised method.</p><h4><strong>Materials and Methods</strong></h4><p>Analysis was carried out using a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/55"><strong>Waters Xevo TQ-XS tandem quadrupole MS</strong></a><strong> </strong>with an APGC™ source, coupled to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC"><strong>Agilent 8890 GC</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=8&amp;search=CIS-4+PTV"><strong>Gerstel CIS-4 PTV injector</strong></a>, with <strong>autosampling via </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=PAL+3+RSI"><strong>PAL 3 RSI</strong></a>. Chromatographic separation used a Restek Rtx-Dioxin2 column. Calibration standards from Wellington Laboratories were diluted to test both linearity and detection limits, and internal QC metrics were adapted to accommodate the MS/MS platform.</p><h4><strong>Results</strong></h4><p>The adapted workflow successfully replicated key EPA1613 QC checks, including relative response factors, isotopic ratios (±15%), and detection limits. The system showed excellent mass accuracy and resolution, verified through an automated Python-based script. Ionization suppression events were detected and visualized, aiding sample quality assessment. Signal-to-noise ratio evaluation, even in low-noise MS/MS traces, was possible after modifying detector settings.</p><h4><strong>Conclusion</strong></h4><p>This work proves that a GC-APCI-MS/MS system can fully comply with revised EPA1613 guidelines. The platform demonstrated robust quantitative performance, reproducibility, and reliable QC monitoring. It represents a valid and cost-effective alternative to HRMS for regulatory dioxin and furan analysis in environmental samples.</p>

News from LabRulezGCMS Library - Week 27, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 14th July 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you posters by <strong>Agilent Technologies / ASMS, Shimadzu / ASMS, </strong>presentation by<strong> Liège University / MDCW </strong>and technical note by<strong> Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Optimizing Hydrogen Carrier Gas on GC/MS Using the HydroInert EI Source and 5Q Columns&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_gc_gc_5q_columns_ei_source_asms_2025_mp_358_en_agilent_c5cf1876f0.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Hydrogen is widely recognized for its benefits in gas chromatography (GC), including cost-effective generation in the lab, rapid chromatography, and higher sample throughput. However, its reactivity can lead to hydrogenation and dechlorination reactions in the mass spectrometer electron ionization (EI) source, complicating its application in many scenarios. To address these issues, Agilent has developed a specially designed extractor source for the Inert Plus GC/MSD and triple quadrupole GC/MS systems, enhancing performance with hydrogen carrier gas. The Agilent HydroInert source maintains mass spectral fidelity and allows users to utilize existing helium-based mass spectral libraries.</p><p>This study investigates how the 5Q series of columns impact the performance and durability of the HydroInert source tune. The study involved cycling through 10,000 oven temperature ramps without any injections to assess the effects of column bleed from the 5Q phase. Furthermore, the study examined how the combination of sample matrix and column bleed from the 5Q phase affects source longevity.</p><h4><strong>Experimental</strong></h4><h5><strong>HydroInert Functionality with 5Q Columns (no Injection)&nbsp;</strong></h5><p>An experiment was designed to investigate the effects of ultra low bleed columns (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?instrumentationItems=19&amp;manufacturerItems=1&amp;search=HP-5Q"><strong>HP-5Q</strong></a>) on the functionality of the HydroInert source over time. A method simulating a large oven temperature ramp cycle (Table 1) over 12 minutes was created. The syringe was removed from the ALS tower to simulate injections, but to isolate the source of siloxanes to column bleed from the HP-5Q only. 10,000 injections were executed, and a system tune was performed every 100 injection to monitor source parameter shifts.</p><p>The Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7000E"><strong>7000E</strong></a> was run in SCAN mode, scanning from 50-450 m/z during each run. Air leaks were detected and immediately remedied when found to ensure the experiment was free from oxides. Liner and septum were not changed during this experiment.</p><h4><strong>Results and Discussion</strong></h4><h5><strong>HydroInert Functionality with 5Q Columns (no Injection)&nbsp;</strong></h5><p>Results of the effects of 10,000 oven temperature cycles on the HydroInert source tune parameters are shown in Figure 2. Repeller and ion body voltages are set automatically by the tune algorithm to maximize the transference of ion on the 7000E. Throughout the 10,000 injections the ion body voltage remained stable. The EM voltage gain across 10,000 injections was as expected. The source was in use for 120,000 minutes during this study and data was being collected throughout the duration of the study in SCAN mode. During this study, three leaks were detected at the MS transfer line and were corrected as soon as they were detected. The leaks are reflected in the spike in O2 percentage. A new ion body will typically have a voltage of 16-22 V on a HydroInert source. When an ion body begins to lose functionality the ion body voltage will begin to rise to compensate for the loss. Eventually the ion body voltage tops out at 29-30 V and the tune begins to show lower abundance of tune ions, until the source fails to tune. In the current study the ion body voltage was set by the tune algorithm between 19-24 V. This is a stable and normal operating range for the ion body. It is important to remember that a single elevated ion body tune is not cause for concern, there needs to be a trend of elevation over time. The overall purpose of this first study was to examine what baseline changes would occur to the HydroInert tune parameters when using a 5Q column in leak free conditions. Water and oxygen are known to speed the liberation of column bleed, which in turn reduces the functionality of the HydroInert source. This study shows that under leak free conditions, with a 5Q column, the HydroInert source can function optimally for an extended period. This study adds to a growing body of evidence that has demonstrated one of the main factors in HydroInert longevity is leak state of the system.</p><h4><strong>Conclusions</strong></h4><p>Agilent HydroInert source longevity is dependent on application and method conditions. However, by using the best practices highlighted above, the longevity of HydroInert parts can be prolonged. The HydroInert source cannot be mechanically or chemically cleaned, thus when source parts show reduced functionality, replacement of the recommended parts is required to restore functionality. Replacement intervals will be method and application dependent.</p><h3><strong>2. Liège University / MDCW: MOSH&amp;MOAH in food ingredients and additives and the advantages of using LC/GC×GC(-FID/TOFMS) for their analysis&nbsp;</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/FL_02_2025_MDCW_AG_MOSH_MOAH_additives_a05df36b39.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This presentation by Aleksandra Gorska and colleagues (Gembloux Agro-Bio Tech) addresses the analysis of MOSH (mineral oil saturated hydrocarbons) and MOAH (mineral oil aromatic hydrocarbons) in food ingredients and additives, particularly those derived from oils and fats. These contaminants are widespread in the food chain due to packaging, lubricants, or storage conditions. While MOSH can accumulate in human tissues, MOAH—especially those with three or more aromatic rings—pose genotoxic risks. The European Food Safety Authority (EFSA) has recently emphasized a lack of data on such impurities in food additives.</p><p>To fill this gap, the researchers developed and applied an advanced analytical workflow based on <strong>HPLC-GC×GC-FID/TOFMS</strong>, replacing the traditional HPLC-GC-FID approach. This multidimensional technique combines high-resolution separation with both flame ionization detection (FID) and time-of-flight mass spectrometry (TOFMS), allowing detailed structural characterization, efficient removal of interfering compounds, and the ability to separate MOAH by the number of aromatic rings.</p><p>Key benefits of the HPLC-GC×GC-FID/TOFMS system include clearer chromatograms with structured elution patterns, improved purification and separation of complex MOAH profiles, and identification of contamination markers such as DIPN (indicating migration from recycled packaging). Additionally, the system enables <strong>simultaneous quantification of MOAH and polycyclic aromatic hydrocarbons (PAHs)</strong>, which have distinct analytical requirements and toxicological profiles.</p><p>The study concludes that, despite its complexity, the HPLC-GC×GC-FID/TOFMS technique provides substantial analytical advantages and aligns with EFSA’s recommendations. It offers a powerful tool for ensuring food safety in products containing oil- or fat-derived additives, enabling more accurate risk assessments and source tracking of contamination.</p><h3><strong>3. Shimadzu / ASMS: Highly sensitive and efficient analysis of aroma components using trapped Headspace GC-MS&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_2025_MP_352_97902375e7.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The aroma composition of foods has been the subject of considerable research in recent years. It is well known that the presence of volatile compounds and their composition determine the specific aroma of foods and the flavor of the resulting products. Static headspace technique enables high sensitivity analysis of volatile compounds, normally extracting 1 mL of headspace. But in situations where it is necessary to evaluate the total chemical profile, it is known that components in small quantities also affect the overall aroma. Thus, the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=HS-20+NX"><strong>HS-20 NX</strong></a> was used running in "Trap mode", where by using trapped headspace sampling, it is possible to extract much more volume and analyze, not only the majority components, but all the compounds with high sensitivity.&nbsp;</p><p>The system used to achieve the highest sensitivity is the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=HS-20+NX"><strong>HS-20 NX</strong></a> coupled to the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-QP2020+NX"><strong>GCMS-QP2020 NX</strong></a> single quadrupole mass spectrometer.</p><h4><strong>Results and Discussion</strong></h4><p>After the incubation time, the acquisitions were done by loop mode and trap mode with 3- and 5-times sample concentration. In this way, it is possible to analyze, via trap, the presence of compounds at trace levels, which cannot be observed when analyzed in loop mode. 18 compounds could be identified in the sample when analyzed in loop mode, whereas in trap mode, 35 were identified.</p><p>Some components such as benzene acetaldehyde, gammacaprolactone, methyl butyrate, o-guaiacol, that have a decisive influence on the overall aroma and flavor were detected only in the trap mode, due to their low concentrations in the sample. Even concentrating the sample 5-times in the trap, it was possible to detect these compounds that require greater sensitivity along with compounds present in high concentrations in the sample, such as butanoic acid, acetic acid, and others, without losing analysis efficiency.</p><h4><strong>Conclusion</strong></h4><p>The improvement in analysis sensitivity when using trap mode can be observed when comparing the area for some components with a major impact on the overall aroma but present in small quantities. When concentrating the sample 3-times in the trap, the peak intensities increased from 351.17 to 1401.08%. And it was still possible to have a significant increase of another 168%, on average, by concentrating the sample 5-times. The peak intensities increased from 521.48 to 2517.86% compared to loop mode analysis.&nbsp;<br>These analyses demonstrate that trapped headspace can be used to determine an overall aroma profile in a single analysis and with a single trapping material. The trapped headspace sampler enables ultra sensitivity analysis, identifying compounds at low concentrations which were undetectable with conventional headspace samplers.</p><h3><strong>4. Thermo Fisher Scientific: Data-driven GC and GC-MS instrument monitoring with SmartStatus intelligent software</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/tn_001883_gc_ms_gc_ms_ms_smartstatus_tn001883_na_en_99ce72eef2/tn-001883-gc-ms-gc-ms-ms-smartstatus-tn001883-na-en.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Rising costs can significantly impact an analytical laboratory’s profit margin, and it is crucial to maintain productivity and ensure maximum asset utilization to stay competitive. To balance increased overhead costs, including analytical gases and staff pay, laboratories must ensure that analytical instrumentation consistently produces results, without interruption. Re-analyzing entire runs due to drops in sensitivity, unnecessary downtime, and underutilization of consumables is expensive and time consuming.&nbsp;</p><p>Thermo Scientific™ SmartStatus™ instrument tracking can help laboratories realize additional cost savings. This is done by using data-driven insights to accurately determine when to perform maintenance and replace consumables and parts, so that the system consistently runs smoothly for all samples and meets specifications in the initial analysis. This ensures that consumables and parts are replaced on the correct schedule and avoids excess instrument downtime.&nbsp;</p><p>SmartStatus instrument tracking is an intelligent instrument health software that allows users to track key aspects of their GC-MS system. It is available as standard on the Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/483"><strong>TRACE™ 1600 GC series,</strong></a> Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/487"><strong>AI/AS 1610 liquid autosampler</strong></a>, Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/484"><strong>ISQ™ 7610 GC-MS series</strong></a>, and the Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/485"><strong>TSQ™ 9610 GC-MS/MS series</strong></a>. In this technical note, the new SmartStatus instrument tracking capabilities are highlighted with examples of how it can enable analytical laboratories to keep instruments producing consistent results.</p><h4><strong>SmartStatus software overview&nbsp;</strong></h4><p>SmartStatus intelligent software, available within Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Chromeleon™ Chromatography Data System (CDS)</strong></a>, allows monitoring of the entire analytical system including Thermo Scientific™ autosamplers, GC, GC detectors (FID and TCD), and mass spectrometers (MS). Hundreds of key instrument parameters are monitored by SmartStatus software, which provides real-time data and insights informing the user to potential problems before they arise to ensure maximum instrument uptime. This allows users to make informed decisions on which parts of the analytical system require attention and when. By performing preventative maintenance using data-driven guidance, optimal instrument performance is sustained day in and day out. Figure 1 shows the SmartStatus software overview page for a TSQ 9610 triple quadrupole MS coupled to a TRACE 1610 GC and AI/AS 1610 liquid autosampler. This overview page allows a user to quickly determine if the system is ready to run or requires attention.&nbsp;</p><p>For more information on instrument status, there is a detailed view for each part of the system. This next level view shows how many injections have been performed for the various GC consumables, the lifetime of the MS detector and filament, and when the last tune was performed. Figure 2 shows an example of the GC and MS parameters and how they are monitored. Each parameter is represented as a counter gauge. As the usage increases, the gauge changes color to quickly notify the user of any maintenance that is required or will be needed soon. This allows users to plan maintenance in advance to fit it around their schedule and workload. SmartStatus instrument tracking can be monitored directly in Chromeleon CDS, and consumables usage can also be monitored directly on the TRACE 1610 GC touch screen through the dedicated instrument health icon, as shown in Figure 3.</p><p>The ISQ 7610 GC-MS and the TSQ 9610 GC-MS/MS detector lifetime is monitored using a predictive algorithm. This assesses the voltages on the detector and predicts the lifetime remaining on the system so that preventative maintenance can be planned. As the ISQ 7610 GC-MS and TSQ 9610 GC-MS/MS are equipped with the XLXR™ electron multiplier detector as standard, the lifetime of the detector is several years.1 By monitoring the detector intelligently, users can avoid unnecessary downtime. Figure 4 shows monitoring of the detector within SmartStatus software.</p>

News from LabRulezGCMS Library - Week 29, 2025

<p><strong>Gas Chromatography (GC) remains a cornerstone in analytical chemistry, particularly for impurity profiling, solvent quantification, and process monitoring. But as industries face increasing complexity—whether it’s trace-level detection in pharmaceuticals or quality control in fuels—the need for more selective, sensitive, and flexible detectors has never been greater.</strong></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Shedding_Light_on_Trace_Level_Impurity_Detection_in_Modern_GC_Workflows_3cde3edd45.jpg" alt="Thermo Fisher Scientific: Shedding Light on Trace-Level Impurity Detection in Modern GC Workflows." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Shedding_Light_on_Trace_Level_Impurity_Detection_in_Modern_GC_Workflows_3cde3edd45.jpg 245w," sizes="100vw" width="1200" height="600"></p><p>GC-LUMA embeds a next-generation vacuum ultraviolet (VUV) detector that bridges the gap between the universal simplicity of an FID, the selectivity of a mass spectrometer, and the robustness required for high-throughput laboratories. This article unpacks the core insights from a recent expert webinar that explored the technology, real-world applications, and data workflows behind the GC-LUMA system.</p><h3><strong>What makes GC-LUMA unique?</strong></h3><p>The GC-LUMA detector operates in the vacuum ultraviolet (VUV) region of the electromagnetic spectrum, where virtually all organic compounds absorb light. This gives LUMA its defining feature: universal detection, with high absorption sensitivity and the ability to differentiate compounds based on their spectral fingerprints.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Shedding_Light_on_Trace_Level_Impurity_Detection_in_Modern_GC_Workflows_2_3ce03ce7c3.jpg" alt="Thermo Fisher Scientific: Shedding Light on Trace-Level Impurity Detection in Modern GC Workflows: Thermo Scientific TRACE 1610 GC equipped with LUMA detector (VUV Analytics Inc.)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Shedding_Light_on_Trace_Level_Impurity_Detection_in_Modern_GC_Workflows_2_3ce03ce7c3.jpg 242w," sizes="100vw" width="1200" height="773"></p><article><div><p>Unlike traditional VUV detectors that rely on CCD sensors, LUMA uses a 12-channel photodiode array. Each channel corresponds to a specific wavelength band (from ~118 to 240 nm), offering low-ppb sensitivity. It supports stable, linear quantification via Beer’s Law and provides spectral selectivity that enables analysts to distinguish between structurally similar compounds, such as isomers. Another practical advantage is that the LUMA detector does not require a vacuum pump, simplifying the system’s footprint and maintenance requirements. As a result, GC-LUMA allows users to extract both quantitative and qualitative information in a single run, making it a powerful and versatile tool.</p><h3><strong>GC-LUMA in practice: pharmaceutical applications</strong></h3><p><a target="_blank" rel="noopener noreferrer" href="https://catsci.com/people/dr-sam-whitmarsh/">Dr.&nbsp;Sam Whitmarsh of CatSci Ltd</a>.&nbsp;presented several practical case studies from pharmaceutical process development, where GC-LUMA proved especially valuable. In early-stage synthesis projects, such as those involving valsartan routes, GC-LUMA was used for detailed impurity profiling. The detector’s capability to combine impurity, solvent, and water analysis into a single method proved especially useful, particularly when working with compounds that are not easily detected by FID, such as hydroxylamine or water.</p><p>One compelling use case involved the deconvolution of co-eluting solvents. In scenarios mimicking worst-case chromatographic conditions, LUMA successfully resolved overlapping peaks by identifying differences in their absorbance at specific VUV wavelengths. This ability significantly reduces the need for extensive method re-optimization and enables faster turnaround in process development.</p><p><i>“LUMA gives us the selectivity of a GC-MS, but with the ease-of-use of an FID. In some cases, it’s even an order of magnitude more sensitive than FID for low-carbon or polar compounds.”</i> – <i>S. Whitmarsh</i></p><h3><strong>Water by GC: a new frontier</strong></h3><p>Traditionally, water analysis by GC presents challenges. FID cannot detect water, and manual methods like Karl Fischer titration are time-consuming and prone to variability. GC-LUMA changes this dynamic by enabling water detection as part of the routine chromatographic workflow. The detector quantifies water across a wide concentration range, from parts per million (ppm) to percent levels, and demonstrates broad linearity, for example, from 20 ppm to 2%.</p><p>Using internal standards such as tetrahydrofuran (THF), GC-LUMA enhances reproducibility while allowing simultaneous analysis of water, solvents, and impurities. This capability is particularly relevant in oligonucleotide manufacturing and other pharmaceutical contexts where precise control of residual moisture and solvent levels is critical.</p><h3><strong>Smarter data with Chromeleon CDS</strong></h3><p>As explained by <a target="_blank" rel="noopener noreferrer" href="https://theorg.com/org/vuv-analytics/org-chart/rafael-acosta">Rafael Acosta, Product Manager at VUV Analytics Inc</a>., the integration of GC-LUMA with <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Thermo Scientific Chromeleon CDS</strong></a> provides a seamless data environment that enhances usability and reproducibility. With native driver integration for TRACE 1610 GC and CDS, analysts benefit from a streamlined three-step setup process that includes wavelength range selection, acquisition frequency, and channel configuration.</p><p>Chromeleon CDS further extends the power of LUMA through automatic peak purity scoring and spectral match evaluation. Users can create and manage compound libraries from reference standards and visually confirm co-elutions or potential interferences by overlaying spectral data. In one example, positional xylene isomers, which typically co-elute chromatographically, were clearly differentiated using their VUV absorbance spectra. This integration not only improves confidence in qualitative identification but also aligns with the data integrity needs of regulated environments.</p><p><i>“Chromeleon’s intuitive approach to data analysis provides a way to visualize LUMA spectra data, obtain library matching capabilities and peak purity information, which makes your method development more robust and less questionable in terms of potential coelutions.” – R. Acosta</i></p><h3><strong>All-in-one methods: a new QC paradigm</strong></h3><p>Perhaps the most compelling outcome of GC-LUMA’s flexibility is its potential to consolidate multiple quality control tests into a single analytical method. A case study involving paracetamol illustrated how GC-LUMA could be used for identity confirmation via spectral fingerprinting, assay and impurity quantification, Class 2 residual solvent detection (such as methanol and pyridine), and water determination—all within one injection.</p><p>For QA/QC laboratories, this represents a paradigm shift. By reducing the number of instruments and analytical methods required, labs can achieve greater efficiency, consistency, and throughput. It also simplifies training, documentation, and regulatory compliance.</p><p><i>“When you start to think about application in a manufacturing environment, this could be really advantageous that you’re really coalescing quite a large number of tests into one run. And that could be very effective in terms of cost and speed to release some materials and the number of pieces of equipment that you’d need to have up and running to do that” – S. Whitmarsh</i></p><h3><strong>Filling the analytical gaps</strong></h3><p>GC-LUMA doesn’t aim to replace FID or MS. Rather, it complements them by occupying a unique space in the GC detector landscape. It offers the universality of a TCD, the selectivity of an MS, and the ease of use of an FID—but with enhanced sensitivity and spectral capability. Ideal for routine labs, process development teams, and regulated QC environments, GC-LUMA delivers more than just data: it delivers clarity, confidence, and actionable insight.</p><p>With its spectral power, method simplicity, and seamless data integration, GC-LUMA provides a compelling new option for analysts seeking to elevate their GC workflows and make better-informed decisions based on richer, more reliable information.</p><blockquote><p><strong>Want to learn more?</strong> Watch the full webinar available on-demand <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5325"><strong>Shedding Light on GC‑LUMA: Revolutionizing Trace Level Impurities Detection</strong></a>, or explore technical resources at <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/chromatography/gas-chromatography-gc/gc-systems/related-products/vuv-detector.html">VUV Detector for TRACE 1600 Series GC</a></p><p><strong>Visit us on&nbsp;</strong><a target="_blank" rel="noopener noreferrer" href="https://www.linkedin.com/showcase/72003132/admin/dashboard/"><strong>LinkedIn:</strong></a><strong>&nbsp;</strong>#TRACE1610 #ImpurityAnalysis #GCInnovation #PharmaQAQC</p></blockquote></div></article><section><blockquote><h4><strong>Dr. Daniela Cavagnino</strong></h4><p>Dr. Daniela Cavagnino is Product Marketing Manager for GC and Sampling Solutions. She started her career in gas chromatography at Thermo Fisher Scientific spending several years in the R&amp;D laboratories working on GC technology innovation. Then, she conveyed her technical background into product management and marketing management roles with more than 20 years’ experience in promoting GC/GCMS technology and applications in several different market segments.</p></blockquote></section>

Shedding Light on Trace-Level Impurity Detection in Modern GC Workflows

<p><strong>Many elements, such as chromium, zinc or selenium are considered essential micronutrients for humans and are subject to ongoing research. Their concentration in foods can be accurately determined using inductively coupled plasma mass spectrometry (ICP-MS).</strong></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Deciphering_Selenium_Nutrition_Using_Speciation_Analysis_with_ICP_MS_3ecef88508.jpg" alt="Thermo Fisher Scientific: Deciphering Selenium Nutrition Using Speciation Analysis with ICP-MS" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Deciphering_Selenium_Nutrition_Using_Speciation_Analysis_with_ICP_MS_3ecef88508.jpg 245w," sizes="100vw" width="1200" height="600"></p><article><div><p>However, beyond the actual levels of an element in a sample, <strong>the precise chemical form in which it is present is important</strong>. Trace elements may occur in different oxidation states (for example, <strong>essential Cr (III) and its carcinogenic counterpart Cr (VI)</strong>) or may be found incorporated into organic molecules. This may lead to significantly different results when assessing potential hazards from a sample with respect to toxicity. For example, <strong>fruit juices such as apple juice may only contain 10 µg∙L<sup>-1 </sup>of arsenic</strong>, as it is mostly found as inorganic arsenic, whereas <strong>fish and seafood can be safely consumed even though they may contain total concentrations 1000-fold higher</strong>, as arsenic is commonly found in organic forms. The qualitative and/or quantitative determination of different chemical forms of an analyte in a sample is often referred to as <strong>speciation analysis</strong>.</p><p>Prof. Dr. Marc Birringer, Alexander Maxones and Simon Glas from the University of Applied Science in Fulda, Germany, working at the department for nutritional, food and consumer sciences, explore the importance of <strong>selenium (Se) in foods</strong>, leveraging speciation analysis to assess different selenium species for their <strong>bioavailability</strong>.<i> “The journey on selenium species started in the 1990s”</i>, says Prof. Birringer, <i>“when people started to understand why selenium is important for biochemistry and nutrition. When we started with ICP-MS as a new technique in our lab, we learned that this technique can really give us a lot of information in single and multi-element analysis, and we planned to perform speciation analysis, too.”</i></p><p><strong>Selenium is an essential trace element</strong> that is low in abundance in Germany. Important sources for this essential trace element are <strong>fish, meat or eggs</strong>. Because these foods are not part of a vegetarian’s or vegan’s diet, they are particularly susceptible to the potential risk of malnutrition. <strong>Mushrooms, in particular porcini mushroom (boletus edulis), could be an alternative source</strong> when meat or fish are not part of the diet based on an individual’s choice. One compound that is particularly abundant is <strong>selenoneine, a derivative of ergothioneine</strong>, where a selenium atom replaces a sulfur atom.</p><p>Whereas there are a lot of chromatographic methods established to separate other water-soluble selenium compounds, like inorganic selenium (Se (IV) and Se (VI)), methods allowing separation of <strong>organic selenium compounds like selenoneine are more difficult to optimize when ICP-MS is used</strong> as an element-specific detection system. <strong>Separation based on hydrophilic interaction chromatography (HILIC)</strong> typically start with high amounts of organic solvents in the mobile phase, which require the ICP-MS to be equipped accordingly., i.e. <strong>oxygen addition to the plasma and platinum tipped cones</strong>.</p><p><a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/chromatography/ion-chromatography-ic.html"><strong>Ion chromatography (IC)</strong></a> is well known for its ability to separate charged ions or polarizable species and is often the technique of choice for speciation analysis of elements such as arsenic or selenium. Typical IC systems, such as the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/410"><strong>Thermo Scientific Dionex ICS-6000 Ion Chromatography systems,</strong></a> are fully inert and can therefore leverage eluents with very high or low pH values. &nbsp;&nbsp;&nbsp;</p><p><i>“We have an ICS-6000 HPIC in the laboratory, but that system is usually blocked for other assays. However, the </i><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products?category=39&amp;search=Vanquish"><i><strong>Thermo Scientific Vanquish HPLC</strong></i></a><i> was also compatible with the mobile phase we used, which was at pH 2</i>”, says Prof. Birringer. “<i>This system was used for the separation with a </i><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2076"><i><strong>Thermo Scientific Dionex IonPac CS12 column</strong></i></a><i>.&nbsp; This allowed good separation for the organic compounds containing selenium, even though the separation of the inorganic and ionic species was not ideal under these conditions</i>.”</p><p>During method development, it was very important to also monitor sulfur, as there is no standard available for selenoneine and instead, the sulfur-containing analog ergothioneine was used. For both elements, the use of a triple quadrupole ICP-MS system such as the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1488"><strong>Thermo Scientific iCAP MTX ICP-MS</strong></a> provides significant advantages. Both elements are potentially biased by polyatomic interferences (especially the most abundant isotopes <sup>32</sup>S and <sup>80</sup>Se), which can be efficiently reduced using oxygen as a reactive gas.</p><p>“<i>What we found in the boletus edulis was a lot of compounds that we did not know before or could at least not explain as we have no mass spectra to confirm structures, but we do have the ICP-MS data</i>”. They must be present in low concentrations and would likely be found in the noise in a normal LC-MS run states Prof. Birringer.</p><p>Coupling of the two systems is straightforward. When water-based eluents are applied, the outlet of the column can be directly connected to the nebulizer of the ICP-MS system using narrow bore tubing and a zero dead volume connector. &nbsp;“I´m really comfortable with the system, and I think it gives us a lot of possibilities” says Alexander Maxones. “<i>I would like to explore other column options for future projects, as I think smaller particles would be beneficial for further separation of species</i>”, he adds.</p><p>For data evaluation, <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/76"><strong>Thermo Scientific Chromelon CDS software</strong></a> was used, as it provides more options for peak integration and smoothing of raw data, if needed. The original data collected on the ICP-MS can be directly imported into Chromeleon CDS software.</p><p>“<i>The methodology developed can now be applied to a wider range of samples. We have found at least five unknown compounds in boletus edulis, but it is clear from the literature that other mushrooms, for example shiitake, can also accumulate some selenium. We are sure they have similar but also different compounds to be investigated</i>”, says Prof. Birringer. Next is additional food matrices, but also human samples.</p><blockquote><ul><li>For more information, please visit the<strong> </strong><a target="_blank" rel="noopener noreferrer" href="https://www.hs-fulda.de/oecotrophologie/labore/analytik"><strong>laboratory´s website</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/mass-spectrometry/inductively-coupled-plasma-mass-spectrometry-icp-ms/quadrupole-icp-ms-systems.html"><ins><strong>Quadrupole ICP-MS Systems</strong></ins></a>.</li><li><strong>Visit us on&nbsp;</strong><a target="_blank" rel="noopener noreferrer" href="https://www.linkedin.com/showcase/72003132/admin/dashboard/"><strong>LinkedIn:</strong></a>&nbsp;#ICP-MS</li></ul></blockquote></div></article><section><blockquote><h4><strong>Daniel Kutscher</strong></h4><p>Dr. Daniel Kutscher manages the Application Development for trace elemental analysis and GC/GC-MS products at the Thermo Fisher Scientific Center of Excellence in Mass Spectrometry in Bremen, Germany. After graduation in Chemistry in 2007, Daniel obtained his PhD from the University of Oviedo in 2011. In the same year, he joined Thermo Fisher Scientific and has had different roles in application development and marketing.</p></blockquote></section>

Deciphering Selenium Nutrition Using Speciation Analysis with ICP-MS

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 18th August 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies </strong>and <strong>Waters Corporation</strong> and technical notes by<strong> Shimadzu </strong>and <strong>Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies: Deciphering the Microbiome: Targeted LC/MS/MS Analysis of Bile Acids in Biological Samples</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_deciphering_microbiome_bile_acids_samples_5994_8263en_agilent_dc02f26cab.pdf"><strong>Full PDF for download</strong></a></li></ul><p>BA analysis using liquid chromatography-mass spectrometry (LC/MS) is both critical and challenging due to the inherent complexity of bile acids. These compounds encompass a wide range of structurally similar and isomeric species that often exhibit nearly identical mass-to-charge ratios (m/z) and retention times. This similarity makes achieving baseline separation and accurate identification particularly difficult.&nbsp;</p><p>Additionally, bile acids are relatively stable molecules that do not typically undergo extensive fragmentation in a mass&nbsp;spectrometer. Additionally, the more challenging fragmentation complicates the differentiation of isomeric bile acids emphasizing the need for a standardized method also leveraging retention times.&nbsp;</p><p>Compounding these issues, many of the microbiota-produced bile acid species are typically present at low concentrations in biological samples, which often contain matrix components that can lead to ion suppression or enhancement. These matrix effects can interfere with accurate quantification, further complicating the analysis. Moreover, the need for high sensitivity and specificity to distinguish closely related bile acid species adds another layer of complexity.&nbsp;</p><p>To address these challenges, standardized and highly optimized chromatographic methods, advanced mass spectrometric techniques, and robust sample preparation protocols are essential. Together, these strategies enhance the reliability of BA analysis, enabling accurate profiling for both research and clinical research applications.&nbsp;</p><p>A previously described LC/TQ method was used to analyze 26&nbsp;bile acids.1 This present study introduces a new method using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6495D+LC%2FTQ"><strong>6495D LC/TQ</strong></a> with fourth-generation ion funnel technology, which improves sensitivity and expands the scope for the analysis of 68 unique bile acids in complex matrix. This bile acid method is compatible and consistent with the Agilent Standardized LC/MS platform for omics analysis and is easily transferable in the laboratory and therefore suitable for rapid delivery of new insights.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><p>The LC/MS platform consisted of a 6495D triple quadrupole mass spectrometer with fourth-generation iFunnel technology, coupled with an Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity+II+Bio+LC"><strong>1290 Infinity II Bio LC</strong></a> system with the Agilent standardized configuration for omics applications. The acquisition method is fully compatible with an Agilent 6495C model and a regular stainless‑steel Agilent 1290 Infinity II LC with the same standard omics&nbsp;configuration. All methods using the Infinity II LC systems are fully compatible with Infinity III LC systems and give identical method performance.&nbsp;</p><h5><strong>Software&nbsp;</strong></h5><p>MS data were acquired using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+acquisition+software"><strong>MassHunter acquisition software</strong></a> 12.1, which includes built-in source and compound optimizer tools for method development. Agilent&nbsp;<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Qualitative+Analysis"><strong>MassHunter Qualitative Analysis</strong></a> 12.0 software was used to visualize the acquired dataset and assess data quality before&nbsp;quantification.&nbsp;</p><p>Bile acid levels from the LC/MS/MS datasets were quantified using MassHunter Quantitative Analysis 12.0 software. Quantitation methods for both relative and absolute measurements were developed using one of the quality control (QC) injections. Statistical analysis was performed with Agilent&nbsp;Mass Profiler Professional (MPP) 15.1.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A robust and standardized targeted dynamic-MRM LC/MS/MS method for the analysis of bile acids was developed on an Agilent 6495D triple quadrupole/LC platform. Optimal bile acid extraction conditions from plasma and fecal samples were established along with LC/MS conditions that allowed the measurement of a large panel of bile acids in a single chromatographic run. This analytical method is highly versatile and applicable to both plasma/serum and fecal samples, offering valuable insights into systemic and gut-specific bile acid profiles. In plasma, it provides a reliable means to assess circulating bile acids, which are key indicators of liver function, metabolic health, and disease states. In fecal samples, the method enables detailed profiling of bile acids involved in gut microbiota interactions and intestinal health, shedding light on digestion and enterohepatic circulation dynamics.</p><h3><strong>2. Shimadzu: Enhancing Selectivity in Reversed-Phase Analysis Through Effective Utilization of Mobile Phase pH</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c190_e335_442eed699a.pdf"><strong>Full PDF for download</strong></a></li></ul><p>When analyzing ionizable compounds, the pH of the mobile phase plays a crucial role in improving peak shape and separation. However, conventional silica-based columns have limitations in utilizing high-pH mobile phases. Additionally, while polymer-based columns can operate across a wide pH range, they have drawbacks such as lower mechanical strength and column efficiency. In this technical report, we present examples of measurements conducted using mobile phases with various pH levels, employing the Shim-pack Scepter and <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Shim-pack+NovaCore+columns"><strong>Shim-pack NovaCore columns</strong></a>—organic silica hybrid columns that combine the advantages of silica-based columns with exceptional high-pH durability.</p><h4><strong>2. The Relationship Between Compound Ionization and Mobile Phase pH</strong></h4><p>Figure 1 shows the relationship between the pKa of the compound and the pH of the mobile phase. The horizontal axis represents the value obtained by subtracting the pKa of the compound from the pH of the mobile phase. In general, the ionization ratio of weakly acidic compounds is known to become 1 % (nearly neutral) when the pH is 2 below their pKa. Conversely, when the pH is 2 above the pKa, the ionization ratio becomes 99 % (nearly ionized). On the other hand, weakly basic compounds are known to ionize 99 % (nearly ionized) when the pH is 2 below their pKa. Conversely, when the pH is 2 above the pKa, the ionization ratio becomes 1 % (nearly neutral).</p><h4><strong>3. Suppression of Ionization in Basic Compounds&nbsp;</strong></h4><p>In the case of basic compounds, the pH of the mobile phase must be high in order to suppress ionization. However, in general, traditional silica-based columns such as C18 with silica gel as the base particle may begin to disintegrate when the pH exceeds 7, so a high-pH mobile phase may not be usable. On the other hand, polymer-based particles have the advantage of being usable over a wide pH range from 1~14, but their mechanical strength and separation efficiency are lower than silica-based columns. Therefore, it is ideal to have a column that combines the advantages of silica-based and polymer-based packing material. The Shim-pack Scepter and Shim-pack NovaCore meet these needs (see Table 1).</p><h4><strong>4. Organic Silica Hybrid Columns in the Shim-pack Series&nbsp;</strong></h4><p>The fully porous Shim-pack Scepter and the core-shell Shim-pack NovaCore columns use organic silica hybrid material for the base particles to maintain the high physical strength of traditional silicabased columns while significantly improving their durability under high pH conditions. Figure 2 shows the change in column performance when a high-pH mobile phase is delivered for an extended period. This confirms the high pH durability of Shim-pack Scepter and Shimpack NovaCore compared to column A, a traditional silica-based column.</p><h3><strong>3. Thermo Fisher Scientific: Configuring a combustion-ion chromatography system using a complete workflow&nbsp;</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/tn_003773_ic_ic_systems_Combustion_IC_System_environmental_tn003773_na_en_v9_358da61ec1.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Analyzing samples with complex matrices can be challenging due to the incompatibility of the sample’s physical properties with the analytical technique. For example, ionic halide content can only be measured by ion chromatography (IC) when the sample is fully dissolved in a liquid, preferably water, extracted, or washed off the surface of a solid material. Combustion-ion chromatography (C-IC) has the advantage of eliminating complex sample matrices to directly measure the total halogens and total sulfur.<sup>1-5</sup> C-IC has been demonstrated for halide determinations in other challenging liquid matrices, such as tea and wastewater.<sup>6,7</sup> In addition, adsorbable organic fluorine (AOF), in conjunction with C-IC, has been demonstrated and incorporated into U.S. EPA Method 1621 to screen for perand polyfluoroalkyl substances (PFAS) in water samples.<sup>8-14&nbsp;</sup></p><p>A new C-IC total workflow system has been introduced: the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2150"><strong>Thermo Scientific™ Cindion™ Combustion Ion Chromatography System</strong></a>. It includes a standalone sample preparation module, the Thermo Scientific™ Cindion™ Combustion/Absorption Module, and an autosampler that can be configured for solid or liquid samples. A standalone Thermo Scientific™ Cindion™ LPG/gas Module is also an option.&nbsp;</p><p>In this technical note, we describe the configuration and operation of the Cindion C-IC system with the following configurations: Cindion combustion/absorption Module with Cindion autosampler and each of numbers 1-4 below.&nbsp;</p><ol><li>Solids sampler and with the offline Cindion adsorption module needed for U.S. EPA Method 162115&nbsp;</li><li>Solids sampler&nbsp;</li><li>Liquids sampler&nbsp;</li><li>Eluent monitor with any configuration</li></ol><h4><strong>Instruments&nbsp;</strong></h4><h5><strong>Cindion C-IC system:&nbsp;</strong></h5><ul><li>Cindion combustion/absorption module (P/N B51006425) with Thermo Scientific™ Cindion™ C-IC Solids Kit (P/N B51006427)&nbsp;</li><li>Thermo Scientific™ Cindion™ Solids/Liquids Autosampler (P/N B51006429)&nbsp;</li><li>Thermo Scientific™ Cindion™ Adsorption Module (P/N B51006430) that includes 6 column holders&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1078"><strong>Thermo Scientific™ Dionex™ Inuvion™ </strong></a>with Reagent-free Ion Chromatography (RFIC™) System (P/N 22185-60108)&nbsp;</li><li>Optional Thermo Scientific™ Dionex™ Inuvion™ Eluent Monitor, 4 L (P/N 22185-62708)&nbsp;</li><li>Thermo Scientific™ Muffle Furnace, 2 L small bench top, to clean combustion cups, (Thermo Scientific FB1415M, Fisher Scientific 10-552) – recommended for U.S. EPA Method 1621</li></ul><h5><strong>Software&nbsp;</strong></h5><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/76"><strong>Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)</strong></a>, version 7.3.2 MUd with Cindion C-IC and eluent monitor drivers.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This technical note provides comprehensive guidance on configuring and operating the full Cindion C-IC system workflow. The system offers a complete workflow, starting from offline sample preparation for AOX analysis, progressing through combustion and absorption, and concluding with IC analysis. It includes an autosampler for solids and liquids, along with an optional module for compressed and liquefied gases, ensuring versatility in sample handling. The Z-fold combustion tube is designed to introduce oxygen at multiple points and create an extended flow path that enhances combustion efficiency while minimizing length. To minimize devitrification, the system introduces water only during combustion. Additionally, Chromeleon CDS seamlessly controls Cindion C-IC system operation and data processing.</p><h3><strong>4. Waters Corporation: Slalom-Aided Anion Exchange Chromatography for Enhanced Analysis of Plasmid DNA Topological Impurities</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008928_en_7fae99acf4.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>Benefits&nbsp;</strong></h4><ul><li>Baseline resolution of DNA isoforms achieves complete separation of supercoiled, open circular, and linear forms of pBR322, ΦX174 RFI/RFII, and Cas9 plasmid</li><li>Dual mode retention mechanism demonstrates separation driven by both anion exchange and flowdependent slalom chromatography mechanisms</li><li>Single method offers broad applicability using a single gradient method on the Protein-Pak Hi Res Q Column to analyze diverse nucleic acid structures with flow rate optimization to achieve desired selectivity through slalom effects</li></ul><p>In the present study, for the first time, the synergy between traditional AEX and slalom retention mechanisms using a Protein-Pak Hi Res Q Column has been systematically investigated. More specifically, two experimental variables have been purposely manipulated to optimize the separation of 3 unique plasmids. The salt gradients (for AEX selectivity) and shear force-inducing flow rates were adjusted to optimize the slalom-based selectivity of the separations. The dual-mode AEX–slalom separation was evaluated and optimized for three biologically relevant DNA constructs: ΦX174 RF I/II (5.4 kbp), pBR322 (4.4 kbp), and a 7.0 kbp Cas9-encoding plasmid. Using defined mobile phase conditions consisting of Tris buffer with 5% urea and a precisely controlled sodium chloride (NaCl) gradient, flow-rate-dependent resolution of OC, L, and SC topological forms was observed. The resulting data elucidates key operational parameters that can be leveraged to significantly enhance resolution, method reproducibility, and scalability, ultimately achieving a powerful analytical approach tailored for emerging gene therapy applications.</p><h4><strong>Experimental</strong></h4><h5><strong>LC Conditions</strong></h5><p><strong>LC system:&nbsp;</strong></p><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY™ Premier System</strong></a> with:</li><li>Binary Solvent Manager (BSM, p/n: 186018000)</li><li>Flow-Through Needle Sample Manager (SMFTN, p/n: 186018002)</li><li>Column Manager-A (CM-A, p/n: 186018003)&nbsp;</li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>This application note demonstrates the utility of Protein-Pak Hi Res Q Column and strong anion-exchange chromatography for resolving the three plasmid DNA isoforms, supercoiled (SC), open circular (OC), and linear (L), across a wide range of DNA sizes, including pBR322 (4.361 kbp), ΦX174 RF I/II (5.386 kbp), and the pCMVCas9 (7.037 kbp) plasmid. Using a mobile phase system containing 5% urea and a NaCl gradient, the method achieved excellent resolution of all topological forms by tuning the flow rate applied throughout the gradient method. Notably, this strategy offers a streamlined alternative to traditional method development approaches that require manual changes in mobile phase additives or compositions. Indeed, flow rate was found to influence resolution significantly due to the difference in entropic elasticity of DNA plasmid (open-circular, supercoiled) and linear isoforms. For example, optimum flow rates were found to be equal to 0.8, 0.5, and 0.3 mL/min for the separation of pBR322, ΦX174 RFI RFII Mixture, and pCMV-Cas9 plasmids, respectively. Higher flow rates are needed to increase the retention of shorter linear DNA isoforms relative to the open circular plasmid. These results highlight the method’s adaptability and precision for analyzing plasmid topology, providing analysts with enhanced control critical for assessing identity, integrity, and purity in plasmid-based therapeutics and gene therapy workflows.</p>

News from LabRulezLCMS Library - Week 34, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 22nd September 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies, Shimadzu </strong>and <strong>Waters Corporation </strong>and<strong> </strong>poster by <strong>Thermo Fisher Scientific / HPLC Symposium!</strong></p><h3><strong>1. Agilent Technologies: Quantitation of N-Nitroso Nebivolol in Nebivolol Tablet Formulation</strong></h3><p><strong>Using an </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6495D+triple+quadrupole"><strong>Agilent 6495D triple quadrupole LC/MS system</strong></a></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_nebivolol_tablet_formulation_6495_qqq_lc_ms_system_5994_8053en_agilent_e7f21eb12f.pdf"><strong>Full PDF for download</strong></a></li></ul><p>N-Nitroso Nebivolol is a NDSRI of Nebivolol, a beta-1 adrenergic receptor antagonist commonly used in the treatment of hypertension and heart failure. In the carcinogenic potency categorization published by the FDA, N-Nitroso Nebivolol has been categorized as Class 4, indicating the maximum allowable intake limit for the impurity to be 1,500 ng/day. Nebivolol has maximum daily dosage limit of 40&nbsp;mg for adults.</p><p>Considering a maximum daily dose of 40&nbsp;mg and allowable intake of 1,500&nbsp;ng/day for the nitrosamine impurity in the formulation under study, the specification limit of N-Nitroso Nebivolol has been calculated as 22.5 ng/mL for the 0.6 mg/mL test concentration used during this study.&nbsp;</p><p>This application note demonstrates a highly specific, sensitive, and reproducible method for the quantitation of N-Nitroso Nebivolol in a 20 mg Nebivolol tablet formulation. The method uses a 1290 Infinity II LC coupled to a 6495D triple quadrupole LC/MS/MS. The multiple reaction monitoring (MRM) conditions and ion source parameters were automatically optimized using the optimizer tool available with MassHunter Acquisition software to maximize the sensitivity of the target analyte. The API peaks were diverted to waste with the help of an integrated, software-controlled diverter valve during quantitation of the&nbsp;impurity.</p><h4><strong>Experimental</strong></h4><h5><strong>Equipment&nbsp;</strong></h5><p>The analysis was performed on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity+II+LC"><strong>1290 Infinity II LC system</strong></a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6495D+triple+quadrupole"><strong>6495D triple quadrupole LC/MS/ MS</strong></a>. The LC system was equipped with the following&nbsp;modules: – Agilent 1290 Infinity II high-speed pump (G7120A) – Agilent 1290 Infinity II multisampler (G7167B) – Agilent 1290 Infinity II multicolumn thermostat (G7116B) – Agilent 1290 Infinity II diode array detector (G7117A)</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A highly sensitive and robust MRM method was developed for the quantitation of N-Nitroso Nebivolol in 20&nbsp;mg Nebivolol tablet formulation using an Agilent 6495D triple quadrupole LC/MS system. The chromatographic method developed provided good separation between the analyte and the API. The method showed LOD and LOQ of 2 and 5 pg/mL, respectively. The minimum signal-to-noise ratio at the LOQ level was found to be more than 50:1 (Peak to Peak). The calibration curve from 5 pg/mL to 50&nbsp;ng/mL was found to be linear, with 1/x weighting. R and R2 values were 0.999 and 0.997, respectively. Spike recovery analysis showed the efficiency of sample extraction with a recovery percentage of 116.8% in API, 108.3% in placebo, and 111.8% in tablet formulation at the spiking level of 200 pg/mL. The method was found to be highly reproducible at the LOQ level, while the %RSD value for the area response of seven replicate injections was approximately 3.1%.</p><h3><strong>2. Shimadzu: Efficient Method Development for Synthetic Peptide and Related Impurities</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00780_en_4d0aa014ea.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>LabSolutions MD improves the efficiency of the entire workflow for method development of synthetic peptide and impurities.&nbsp;</li><li>Screening for multiple mobile phases and columns can be automated using mobile phase and column switching valves.&nbsp;</li><li>Molecular weights of peptides and related impurities can be estimated and accurately tracked with LCMS-2050, a single quadrupole mass spectrometer.</li></ul><p>Peptide therapeutics, characterized by specific amino acid sequences crucial to their function, can be synthesized chemically, similar to small molecule drugs. The production of synthetic peptides involves multiple steps, including deprotection, activation, coupling, and the cleavage of the final sequence from the solid support. Impurities, such as those resulting from premature chain termination or missing amino acids, can affect the safety and efficacy of the final product. Therefore, these impurities must be separated by liquid chromatography (LC). In LC analysis, selecting the appropriate mobile phase and column across a wide range of combinations is critical for achieving optimal separation, as it significantly impacts the separation. However, since the separation pattern varies depending on the peptide chain lengths, amino acid compositions, and presence of modifications, optimizing separation for each peptide sequence is time-intensive. This study describes how to efficiently find the best separation conditions for peptides and related impurities utilizing LabSolutions MD, a dedicated software for supporting method development, through both screening and optimization phases.</p><h4><strong>Experimental</strong></h4><ul><li><strong>LC System: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+X3"><strong>Nexera X3</strong></a> (Method Scouting System)</li><li><strong>MS System: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-2050"><strong>LCMS-2050</strong></a></li></ul><h4><strong>Automated Peak Tracking by LCMS-2050&nbsp;</strong></h4><p>LC chromatograms obtained with a gradient time of 5 min, flow rate of 0.6 mL/min, and initial concentration of 5 % and 15 %, along with molecular weights for FLP and impurities, are shown in Fig. 18. The UV spectra for each impurity are displayed in Fig. 19. The similarity between UV spectra of Met(O2), p.A1del, p.A1_E2del, p.A1_K3del, and p.A1_D5del is greater than 0.99, suggesting that peak tracking based on UV spectra would be challenging. In contrast, LabSolutions MD enables peak tracking based on molecular weights acquired by LCMS-2050, facilitating accurate identification of compounds with similar UV spectra (Fig. 18). The estimated molecular weights for each compound show small mass errors compared to the theoretical values (Table 3), which can be used to confirm the molecular weights of known compounds as well as to approximate the molecular weights of unknown impurities.</p><h4><strong>Conclusion</strong></h4><p>The separation patterns of synthetic peptides vary depending on mobile phase composition, column type, and various LC parameters, such as gradient conditions, column oven temperature, and flow rate. Separation behavior can also differ based on peptide structure, including length, amino acid composition, and the presence of modifications. Therefore, it is necessary to optimize the separation for each peptide sequence individually. However, optimizing analytical conditions through numerous analyses and data processing can be time-consuming. LabSolutions MD automates the entire workflow, including generating analysis schedules, preparing mobile phases, and processing the data, thanks to functionalities such as automated peak tracking, ranking of chromatograms, and design space visualization. This article introduced a case where the optimal separation conditions for synthetic peptides were efficiently identified through screening and optimization phases. LabSolutions MD also offers fully automated gradient optimization by AI algorithm to meet user-defined criteria. For more details, please refer to the application news, “Automatic Optimization of Gradient Conditions by AI Algorithm on Synthetic Peptide and Impurities: 01-00814”.</p><h3><strong>3. Thermo Fisher Scientific / HPLC Symposium: Sensitive cationic lipids impurities analysis with quantitation by charged aerosol detection and simultaneous mass confirmation by MS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_sensitive_cationic_lipids_impurities_analysis_quantitation_po_en_3dacf61554.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Cationic lipid is a critical component in lipid nanoparticle formulations for delivering nucleic acids such as mRNA, siRNA, antisense oligonucleotides etc. [2] Cationic lipids are amphiphilic molecules that possess a hydrophilic region, a hydrophobic region, and a linker structure connecting the two. [1] Charged aerosol detector (CAD) and evaporative light scattering detectors (ELSD) are preferred for characterizing lipid nanoparticle components, with CAD being the better choice for impurity quantification due to its higher sensitivity [3]. In a previous study, an inverse gradient method was developed to quantify impurities in cationic lipids raw materials.[1] To demonstrate the inverse gradient method on CAD HP, the same cationic lipids -- R-DOTAP, DLin-KC2- DMA and ALC-0315 -- were measured to this experiment as in Application note 003384 [1]. New diverter valve and software features were showcased, along with method’s sensitivity and repeatability.</p><h4><strong>Materials and methods</strong></h4><p>Using the inverse gradient method from Application note 003384 [1], to demonstrate impurity analysis in cationic lipids on the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2176"><strong>Thermo Scientific Vanquish Charged Aerosol Detector HP (CAD HP)</strong></a> integrated in the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/743"><strong>Thermo Scientific Vanquish Flex Inverse Gradient UHPLC System</strong></a>, with parallel mass confirmation by the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/413"><strong>Thermo Scientific ISQ EM Single Quadrupole Mass Spectrometer</strong></a>.&nbsp;</p><p><strong>Methods:</strong> The workflow uses a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/743"><strong>Vanquish Flex Inverse Gradient LC system</strong></a> with Vanquish CAD HP and <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1970"><strong>Thermo Scientific Hypersil GOLD C8 column</strong></a>.</p><h5><strong>Data Analysis&nbsp;</strong></h5><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/76"><strong>Thermo Scientific Chromeleon Chromatography Data System (CDS)</strong></a> 7.2.10 was used for data acquisition and analysis.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>The CAD HP integrates perfectly into the Vanquish Inverse Gradient LC system and offers high sensitivity and excellent repeatability for quantitative cationic lipid impurity analysis, while the ISQ EM MS provides straightforward mass confirmation with high repeatability, all under compliance-ready conditions.</p><h3><strong>4. Waters Corporation: Quantitative Analysis of Four Long-Chain Lysophosphatidylcholines (LPCs) in Dried Blood Spot using Liquid Chromatography Tandem Mass Spectrometry for Clinical Research</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008826_en_dc154872b6.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>Benefits</strong></h5><ul><li>Good chromatographic resolution of all forms</li><li>Short extraction time compared to traditional methods for lipid extraction</li><li>Short analysis injection-to-injection 7 minutes</li></ul><p>Historically, very long chain fatty acids have been quantified using direct transesterification and gas chromatography methods which involve time-consuming and labor-intensive sample preparation and analysis. Consequently, simpler LC-MS/MS methods have been reported for the measurement of long-chain LPCs (LPCs generic chemical structure, Figure 1) in DBS. Interferences have been reported using positive ESI, thus researchers have developed methodologies utilizing negative ESI to circumvent isobaric interferences when there is lack of chromatographic resolution. Here a UHPLC-MS/MS method is described using acetate adducts for the reliable analysis of four long-chain LPCs in DBS for clinical research.&nbsp;</p><p>A UHPLC-MS/MS method for quantifying a panel of LPCs (C20:0, C22:0, C24:0, and C26:0-LPCs) was developed. The mobile phase composition consisted of a mixture of water, acetonitrile, and isopropanol with 5 mM ammonium acetate as a modifier. The DBS sample extraction used a working solution prepared with the deuterated LPC internal standards in methanol. The method was developed with an ACQUITY UPLC I-Class PLUS System (Fixed Loop) using an ACQUITY Premier CSH C18 Column, which provided baseline resolution of endogenous isobaric interferences for the saturated forms of the targeted LPCs. The detector was a Xevo TQ-S micro Mass Spectrometer operated in negative ESI mode. This methodology resulted in a total analysis time (injection-to-injection) of 7 minutes.</p><h5><strong>LC Conditions&nbsp;</strong></h5><ul><li><strong>LC system: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/199"><strong>ACQUITY UPLC I-Class PLUS FL&nbsp;</strong></a></li><li><strong>System Detection: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/209"><strong>Xevo TQ-S micro Mass Spectrometer&nbsp;</strong></a></li><li><strong>Plate:</strong> Waters 96-well Sample Collection Plate, 350 µL&nbsp;</li><li><strong>Column(s): </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1952"><strong>ACQUITY Premier CSH C18 Column</strong></a>, 2.1 mm x 50 mm, 1.7 µm (p/n: 186009460)</li></ul><h5><strong>MS Conditions&nbsp;</strong></h5><ul><li><strong>MS system:</strong> Xevo TQ-S micro Mass Spectrometer</li></ul><h5><strong>Data Management&nbsp;</strong></h5><ul><li><strong>MS software: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/635"><strong>MassLynx™ v4.2 Software SCN 1045&nbsp;</strong></a></li><li><strong>Informatics: </strong>TargetLynx™ XS v4.2 Software SCN1045 and QUAN Review</li></ul><h4><strong>Results and Discussion&nbsp;</strong></h4><p>During method development, different types of column chemistry, mobile phase composition, and ESI polarity modes were assessed to optimize chromatographic peak shape, analytical sensitivity and manage interferences. In positive mode, ammonium formate favored the formation of m/z 184 and m/z 104 as daughter ions for all the LPCs. The m/z 184 ion lacks specificity because most phospholipids share this moiety, so the ion m/z 104 was selected as quantifier. Having evaluated conditions in positive mode for the analysis of the four saturated LPCs, it was observed that some existing interferences were not only affecting the parent masses of the analytes but their corresponding internal standard parent ion masses too. Hence, negative ionization using ammonium acetate as modifier was assessed for the detection of LPCs. Acetate adducts [M+CH3COO]- were the most abundant parent ion masses, generated under these conditions for each LPC. The acyl-chain product ions generated in negative ionization reduce the detection of interferences coming from other phosphocholine headgroups. The latter detection conditions were used for the validation of the method presented herein.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>An LC-MS/MS clinical research method for measuring C20:0, C22:0, C24:0, and C26:0 LPCs with the ACQUITY UPLC I-Class PLUS FL System, and the Xevo TQ-S micro Mass Spectrometer that:</p><ul><li>Demonstrates good linearity, with no significant carryover, or matrix effects</li><li>Offers good precision with a total reproducibility and repeatability <span>≤</span>10% CV</li><li>Offers reliability in the identification of LPCs from interfering isobaric compounds Provides good selectivity and analytical sensitivity in negative mode and is relatively fast as approximately 220 samples can be analyzed in 24 hours</li></ul>

News from LabRulezLCMS Library - Week 39, 2025

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