Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 12th August 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!
<blockquote>
<h4>👉 <a href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></h4>
</blockquote>
<blockquote>
👉 Need info about different analytical techniques? Peek into <a href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.
</blockquote>
This week we bring to you a poster from <a href="https://gcms.labrulez.com/events/568">ASMS 2024</a> by LECO, applications and other documents by Agilent Technologies, and Shimadzu!
<h4>1. LECO: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/Leachables_Topical_Ointments_Sample_Prep_BTX_GC_TOFMS_Chroma_TOF_Sync_JB_ASMS_24_LPSS_325_c545e07c6d.pdf">Employing Novel Sample Preparation and Analysis by GC-TOFMS for Improved Target and Non-Target Detection of Leachables in Cream/Gel Drug Products</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Introduction: Topical ointments are commonly used to treat diseases and skin conditions by introducing the active drug ingredient through the dermis. To ensure the safety of the product for consumers, the US FDA requires that these formulations undergo leachables studies to determine the presence of chemicals which may migrate into the product from the packaging materials. Topical ointments such as creams and gels often take the form of oil-in-water emulsions which presents a challenging matrix for these analyses. Since these emulsions cannot be analyzed directly, novel sample preparations must be developed. Even with improved sample preparation techniques, the resulting extracts can still be challenging for traditional GC-MS systems. In this collaborative study, two different sample preparation methods were employed to extract a group of five chemicals commonly found in metal packaging containers such as tubes and tins. Unspiked and blind spiked samples from extraction methods A and B were provided for analysis on LECO’s Pegasus® BTX GC-Time-of-Flight (TOF) MS system. The goal was to determine the ability of the system to effectively detect and identify these chemicals with a non-target approach by leveraging mass spectral deconvolution and a software tool (ChromaTOF® Sync) designed for the comparison of samples.
Conclusions
<ul>
<li>The Pegasus BTX GC-TOFMS successfully detected and identified all five spiked leachables in this non-target case study. Non-target analyses can be critically important for extractable and leachable studies to ensure drug product safety.</li>
<li>ChromaTOF Sync was used to successfully compare unspiked and blind-spiked ointment extracts to quickly find the leachable analytes which were present at significantly higher levels in the spikes. Automated deconvolution was crucial for uncovering the spiked analytes from the complex matrix interferences.</li>
<li>A brief demonstration of GCxGC separation power to improve the trace level identification of 9,10-anthracenedione in the presence of heavy matrix background was effectively demonstrated.</li>
</ul>
<h4>2. Agilent Technologies: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/an_residual_nmp_lithium_ion_battery_electrodes_5994_7677en_agilent_66bf9d9256.pdf">Analysis of Residual N-Methyl-2-Pyrrolidone (NMP) in Lithium-Ion Battery Electrodes</a></h4>
<ul>
<li>Application</li>
</ul>
An analysis approach using the Agilent 8697 headspace sampler with the Agilent 8860 GC system and flame ionization detector
Abstract: Accurately measuring N-methyl-2-pyrrolidone (NMP) residue is crucial for ensuring appropriate control of electrode quality in lithium-ion battery manufacturing. This necessitates the extraction of residual NMP from battery electrodes for subsequent gas chromatography (GC) analysis. Two common extraction approaches include liquid extraction (LE) of NMP from electrodes and heated extraction through a headspace sampler. This application note describes an NMP analysis method using headspace-based extraction and GC analysis with a flame ionization detector (FID). Residual NMP analysis was then conducted on real electrode samples to compare the results between headspace sampling (HS) and LE techniques.
Conclusion: In this study, a method for analyzing residual NMP in electrodes was developed using the Agilent 8697 headspacesampler coupled with the Agilent 8860 GC system and FID. The method&#39;s investigation assessed the system&#39;s performance in terms of matrix-matched calibration, quantitation precision, detection limit, and system carryover. The HS approach demonstrated an excellent detection limit and quantitation precision for targeted NMP analysis. In the carryover test, no NMP was detected in the blank run immediately after analyzing a blank cathode spiked with 100 µg NMP. The comparison between HS and LE analytical methods showed that HS could accurately quantify NMP in anode samples. The recovery rate of NMP from cathodes using the HS technique was approximately 65 to 78% of that achieved by the LE-based method. Given its operational simplicity and quantitation precision, HS is suitable for the process control of an established electrodes manufacturing route, while LE is recommended for the development of manufacturing processes and troubleshooting electrode quality issues.
<h4>3. Agilent Technologies: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/flyer_5q_gc_column_campaign_5994_7659en_agilent_5f55755564.pdf">Get the Most from Your MS Agilent J&amp;W DB-5Q and HP-5Q GC columns</a></h4>
<ul>
<li>Other</li>
</ul>
<h5>Agilent J&amp;W DB-5Q and HP-5Q GC columns</h5>
Meet the new gold standard for GC/MS
Agilent J&amp;W 5Q GC columns are designed to ensure optimal analyte delivery to your quadrupoles. They combine industry-leading ultra inert performance with ultra low-bleed technology, setting a new standard for GC/MS column reliability and productivity.
<ul>
<li>Ultra low-bleed performance enhances data accuracy with high spectral fidelity and stable baseline integration.</li>
<li>Ultra inert performance increases sensitivity for active, trace-level analytes and provides balanced deactivation for multiclass analyte panels.</li>
<li>Ultrafast conditioning and outstanding column durability improve uptime by minimizing the frequency of column changes.</li>
<li>Identical selectivity to current 5ms columns simplifies adaptation to existing retention time libraries and retention time locking.</li>
<li>Compatibility with any GC/MS system ensures a seamless fit for all Agilent GC platforms.</li>
</ul>
<h4>4. Shimadzu: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c180_e101_c8f3739683.pdf">GC/GC-MS Glass Insert/Liner Selection Guide</a></h4>
<ul>
<li>Guides</li>
</ul>
<h5>Contents</h5>
1. Introduction
<ul>
<li>1-1. Glass Inserts/Liners 3</li>
<li>1-2. Sample Injection Unit/Injection Method 4</li>
</ul>
2. Glass Insert Selection
<ul>
<li>2-1. Glass Insert Selection by GC Model/Sample Injection Unit<ul>
<li>GC-2030/GC-2050</li>
<li>GC-2010 series</li>
<li>GC-2014 series</li>
<li>GC-2025</li>
<li>HS-10</li>
</ul>
</li>
<li>2-2. Glass Insert Selection by Application<ul>
<li>SPME/SPME Arrow</li>
<li>Aqueous Solvent Analysis</li>
<li>SPL (Split/Splitless)</li>
</ul>
</li>
</ul>
3. Selection Guide
4. All Glass Insert List
<ul>
<li>4-1. Glass Insert Compatible Instruments</li>
<li>4-2. Glass Insert Information Table</li>
</ul>
5. Accessories

News from LabRulezGCMS Library - Week 33, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 19th August 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!
<blockquote>
<h4>👉 <a href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></h4>
</blockquote>
<blockquote>
👉 Need info about different analytical techniques? Peek into <a href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.
</blockquote>
This week we bring to you a posters from <a href="https://gcms.labrulez.com/events/568">ASMS 2024</a> by LECO, Agilent Technologies, Shimadzu, and Thermo Fisher Scientific!
<h4>1. LECO: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/NIST_LIBRARY_MATCH_QUALITY_HRT_MMS_CF_ASMS_24_LPSS_320_90d3c6e8c9.pdf">Evaluation of the NIST Library Matching Quality of Mass Spectra Generated by the GC-HR-TOFMS with Multi-Mode Ionization Source</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Introduction: Comparison of electron ionization spectra against standardized libraries is a staple approach to compound identification in non-targeted GC-MS analysis. High-quality matches are central to the pace of, and confidence in, such analyses. Recent developments in gas chromatography high resolution mass spectrometry have progressed non-targeted analysis applications to a wide variety of studies. However, modern ion-optical design principles which allow gains in sensitivity and resolving power may inadvertently alter fragmentation patterns, which may in turn affect the reliability of automated comparisons against standard libraries. Thus, thorough evaluation and validation of the high-quality spectra matching to the standard libraries, like NIST, is necessary for comprehensive assessment of the promised benefits of new technologies.
Conclusions: This multi-mode ionization source, as assessed using these 207 diverse analytes, generates fragmentation patterns which align very well with the NIST spectral library. Across all analytes in standard solutions, the mean library match score was 935 and the standard deviation for this value was 24.2. Mean match scores were agreeable regardless of moieties present. Percent differences for MRPS #2 spiked into a Pu’er Tea and MRPS #8 spiked into a dietary supplement were - 3.75 % and -1.44 %, illustrating how the system can easily maintain spectral confidence even in complex matrices. Overall, this study suggests the electron ionization mode of this multimode ion source, in combination with its high-resolution time of flight mass analyzer, yields spectra in excellent agreement with the quadruple dominated NIST library.
<h4>2. Agilent Technologies: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_7000d_mrm_fast_analysis_enviro_compounds_asms_2024_thp360_en_agilent_d338929001.pdf">Fast Analysis of 140 Environmental Compounds by GC/MS/MS</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Introduction: Pesticides, polycyclic aromatic hydrocarbons (PAHs), and polychlorinated biphenyls (PCBs) are persistent environmental pollutants with the potential for bioaccumulation.¹ Previously, these compound classes have been analyzed using gas chromatography with an electron capture detector (GC-ECD), but this requires full chromatographic separation of all analytes for confident chemical identification. With a triple quadrupole detector (QQQ), analysis time significantly drops due to mass identification eliminating the need to chromatographically separate all components. Further, multiple reaction monitoring (MRM) mode on the QQQ provides a higher confidence in peak identification than analysis by scan or selected ion monitoring (SIM) mode. Combining chromatographic separation and MS/MS analysis is especially useful for PAHs and PCBs where multiple analytes may have the same m/z value.
Conclusions: Transitioning methods from GC-ECD to GC/MS/MS is highly beneficial.
By running in MRM mode, we enable the following:
<ul>
<li>Significant time-savings</li>
<li>Increased confidence in hits</li>
<li>Sample quantification remains the same</li>
</ul>
<h4>3. Shimadzu: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Th_P364_Novel_High_Sensitivity_Detector_for_GCMS_adcdac36c4.pdf">Novel High Sensitivity Detector for GC/MS</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Overview
<ul>
<li>We have developed a novel high sensitivity detector which has a simple structure to achieve high ion transmission and eliminate neutral molecules simultaneously.</li>
<li>Signal to noise ratio (S/N) was 1.5 times higher than that with a conventional detector.</li>
</ul>
Introduction: 
In GC/MS, numerous neutral molecules originated from carrier gas pass through quadrupole mass filter without being removed, and thereby they are finally transferred to ion detector. When they enter the detector, they may cause noise in the detecting signal. For this problem, some detector structures have already been proposed to remove these neutral molecules. However, they have complex structures and the room for improvement of ion transmission. In this study, we have developed the new high sensitivity detector which has a simple structure to achieve high ion transmission and to eliminate neutral molecules simultaneously.
Conclusions:
<ul>
<li>We have developed the new high sensitivity detector and achieved the high ion transmission and removal of neutral molecules simultaneously.</li>
<li>Signal intensity was increased by 1.2 times and noise was reduced by about 20%, S/N was 1.5 times higher than that with the conventional detector.</li>
<li>This noise reduction effect will be larger in the high flow analysis. In addition, this detector is promising to extend the lifetime of the detector due to less contamination from neutral particles in the conversion dynode and electron multiplier.</li>
</ul>
<h4>4. Thermo Fisher Scientific: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_142_utilizing_hydrogen_pesticides_food_gc_ms_po142_asms2024_en_7ed0951b93.pdf">Utilizing hydrogen carrier gas for sensitive analysis of pesticides in food using gas chromatography mass spectrometry</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
<h5>Abstract</h5>
Purpose: To demonstrate the performance of the Thermo Scientifc HeSaverH2Safer kit for iConnect split-splitless (SSL) injection module for trace analysis of pesticides using H2 as a carrier gas as a safe and sustainable solution for laboratory operations 
Methods: In this study, hydrogen was used as a carrier gas for GC-MS/MS analysis of trace levels of pesticides in food. The GC was fitted with a new hydrogen safer split/splitless injector, with chromatographic separation performed on a TG-5 SIL MS (30 m × 0.25 mm, 0.25 μm) capillary GC column. The chromatographic conditions applied ensured critical pair separation was achieved. The GC-MS/MS system was equipped with an advanced electron ionization (AEI) source to increase sensitivity for analyte detection. Quantification and assessment of critical regulatory requirements, such as linearity and sensitivity, were performed in a single software.
<h5>Conclusions</h5>
<ul>
<li>The use of the HeSaver-H2Safer technology allows for a safe and compliant use of hydrogen as an alternative carrier gas in GC/GC-MS applications without the need to install a hydrogen sensor and removes any risk of unwanted reactions with the sample in the hot SSL injector.</li>
<li>When used with hydrogen, the limited carrier gas consumption offered by the HeSaverH2Safer mode permits a very controlled system demand for hydrogen, making this solution ideal for laboratories working with hydrogen generators.</li>
<li>Migrating the GC-MS/MS method from helium to hydrogen requires an adaptation of method parameters to address (i.e., retention time shift and different fragmentation patterns).</li>
<li>97% of pesticides in baby food and 98% in honey showed a linear response in the concentration range 0.005–0.500 mg/kg and the relative standard deviation for N=5 repeats of each sample type at 0.01 mg/kg was equal or lower than 10% for 98% of the evaluated compounds.</li>
</ul>

News from LabRulezGCMS Library - Week 34, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 26th August 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!
<blockquote>
<h4>👉 <a href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></h4>
</blockquote>
<blockquote>
👉 Need info about different analytical techniques? Peek into <a href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.
</blockquote>
This week we bring to you a posters from <a href="https://gcms.labrulez.com/events/568">ASMS 2024</a> by LECO, Agilent Technologies, Shimadzu, and Thermo Fisher Scientific!
<h4>1. LECO: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Long_Lifetime_Ion_Detector_GC_G_Cx_GC_TOFMS_MS_ASMS_24_LPSS_326_4c9e1fb7a1.pdf">A Novel Long-Lifetime Ion Detector for GC-TOFMS and GCxGC-TOFMS with Sub-Femtogram Detection Limits</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Introduction: Ion detection efficiency and fast response times are critical aspects of the ion detectors used in time-of-flight mass spectrometry (TOFMS). With modern advancements in ionization, ion optics, and ion transfer efficiency, TOFMS systems are capable of generating high ion flux onto the ion detectors. Having an ion detector that is capable of maintaining optimal performance over a long period of time while accepting high amounts of ion flux is a significant challenge in development of TOFMS instrumentation. Improvements in detector life will minimize maintenance costs and improve TOFMS user experience. A novel long-lifetime ion detector was developed in partnership with El Mul Technologies for use in LECO’s Pegasus® BTX GC and GCxGCTOFMS. The system was thoroughly evaluated for sensitivity and robustness, including longevity of the detector.
Conclusions: The Pegasus BTX GC(GCxGC)-TOFMS with a novel Long-Lifetime Ion Detector has demonstrated the following performance characteristics:
<ul>
<li>Sub-2 fg IDL for GC-TOFMS and Sub-fg IDL for GCxGC-TOFMS</li>
<li>Linear dynamic range of 5 orders of magnitude in GC-TOFMS and 4 orders of magnitude in GCxGC-TOFMS</li>
<li>Robust operation: the detector bias remains consistent and BTX peak intensity remains consistent over long periods of time, even with large numbers of samples acquired and significant amounts of charge accumulation on the detector.</li>
</ul>
<h4>2. Thermo Fisher Scientific: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_153_dioxin_analysis_gc_orbitrap_capabilities_po153_asms2024_en_f72a355ee6.pdf">Meeting the challenges of Dioxin analysis and more with GC-Orbitrap high mass resolution capabilities</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
<h5>Abstract</h5>
Purpose: Evaluate the performance of gas chromatography (GC) Orbitrap high mass resolution spectrometry for trace analysis of polychlorinated dibenzo-p-dioxins/furans (PCDD/PCDF) at current maximum allowable limits in soil according to EPA 1613 method criteria.¹ 
Method summary: Sample analysis was carried out on the Thermo ScientificOrbitrap Explorisᵀᴹ GC 240 mass spectrometer. A sample volume of 1.5 μL was injected for chromatographic separation using a TG-Dioxin (60 m × 0.25 mm, 0.25 μm) capillary GC column with a Thermo Scientific TRACE 1610 GC. Ion source conditions were optimized to fulfill sensitivity criteria of EPA 1613. Performance was evaluated through analysis of a raw soil extract previously analyzed using a regulatory compliant method². Quantification was performed using isotopic dilution in Thermo Scientific Chromeleon Chromatography Data System (CDS) software using the Dioxin Analyzer workflow . 
Results: The Orbitrap GC mass spectrometer fulfilled the high sensitivity, mass accuracy and resolution criteria of EPA 1613 at femtogram (fg) levels within a raw soil extract. Combined with a large dynamic range (0.05 – 100 pg•μL⁻¹), the OE GC provides users with an alternative analytical approach to deliver sensitive and accurate analysis of PCDD/F while enabling laboratories to meet future analytical challenges with high resolution accurate mass data.
<h4>3. Shimadzu: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Th_P_347_ASMS_Poster_Cafe_Ana_V6_239x117_03f5bcb26c.pdf">Ensuring food safety through the study of potential extractables and leachables in roasted coffee packaging by ultra-sensitive Headspace GC/MS</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Introduction
<ul>
<li>The main function of food product packaging is to protect food against any contaminant. However, in some circumstances, this packaging can release possible substances that pose a risk to human health. These are extractables and leachables (E&amp;L) compounds that migrate from materials into the product, especially under factors such as temperature, time, and solvents.</li>
<li>Notably, Brazilian legislation lacks a consolidated assessment to monitor these compounds in the food industry.</li>
<li>The Headspace Shimadzu HS-20 NX trap model allows the concentration of compounds, up to 10 times, in a trap material. This means that even very small traces of these contaminants can be detected and quantified accurately.</li>
<li>When coupled with GCMS-QP2020 NX (Fig.1), the HS-20 NX becomes a powerful tool for identifying and analyzing potential toxic contaminants, significantly contributing to food safety and compliance with quality regulations.</li>
</ul>
Conclusion
<ul>
<li>The use of HS-20 NX in Trap mode with GC/MS enabled the identification of over 100 compounds, comparing the spectra with the National Institute of Standard and Technology (NIST) library. Among these compounds are potential E&amp;L substances, as well as coffee aroma components.</li>
<li>This technique demonstrates high versatility and efficiency by providing high analytical sensitivity capable of identifying compounds even at low concentrations, something unachievable by conventional methods. This evolution represents a notable advancement in coffee and food quality control, enabling precise detection of essential characteristics and components to ensure the excellence of the final product and consumer health.</li>
</ul>
<h4>4. Agilent Technologies: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Th_P_347_ASMS_Poster_Cafe_Ana_V6_239x117_03f5bcb26c.pdf">Faster Qualitative Analysis of Essential Oils Using GC/MS with Hydrogen Carrier Gas and a Hydrogen Optimized EI Source</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Introduction: Due to the price of helium (He), many laboratories are looking for alternative carrier gases for their gas chromatography/mass spectrometry (GC/MS) methods. This work describes the conversion of a GC/MS method for the identification of flavor and fragrance compounds in essential oils from helium to hydrogen (H₂). A single quadrupole GC/MS system was used with hydrogen carrier gas and an EI source optimized to provide spectral fidelity with hydrogen. To increase confidence in compound identifications, deconvoluted mass spectra and linear retention indices (RI) were searched against the NIST23 mass spectral library. A column and chromatographic conditions for hydrogen were chosen that reduce the analysis time by 2.5 times compared to the helium method and generates results comparable to helium.
Conclusions: The data presented here shows that H₂ can successfully be used as a carrier gas for flavor and fragrance analyses with the proper conversion steps.
<ul>
<li>The choice of the 20 m x 0.18 mm id x 0.18 µm film HP-5MSUI column allowed a 2.5 times faster analysis with equivalent chromatographic resolution.</li>
<li>The Method Translation calculator provided chromatographic conditions that maintained the same elution order as with the He method, resulting in excellent agreement of the RI values measured with both methods.</li>
<li>The use of MassHunter Unknowns Analysis software to deconvolute spectra and search them with RI filtering against the NIST23 library significantly simplified identification of the flavor components.</li>
<li>The HydroInert EI source minimized in-source reactions with H₂, resulting in higher LMS values.</li>
</ul>
For further details on this work, please see reference 3. Reference 4 provides more information on flavor components that can react with H₂ in the source, and which benefit from the use of HydroInert. Note that if He is available at an acceptable price, it is the preferred carrier for GC/MS and should be used. However, as shown in this work, H2 can be used if appropriate method adjustments are made to accommodate its use.

News from LabRulezGCMS Library - Week 35, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 9th September 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring to you applications by Agilent Technologies, Shimadzu, and Thermo Fisher Scientific and poster by LECO from ACS meeting!<h4>1. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_002952_gc_ms_isq_environmental_an002952_na_en_9738609742.pdf">Adhering to U.S. EPA Method 524.2 for the analysis of volatile organic compounds in drinking water</a></h4><ul><li>application</li></ul>Goal: Demonstration of a routine analytical method that meets the requirements outlined in U.S. EPA 524.2 for the quantitation of volatile organic compounds (VOCs) in drinking water, using the Teledyne LABS Tekmar Lumin Purge and Trap (P&amp;T) concentrator paired with the AQUATek LVA autosampler system along with a Thermo Scientific™ ISQ™ 7610 MS system coupled with a Thermo Scientific™ TRACE™ 1610 gas chromatograph (GC) and Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS). Method linearity, method detection limit (MDL), precision, and accuracy were assessed to evaluate method performance.Introduction: Analytical testing labs play a crucial role in monitoring surface, ground, and drinking water for volatile organic compounds (VOCs). Common by-products in the processing of household and industrial products, VOCs can contaminate water sources, potentially harming the environment and public health. To safeguard against this, labs use the U.S. EPA Method 524.21 to test water for the presence of VOCs, including four trihalomethane disinfection by-products. This procedure utilizes Purge and Trap (P&amp;T) procedures to remove VOCs with high volatility and low water solubility from water samples, followed by gas chromatography-mass spectrometry (GC-MS).Conclusion: The TRACE 1610 GC, the ISQ 7610 system, and the Tekmar Lumin P&amp;T with the AQUATek LVA autosampler system together offer benefits for executing U.S. EPA Method 524.2. The Tekmar Lumin P&amp;T concentrator enhances sample throughput through efficient trap cooling and moisture control, thus reducing peak interference and extending GC column life. The ISQ 7610 system’s VPI and ExtractaBrite ion source allow ionization source and analytical column replacement without venting the instrument, ensuring minimal downtime, and the XLXR™ detector offers extended linear dynamic range. The collective technology addresses routine VOC analysis challenges, ensuring robust sensitivity, maximized output, and consistent method compliance. The ISQ 7610 system equipped with the VPI coupled with the Tekmar Lumin P&amp;T and the AQUATek LVA autosampler exceeds all the requirements outlined in U.S. EPA Method 524.2 for analysis of VOCs in drinking water:<ul><li>Excellent linearity for all compounds was demonstrated with the %RSD of the calibration response factors passing all method requirements.</li><li>MDL and precision for seven 0.5 ppb standards showed no interference from excessive water and produced very reproducible results. The average MDL result for all 83 target compounds was 0.06 ppb with a precision of 4.06%.</li><li>The precision for n=31 samples over 189 injections displayed &lt;30% RSD accuracy for all compounds as the method requires. The average precision for all 83 target compounds and 2 surrogates gave a %RSD of 6.43% with an accuracy of 98% recovering the compounds. Individually, 4-bromofluorobenzene and 1,2-dichlorobenzene-d4 had a 7.68% RSD with an accuracy of 98% and 4.95% RSD and an accuracy of 95%, respectively, over 189 injections and almost four days of uninterrupted analysis.</li></ul><h4>2. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00706_en_f95bd4b605.pdf">Analysis of Denatured Fuel Ethanol with Brevis GC-2050 Using ASTM D5501</a></h4><ul><li>application</li></ul>User Benefits<ul><li>The compact design of the Brevis GC-2050 enables space-saving in the laboratory.</li><li>As an alternative gas for helium, hydrogen can be used as the carrier gas.</li><li>&nbsp;Analysis of ethanol and methanol in fuels based on ASTM D5501 is possible.</li></ul>IntroductionBioethanol has attracted attention as a form of renewable energy which can be obtained from biomasssuch as corn and sugar cane. ASTM D5501 provides a test method for determination of the concentrations of ethanol and methanol in fuels for concentrations of ethanol from 20 to 100 wt% and concentrations of methanol from 0.01 to 0.6 wt%.In this Application News article, measurements of the purity of ethanol containing gasoline as a denaturant as specified in ASTM D5501 were carried out with a Brevis GC-2050 gas chromatograph, using helium and hydrogen asthe carrier gases.ConclusionEthanol purity tests were carried out as provided in ASTM D5501 using a Brevis GC-2050 gas chromatograph. The splitter linearity test showed no inlet discrimination so that accurate qualitative analysis could be made for denatured fuel ethanol with the wide boiling range components regardless of whether helium or hydrogen was used as the carrier gas.<h4>3. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_aldehydes_beer_pal3_autosampler_5977c_gc_msd_5994_7633en_agilent_1fe3b8541c.pdf">Analysis of Aldehydes in Beer by Agilent PAL3 Autosampler and 5977C GC/MSD</a></h4><ul><li>application</li></ul>AbstractThis application note describes a method for quantitation of four aldehydes (hexanal, furfural, phenylacetaldehyde, and trans-2-nonenal) responsible for off-flavors in beer using an Agilent 8890/5977C GC/MSD with an Agilent PAL3 (SPME) autosampler. The method used fully automated, solvent-free extraction and on-fiber derivatization. The aldehyde compounds were derivatized with the derivatization agent O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) using the on-fiber derivatization procedure. The derivatization agent was first adsorbed onto an Agilent 65 µm PDMS/DVB fiber. Next, the fiber was inserted into a 20 mL headspace vial containing a 2 mL beer sample with agitation at 60 °C for 30 minutes. Both extraction and derivatization procedures were automatically performed using the PAL3 autosampler. The method demonstrated excellent sensitivity, with detection limits of 0.0009 µg/L for hexanal, 0.52 µg/L for furfural, 0.015 µg/L for phenylacetaldehyde, and 0.003 µg/L for trans-2-nonenal. The limits of the quantification for the four compounds were 0.003, 1.72, 0.05, and 0.01&nbsp;µg/L, respectively. The four aldehydes were successfully quantified in four beer samples purchased from a supermarket. Good repeatability was demonstrated with RSD &lt; 4.9% based on three replicate injections of the four beer samples for all four&nbsp;aldehydes.ConclusionThis application note describes the quantitative analysis of four aldehydes (hexanal, furfural, phenylacetaldehyde, and trans-2-nonenal) responsible for off-flavors in beer using an Agilent 8890/5977C GC/MSD with a PAL3 (SPME) autosampler. This method offers the advantages of full automation, rapid analysis, solvent-free extraction, and on-fiber derivatization. With this automated solution, excellent sensitivity was demonstrated for the detection of hexanal (0.0009 μg/L), furfural (0.52 μg/L), phenylacetaldehyde (0.015&nbsp;μg/L), and trans-2-nonenal (0.003 μg/L). Four different brands of beer were analyzed, with hexanal detected in the range of 0.45 to 1.56 μg/L, furfural in the range of 6.62&nbsp;to 50.37 μg/L, phenylacetaldehyde in the range of 6.64 to 10.51&nbsp;μg/L, and trans-2-nonenal in the range of 0.031 to 0.062&nbsp;μg/L. Good repeatability was demonstrated with RSD&nbsp;&lt;&nbsp;4.9% based on three replicate injections of the four beer samples for all four aldehydes.<h4>4. LECO: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/hf_acs21_lpss_284_c35134b9cd.pdf">Combining GC with MS and Olfactory Detection for a Variety of Food, Flavor, and Fragrance Analyses</a></h4><ul><li>Poster / ACS</li></ul>INTRODUCTIONGas chromatography (GC) coupled with mass spectrometry (MS) is an important tool for the characterization of a wide range of food, flavor, and fragrance samples. The components most likely to contribute to the aroma of a sample tend to be volatile and semi-volatile analytes, and GC-MS is well-suited for this type of analysis. Complex samples are effectively separated into the individual analyte components with GC. Time-of-Flight (TOF) MS detection provides important information towards the identification of these potentially important components of the sample with full m/z range data that can be library searched and that is also optimal for deconvolution algorithms. The incorporation of olfactory (O) detection with this data is particularly helpful for connecting the identified features with their contributions to the overall aroma or flavor. This type of sensory directed analysis highlights regions of interest and leads to specific analytes of interest for a focused review of the data. This combination of tools can separate and identify analytes and then determine those that are most important for contributing to the sensory characteristics of the sample. A variety of samples were analyzed with this combination of tools, and the benefits of using the information together are highlighted.CONCLUSIONSIn this work, the combination of a GC separation with MS and O for detection provided a powerful and efficient analytical platform to isolate individual analytes, identify those isolated analytes, and connect them to their sensory impacts. The olfactory data allowed for sensory directed analysis. In each case, the GC separation and full m/z range TOFMS data were crucial for determining the identification of the feature responsible for the characteristic aroma. This collection of tools was demonstrated for the characterization of the most aroma impacting components of a nutmeg essential oil, the distinction of sensory differences in cilantro, and the determination of an off-odor in beer.

News from LabRulezGCMS Library - Week 37, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 30th September 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring to you applications by Agilent Technologies, Waters Corporation, and Thermo Fisher Scientific, and a poster from <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/296">ASMS</a> by Shimadzu!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/TP_093_Analysis_of_PFAS_in_Water_Final_05292024_8fa9fcb27d.pdf">Analysis of Volatile PFAS in Water Using Head-Space Solid Phase Microextraction- Gas Chromatography/Mass Spectrometry (HS-SPME GC/MS)</a></h4><ul><li>Poster / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/296">ASMS</a>&nbsp;</li></ul>Introduction&nbsp;Per- and Polyfluoroalkyl Substances (PFAS) are environmental pollutants with recognized health and environmental concerns due to their probable toxicity, persistence, and ubiquitousness throughout the environment, and consumer and industrial products. PFAS encompass a large family of chemicals with varying physicochemical properties. These properties not only affect their toxicity and environmental fate, but also complicates chemical analysis.In this work, a Head-Space Solid Phase Microextraction-Gas Chromatography/Mass Spectrometry (HS-SPME GCMS) analytical method was developed to analyze six classes of volatile PFAS in water. This HS-SPME method presents the advantage of simplifying sample extraction and handling for the analysis of volatile PFAS in water, hence, minimizing operational costs, potential errors, and risk of sample-cross contamination.ConclusionThis study demonstrated the use of a Shimadzu GC/MS-QP2020 NX single quadrupole instrument configured with the AOC-6000 Plus multifunctional autosampler and an automated head space solid phase microextraction unit for measurement of volatile PFAS compounds in water. Linear calibration curves were obtained for all compounds (R 2 ≥ 0.993 and RF %RSD &lt; 20 %). The HS-SPME GC/MS-QP2020 NX method demonstrated qualitative and quantitative capability of analyzing PFAS compounds.<h4>2. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003028_gc_ms_isq_epa_vocs_an003028_na_en_7646797ef5.pdf">Analysis of volatile organic compounds in drinking water according to U.S. EPA Method 524.4</a></h4><ul><li>Application</li></ul>GoalDemonstration of an analytical method that meets the requirements outlined in U.S. EPA Method 524.4 for the quantitation of volatile organic compounds (VOCs) in drinking water, using the Teledyne LABS Tekmar Lumin Purge and Trap (P&amp;T) concentrator paired with the AQUATek LVA autosampler system along with a Thermo Scientific™ ISQ™ 7610 MS system coupled with a Thermo Scientific™ TRACE™ 1610 gas chromatograph (GC) and Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS). Target analyte linearity, method detection limit (MDL), minimum report level (MRL), and mid-point precision and accuracy were assessed to evaluate method performance.Keywords: EPA, U.S. EPA 524.4, VOCs, phthalates, trace analysis, gas chromatography, single quadrupole mass spectrometry, selected ion monitoring, sensitivity, GRO, THM, volatiles, environmental lab, environmental sample analysis, analytical testing laboratories, ISQ 7610 MS, TRACE 1610 GC, GC-MS.IntroductionVolatile organic compounds (VOCs) are man-made contaminants in various products that pose environmental and public health risks. These compounds are regulated in drinking water, and laboratories follow regulations including U.S. EPA Method 524.2.1 A previous application note described U.S. EPA Method 524.2,2,3 which is the most common method for VOC water testing in the USA. U.S. EPA Method 524.4 is an updated method that allows for nitrogen to be used as the purge gas, thus reducing helium consumption, and is now being more widely used. Targeting 75 VOCs, this method differs by offering more method parameter flexibility but stricter quality control, including the stringent calculation of the minimum reporting level for evaluating calibration checks.Implementing U.S. EPA Method 524.4 can present multiple challenges for laboratories. Striking a balance between optimized method conditions and meeting the acceptance criteria, like detection limit requirements for various compound concentrations, is pivotal. Another major hurdle is managing the water matrix to minimize GC-MS system water introduction, which could lead to detrimental effects and delay sample reporting, thereby increasing public safety risks. Ultimately, maintaining consistency in test results to avoid sample reanalysis is crucial. Another factor for laboratories to consider is the fluctuating cost of helium, which is the analytical gas of choice for this analysis. Reducing the use of helium—a limited resource—will enable the laboratory to reduce operational costs and increase profitability.The following evaluation describes the use of the ISQ 7610 GC-MS system coupled with a TRACE 1610 GC with the Thermo Scientific™ HeSaver-H2Safer™ split/splitless injector and Teledyne LABS Tekmar Lumin P&amp;T concentrator paired with the AQUATek LVA autosampler for U.S. EPA Method 524.4.ConclusionThe combined solution of the TRACE 1610 GC coupled with the ISQ 7610 system and the Tekmar Lumin P&amp;T concentrator with the AQUATek LVA autosampler system successfully addresses the challenges of VOC analysis and provides a robust, sensitive solution needed for ensuring maximized sample throughput and regulatory method compliance for U.S. EPA Method 524.4.<ul><li>Excellent linearity for all compounds was demonstrated with the linear regression (r²≥0.995) of the calibration response factors passing all method requirements.</li><li>MDL and precision for seven 0.5 ppb standards showed no interference from excessive water and produced very reproducible results.</li><li>The precision for n=30 samples over 245 injections displayed &lt;30% RSD for all compounds as the method requires and an average recovery of 91%.</li><li>Utilizing HeSaver-H2Safer technology reduced helium consumption for the method by 4 times, which provides a significant cost savings.</li></ul><h4>3. Waters Corporation: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008298_en_db4158391c.pdf">Extractables Analysis of Nasal Spray Devices Using Gas Chromatography and High- Resolution Mass Spectrometry With Soft Ionization</a></h4><ul><li>Application</li></ul>AbstractDue to concern about the safety of components from plastic, it is crucial to screen for and identify potential extractables and leachables (E&amp;L) in pharmaceutical packaging and medical devices. For volatile, and semi-volatile compounds, gas chromatography-mass spectrometry (GC-MS) with electron ionization (EI) is typically used. Compounds are determined using scientific libraries; however, where compounds are not listed or where the sensitivity of EI-MS is not sufficient, the identification process becomes challenging.Here, we describe an E&amp;L screening experiment using gas chromatography and a quadrupole time of flight high-resolution mass spectrometer (QToF-HRMS) with atmospheric pressure gas chromatography (APGC) for soft ionization. A data independent acquisition (DIA) strategy is utilized to aid screening and elucidation which are combined in a screening software solution.Benefits<ul><li>GC-QToF MS with APGC as an orthogonal technique to LC-QToF-MS allows for comprehensive compound coverage with increased sensitivity compared to typical EI techniques</li><li>The UNIFI™ application within the waters_connect™ platform provides customized workflows to simplify screening and structural elucidation in complex datasets</li><li>The Xevo™ G3 QTof Mass Spectrometer enables confident identification of E&amp;L components in complex matrices through novel ion optics and detection system which maximize transmission</li><li>Soft ionization using the APGC™ source allows for the detection of molecular ions from which elemental compositions can be derived to aid compound identification and confirmation&nbsp;</li><li>MSE, a data independent acquisition, increases confidence in identifications when screening against a library and provides additional information to aid structural elucidation</li></ul>Conclusion&nbsp;When undertaking E&amp;L screening analyses it is important to use a range of analytical techniques to account for different compound chemistries. GC-QToF MS with APGC as an orthogonal technique to LC-QToF-MS allowed for comprehensive compound coverage with increased sensitivity compared to typical EI techniques. Due to the soft ionization of APGC, the intact molecular ion is often present in the spectra. This combined with a data independent acquisition, MSE mode, utilizes full spectral acquisition of the accurate mass information of both precursor and fragment ions.This approach boosts confidence in component identifications when screening against an MS/MS library, while minimizing false positives. For instance, in the LC-QToF-MS there were just under 40 potential compounds matches in sample E48 after considering factors such as retention time match, mass accuracy below 3 ppm, and the presence of at least one fragment ion. A further 38 compound matches in sample E48 were tentatively identified using GC-QToF MS with APGC, with mass accuracy below 3 ppm, and the presence of at least one fragment ion.MSE data also aids in the structural elucidation of unknown substances by utilizing accurate mass and corresponding fragment ions, facilitating comprehensive characterization. This data increases confidence in identifications of components and assists with structural elucidation of unknowns to ultimately aid full characterization. For example an unknown with protonated m/z 284.2703 was tentatively identified as a N-(2-(1-piperazinyl)ethyl)decanamide (mass error 2.33 ppm) by the software.For the extractables analysis of nasal sprays the UNIFI application within the waters_connect platform provided SST benchmarking, screening against a library, summary plots to identify trends, filtering of AET levels, binary compare mode to isolate relevant unknowns, and a Discovery Tool for elucidation of unknowns.<h4>4. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_voc_rubber_gasket_extracts_gc_msd_5994_7777en_agilent_6a0a6bf7d0.pdf">Analysis of Volatile Compounds Identified in Rubber Gasket Extracts Using GC/MSD and High-Resolution GC/Q-TOF</a></h4><ul><li>Application</li></ul>AbstractChemicals that are part of polymeric container closure systems (CCS) and drug delivery systems have the potential to migrate into drug products during manufacturing, storage, transport, and delivery, and must be identified in the final products to ensure their safety.This application note presents a rubber gasket extractables study using a unit mass resolution gas chromatography/mass selective detector (GC/MSD) and a high-resolution gas chromatography/quadrupole time-of-flight (GC/Q-TOF) mass spectrometer to establish a process for identifying GC-amenable extractables and leachable (E&amp;L) compounds.IntroductionElastomeric gaskets, plungers, and O-rings are common sources of leachable compounds in the manufacturing, storage, and delivery of drug products. E&amp;Ls derived from elastomeric components may impact the stability and efficacy of small and large molecule drug products1, and therefore need to be characterized thoroughly. Exposure to some E&amp;L chemicals, such as phthalates and nitrosamines, even at low levels, may cause safety concerns.2 Chemicals derived from the elastomer manufacturing process typically include accelerators, activators, antioxidants, fillers, plasticizers (including phthalates), mold release agents, and other additives3 that may leach into the final product. Some additives present in elastomer packaging materials may also contain polycyclic aromatic hydrocarbons (PAHs)4 and aliphatic hydrocarbons.GC/MS is a commonly used technique for analyzing volatile and semivolatile organic compounds in the E&amp;L space. This study demonstrates the capabilities of GC/MSD to identify GC-amenable compounds present in a solvent extract of a rubber gasket by leveraging chromatographic deconvolution in combination with retention index (RI)-based filtering. Adding a high-resolution accurate mass GC/Q-TOF into the E&amp;L workflow provided a higher number of identified chemicals. It also increased confidence in compound identification and enabled structure elucidation of unknown compounds.The study was performed in the Network Workstation configuration using Agilent OpenLab Electronic Content Management (ECM) XT as the data repository. This configuration enabled tools that facilitate compliance with various national and EU electronic record regulations, including audit trails, user authentication, role-based permission controls, and remote data storage.5ConclusionThe GC/MSD is an effective and accessible tool for the analysis of volatile and semivolatile compounds in complex E&amp;L extracts. The established workflow includes deconvolution and an RI-based library search with the data acquisition performed in a compliant environment.The high-resolution Agilent 7250 GC/Q-TOF enabled the identification of additional components with increased confidence, as well as structure elucidation of the unknown compounds.Furthermore, using the novel ultra-low bleed Agilent J&amp;W DB-5Q GC column resulted in a significant decrease in background, which helps in the identification of late-eluting compounds.

News from LabRulezGCMS Library - Week 40, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 14th October 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring to you applications by Agilent Technologies, Thermo Fisher Scientific, and posters by Shimadzu and LECO!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/aoac_2024_9_m031_d1063f34df.pdf">Interlaboratory comparison study of two gas chromatography injection techniques viz. liquid and dynamic headspace for trace level quantification of Ethylene Oxide (EtO) and 2-Chloroethanol (2-CE) in ginger powder sample by using tandem mass spectrometry</a></h4><ul><li>Poster / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/292">AOAC</a></li></ul>PurposeEtO is one of the most widely produced chemicals worldwide. It is colorless, odorless, flammable gaseous cyclic ether with boiling point of 10.4°C. It has a very strong antibacterial property. Due to its small size, it shows a high diffusivity and strong penetrating properties and is thus very effective in the disinfestation / disinfection of food commodities. EtO is highly carcinogenic, mutagenic and genotoxic impurity for living being. The US National Institute of Health (NIH) classified EtO as “known to be a human carcinogen based on sufficient evidence of carcinogenicity from studies in humans, including epidemiological studies and studies on mechanisms of carcinogenesis.” Considering carcinogenicity and no acceptable threshold for exposure, no Acceptable Daily Intake (ADI) was established for EtO.2-CE, which is one of the prominent metabolite of EtO is also considered to be genotoxic and potentially carcinogenic. Given the inconclusive toxicological picture of 2-CE, it was decided by regulatory authorities to follow the precaution approach and consider 2-CE equally toxic to EtO. Hence it is very important to quantitate EtO and 2-CE in food matrices at trace levels. EU-MRLs (Maximum Residue Levels as per European Commission) for EtO and 2-CE are summarized in Table 1.Various methods have been presented in EURL-SRM-Analytical Observation Report for the analysis of EtO and 2-CE. The choice of the analytical approach depends on both the analytes and the matrix to be analyzed. So, it is important to have a detailed comparison study of different analytical approaches to ensure robustness, reliability and accuracy of the method for the quantification of EtO and 2-CE.This study covers the comparison between liquid injection technique and dynamic headspace injection technique using different extraction processes for ensuring highest extraction efficiencies. Incurred sample is used for this study.Conclusion<ul><li>In comparison between liquid and HS-Dynamic mode, it is evident that HS Dynamic has advantage in method optimization for accurate recoveries. Liquid extraction needs multiple trials to ensure complete extraction of analytes, majorly depending on matrix. Similarly, temperature and extraction time also plays a critical role</li><li>Quantification of EtO and 2-CE impurities in ginger powder sample was successfully performed by using Shimadzu GCMS-TQ8050 NX with AOC-20i/s and HS-20 NX dynamic headspace samplers</li><li>HS Dynamic requires less sample preparation, demonstrates high recovery due to closed system, high accuracy and easy method optimization</li></ul><h4>2. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_phosphine_cereals_spices_8697_headspace_8890_7010c_5994_7859en_agilent_c8f2d8fe74.pdf">Estimation of Hydrogen Phosphide (Phosphine) Residues in Cereals and Spices Using the Agilent 8697 Headspace Sampler and GC/MS/MS</a></h4><ul><li>Application</li></ul><h5>Abstract</h5>This application note demonstrates the use of an Agilent 8890 GC system coupled with the Agilent 8697 headspace sampler and Agilent 7010 GC/TQ to detect and quantify hydrogen phosphide (phosphine) residues in rice and red chili powder. The sample was inserted into a headspace vial and Milli-Q water was added. The vial was crimped and loaded into the headspace sampler, followed by GC/MS/MS analysis. The limit of quantification of 5 ng/g was achieved in rice and red chili powder matrices. Average recoveries ranged from 80 to 110% in various recovery experiments.<h5>Introduction</h5>Fumigants are gases used for controlling pests in stored food products.1 Cereals are mainly disinfected by hydrogen phosphide (commonly known as phosphine) and liberated from stable salts such as zinc phosphide or aluminum phosphide.1 Phosphine is a colorless gas that is used as a fumigant worldwide because of its rapid diffusion and extreme volatility.1 Despite these desirable properties, trace amounts of phosphine may persist in foods several months after treatment and can cause severe health problems.1Due to its high volatility, phosphine is not amenable to club with common multiresidue methods for pesticide residue analysis in food. Thus, special single-residue methods must be applied.2 Previously, methods for the analysis of phosphine have been developed that highlight the use of the Tenax-filled inlet liner along with cryogenic cooling to preconcentrate the phosphine prior to chromatographic separation. These methods require heavy analytical configurations that include a liquid nitrogen handling system. In EU legislation, maximum residue limits for phosphine in foodstuffs range from 0.01 to 0.1 mg/kg, depending on the commodity (Commission Regulation (EC) No. 149/2008).2The method adopted in this application note demonstrates the use of the 8697 headspace sampler for sample introduction to the 8890 GC system coupled with the 7010 GC/TQ.&nbsp;Column configurationTo prevent single, loose particles of the PLOT column stationary phase from entering the ion source of the mass-sensitive detector (MSD), a restriction capillary (1 m × 0.15 mm) was inserted between the PLOT column and the MSD using a purged Ultimate union. This configuration also helps in column replacement without venting the mass spectrometer.<h5>Conclusion</h5>An accurate and rugged method was developed which meets the requirements of the European Union reference laboratory (EURL) for maximum residue limits of phosphine in foodstuffs. This ranges from 0.01 to 0.1 mg/kg, depending on the commodity (Commission Regulation (EC) No 149/2008) for the analysis of phosphine in rice and red chili powder. The LOQ of the method was demonstrated at 5 ng/g for all tested matrices. Repeatable results were found for four successive replicates of matrix-based standards at 20 ng/g concentration levels. Excellent recoveries were obtained in all tested matrices at 10 ng/g spiked concentration levels. Thus, this study demonstrates the usefulness of the developed method for routine analysis of food samples for phosphine analysis at trace levels.<h4>3. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003105_gc_ms_tsq_9610_dioxins_furan_feed_an003105_na_en_26c691ad68.pdf">Trace analysis of polychlorinated dibenzo-p-dioxins/ dibenzofurans using GC-MS/MS in accordance with EU Regulations 2017/644 and 2017/771 for food and feed</a></h4><ul><li>Application</li></ul>GoalTo demonstrate the suitability of the Thermo Scientific™ TSQ™ 9610 triple quadrupole GC-MS/MS system with Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS) software for the routine and regulatory compliance testing of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzo-p-furans (PCDD/Fs) in food and feed samples in accordance with Commission Regulations (EU) 2017/644 and 2017/771.IntroductionPolychlorinated dibenzo-p-dioxins/dibenzofurans (PCDD/F), or dioxins as they are commonly referred to, are classified as persistent organic pollutants (POPs) under the Stockholm Convention. Due to their chemical stability and high fat solubility, these chemicals can accumulate within food chains and pose exposure/health risks to humans through consumption of food items (i.e., diary, meat, and fish). Regulations are in place to monitor food and feed for the presence of dioxins to protect the population.1 Current maximum levels allowable for PCDD/Fs in food and feedstuffs are at the pg·g-1 concentration range due to the toxicity risk they pose.2,3 However, the European Commission has announced plans to lower the current maximum levels in certain feedstuffs in 2024 based an updated risk assessment.4 As of 2014, a change of EU regulations permitted the use of gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) for the analysis of food and feed as an alternative to GC–high-resolution mass spectrometry (GC-HRMS).5,6 With the proposed lowering of some maximum levels, performance of current instrumentation to achieve these targeted limits must be assessed.Achieving these targeted limits places further stress on laboratories in maintaining consistent sensitivity to detect the trace levels of dioxins in difficult food matrices. Another challenge for analysts is the time-consuming data assessment based on regulatory requirements for PCDD/F analysis. Often the necessary tools for PCDD/F quantification (i.e., isotopic dilution quantification) and reporting of regulatory requirements (ion ratio, calibration, and response factor deviation)7,8 do not exist within a single software. This requires analysts to export to external packages (i.e., Microsoft™ Excel™ ) to perform critical calculations leading to transcription errors and added time for reporting. In addition, laboratories must ensure they produce consistent data throughout the analytical run to avoid reanalysis or re-extraction when sample/extract material is limited.In this analysis, the performance of the TSQ 9610 triple quadrupole GC-MS/MS system equipped with the Thermo Scientific™ NeverVent™ advanced electron ionization (AEI) source was used to demonstrate compliance for regulatory limits for PCDD/F in food and feed samples in accordance with EU Regulations. Food and feed samples were provided by the European Union Reference Laboratory for halogenated Persistent Organic Pollutants in feed and food (EURL POPs) (Germany) and Wageningen Food Safety Research, in their capacity as National Reference Laboratory for POPs (NRL POPs, The Netherlands). These samples contained known trace levels of dioxins previously confirmed at the respective institutes or in international proficiency tests. The aim of this analysis was to ensure results were consistent with the previously determined concentrations in food and feed matrices and meet current compliance with the EU regulations.ConclusionThe 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 Analyzer eWorkflow, can deliver reliable regulatory-compliant performance for the quantification and confirmation of PCDD/Fs food and feedstuffs:<ul><li>Femtogram level sensitivity performance for ultra trace level determination of PCDD/F within food and feed samples.</li><li>Check standard performance was within quantitation and ion ratio thresholds for regulatory method compliance at femtogram levels.</li><li>Accurate and precise quantitation at maximum levels and action thresholds for PCDD/F in food and feed.</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.</li><li>Chromeleon eWorkflows, available from Thermo Fisher Scientific also provide error-free execution of each analysis to meet standard operating procedure (SOP) requirements, further simplifying the user experience.</li></ul><h4>4. LECO: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Basil_Comparison_GC_G_Cx_GC_TOFMS_LHF_MDCW_24_LPSS_315_Joe_Binkley_4223f2122d/Basil_Comparison_GC_GCxGC_TOFMS_LHF_MDCW24_LPSS-315-Joe-Binkley.pdf">Characterization and Comparison of Basil Before and After Drying Using GC, GCxGC, and TOFMS</a></h4><ul><li>Poster</li></ul>INTRODUCTIONGC and MS are well-established techniques for the characterization of food, beverage, and flavor samples. Extending the analytical separation to two dimensions with comprehensive two-dimensional gas chromatography (GCxGC) enhances the peak capacity, allows for exploring more complex samples, and allows for determining more individual analytes within complex samples. TOFMS adds to these benefits and often leads to the identification for these isolated analytes, supporting non-target analyses where analytes of interest and importance can be determined through data evaluation. When coupled together, the benefits are often greater than the sum of the individual techniques.Software tools that compare sets of GCxGC samples facilitate these analyses and can effectively reveal useful information from the rich data. In this work, we evaluate the aroma characteristics for basil before and after drying. This type of characterization can be useful for quality control, product development, and batch comparisons, as well as understanding the sensory profile changes associated with curing.CONCLUSIONSIn this work, LECO’s TGM800 was used to determine the moisture level of fresh and cured basil samples and LECO’s Pegasus BT4D GCxGC-TOFMS with ChromaTOF Tile were used to highlight differences between the chemicals which contribute to the sensory profiles of fresh and cured basil. This provided a better understanding of the aroma characteristics of these samples. Many differences were observed between the samples and the analytical tools used in this work were crucial for their determination.

News from LabRulezGCMS Library - Week 42, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 18th November 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applications and posters by Agilent Technologies, Thermo Fisher Scientific, Metrohm, and Shimadzu!<h4>1. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/5991_9356_EN_590f86441b.pdf">Determination of Carbonate Solvents and Additives in Lithium Battery Electrolyte Using the Agilent 5977B GC/MSD</a></h4><ul><li>Application</li></ul>AbstractThis application note describes a method for determining carbonate solvents and additives in lithium battery electrolyte using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=5977B">Agilent 5977B</a> single quadrupole gas chromatography/mass selective detector (GC/MSD). In this method, direct liquid injection is adopted. At a split ratio of 20:1, the target compounds achieved good linearity in a concentration range of 10–500 mg/L. This method has excellent reproducibility, and the instrument detection limits (IDL) for all of the 15 target compounds analyzed were below 1.3 mg/L. During the analysis of the actual electrolyte samples, diluted injection can be used to accurately quantify the target compounds and qualitatively identify unknown additives or impurities.IntroductionLithium battery electrolyte is the carrier of ion transport in a lithium battery, which is generally composed of lithium salt and organic solvent. In the electrolyte, the commonly used lithium salt is LiPF6 , and the solvent is a binary, ternary, or multinary system composed of a mixture of cyclic carbonates and chain carbonates. Selecting the right organic electrolyte is the key to achieving a higher energy density, a longer cycle life, and greater battery safety. Lithium battery manufacturers also add specific additives to extend battery life. Therefore, studies on the composition of lithium battery electrolyte play an important role in the development of new lithium batteries.GC/MS analysis is commonly used in the studies on lithium battery electrolyte, and can accurately and quantitatively analyze the major components of the organic solvent in the electrolyte. Meanwhile, the strong qualitative capacity of mass spectrometry can also qualitatively identify and analyze unknown additives and impurities.This application note describes the method for determining carbonate and carboxylate solvents and additives in lithium battery electrolyte using the 5977B GC/MSD. In regard to the fact that LiPF6 , the main component of the electrolyte, is unstable and can easily decompose, diluted injection was adopted, which ensured good sensitivity, linearity, and reproducibility.ConclusionIn this application note, a method for analyzing carbonate solvents and additives in lithium battery electrolyte was developed with an Agilent 7890 GC and Agilent 5977B GC/MSD. The method is easy to use, and can achieve great separation, a wide linear range, and excellent reproducibility and sensitivity for various components in the electrolyte, making it very suitable for qualitative and quantitative analysis of organic solvents, additives, and impurities in lithium battery electrolyte.<h4>2. Shimadzu / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/292">AOAC</a>: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Th_P264_ASMS_poster_pesticide_GC_MSMS_beb4879814.pdf">Simultaneous Analysis of Pesticides in Food With GC-MS/MS Using Hydrogen Carrier Gas</a></h4><ul><li>Poster / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Th_P264_ASMS_poster_pesticide_GC_MSMS_beb4879814.pdf">AOAC</a></li></ul>IntroductionIn GC-MS/MS analysis, helium gas is generally used as the carrier gas; however, in recent years the shortage of supply and the soaring price of helium gas have resulted in a need to pivot to other options. To address this problem, hydrogen gas is being used as an alternative carrier gas. The characteristics of hydrogen gas are different from those of helium gas, however, and methods using helium gas must be adjusted to appropriate conditions for hydrogen gas. We have developed a quantitative analysis method for 216 pesticides with GC-MS/MS using hydrogen gas. Using this method, good recovery results were obtained in food samples.ConclusionsUsing hydrogen gas as an alternative carrier gas, we simultaneously analyzed 216 food-borne agrochemicals using an ultra-sensitive triple-quadrupole mass spectrometer <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-TQ8050+NX">GCMS-TQ8050 NX</a> combined with AOC-30i and AOC-20s U as injectors.Good recovery rate within 70 ~ 120% were obtained for 70% to 74% of the compounds. This system enables simultaneous analysis of multiple pesticides with high sensitivity and accuracy.<h4>3. Thermo Fisher Scientific / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/170">RAFA</a>: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PFAS_analysis_strategy_story_direct_injection_DLLME_LC_MS_MS_LC_Orbitrap_GC_Orbitrap_7592743c1a.pdf">PFAS analysis strategy story – direct injection, DLLME, LC-MS/MS, LC- Orbitrap / GC-Orbitrap</a></h4><ul><li>Poster / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/170">RAFA</a></li></ul><h5>Abstract</h5>Purpose: This work summarizes key components of PFAS analysis. The choice between direct injection and automated sample preparation depends on the instrument's dynamic range, detection limits, and matrix complexity. Complex matrices like waste/industrial water, soil, food, and biological samples require specific preparation techniques to mitigate matrix effects and ensure accurate quantification. Techniques such as Dispersive Liquid-Liquid Microextraction (DLLME) can significantly improve concentration factors and reduce matrix interference, enhancing overall method performance. Additionally, the choice of the analyzer is a critical consideration.Methods: Direct injection of water sample was performed on Thermo Scientific TSQ Altis Plus triple quadrupole mass spectrometer. For those sample prepared with automated dispersive liquid-liquid microextraction (DLLME), acquisition was performed on a Thermo Scientific <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=Orbitrap+Exploris+MX">Orbitrap Exploris MX</a> high resolution mass spectrometer.Results: The methods presented achieves high-level sensitivity for PFAS analysis in drinking water, detecting compounds in the low ng/L range. Using DLLME, 56 PFAS compounds were quantified to low part per trillion levels from just 15 mL of sample. With a FAPAS®-Drinking Water proficiency test, we validated the three strategies for PFAS analysis: direct injection on TSQ Altis Plus and the DLLME extract injected on both Orbitrap Exploris MX and Thermo Scientific Orbitrap Exploris GC.<h5>Conclusions</h5><ul><li>Compared to traditional SPE workflows, direct injection improves sample throughput in laboratories by significantly reducing the required sample preparation.</li><li>The DLLME method is a promising technique for extracting and pre-concentrating PFAS from drinking water and various other matrices. Its reduced sample volume facilitates easier handling, transportation, and storage.</li><li>Both methods lower costs and environmental impact due to minimal solvent usage and the elimination of filters or SPE cartridges.</li><li>The ease of use and robustness of both LCMS methods are based on fixed configuration including SOP with detailed hardware and consumables, a complete acquisition and processing method with customized view settings and reports, and all data handling performed with Chromeleon CDS 7.3.2.</li></ul><h4>4. Metrohm: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_nir_121_download_0bb1185dc9.pdf">Water content in propylene glycol monomethyl ether (PGME)</a></h4><ul><li>Application</li></ul><h5>Water determination possible within seconds using NIRS</h5>Propylene glycol monomethyl ether (1-methoxy-2-propanol, or PGME) is one of many glycol ether solvents with a wide variety of applications. It is used as an intermediate and in formulations for industrial, professional, or consumer applications, mainly in surface coatings, inks for printing, cleaning solutions, deicing/anti-icing formulations, and agrochemical purposes. It is also used as an extractant and as a coalescing agent and flow improver in water-based paints.Water in propylene glycol methyl ether is usually measured by Karl Fischer (KF) titration which requires chemicals and takes about five minutes per determination. This Application Note describes how near-infrared spectroscopy (NIRS) can be used as a faster and more cost-efficient alternative for water determination in PGME.CONCLUSIONThis Application Note demonstrates the feasibility to determine a key parameter for the quality control of propylene glycol monomethyl ether (water content) with NIR spectroscopy. The main advantages of NIR spectroscopy over wet chemical methods are that running costs are significantly lower and time-to-result is significantly reduced. Additionally, no chemicals are required, and the technique is non-destructive to samples.

News from LabRulezGCMS Library - Week 47, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 25th November 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applications and other documents by Agilent Technologies, Thermo Fisher Scientific, Shimadzu, and a poster from Analytica by LECO!<h4>1. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/AN_003378_Determination_of_sulfur_containing_compounds_formaldehyde_and_organic_halides_in_hydrogen_37d3ef50c9.pdf">Determination of sulfur-containing compounds, formaldehyde, and organic halides in hydrogen for proton-exchange membrane fuel cell vehicles</a></h4><ul><li>Application</li></ul>GoalThe goal of this application note is to demonstrate a suitable analytical method that can be applied for the determination of sulfur-containing compounds, formaldehyde, and organic halides in hydrogen used for proton-exchange membrane fuel cell vehicles in compliance with the Chinese regulation (GB/T 37244-2018) by using thermal desorption coupled to gas chromatography-mass spectrometry and sulfur chemiluminescence detection (SCD).IntroductionThe past energy crisis and global warming led researchers to find alternative cleaner and emission-free energy sources. Hydrogen has been identified as a very promising energy carrier or fuel due to its exceptional energy per mass content. The proton-exchange membrane fuel cell (PEMFC) has garnered considerable attention and represents a breakthrough technology for automotive applications due to its capability to convert hydrogen and oxygen into electricity with only water as a by-product. Studies have shown that impurities such as CO, CO2, NH3, formaldehyde, halogenated compounds, and sulfur-containing compounds in hydrogen can cause serious damage to the performance of PEMFC by reducing its service life. Therefore, an accurate assessment of hydrogen purity is extremely important. This application note is focused on the determination of sulfur-containing compounds, formaldehyde, and organic halide impurities in hydrogen gas.ConclusionThe results obtained in this study demonstrated that the Markes UNITY–CIA Advantage-xr pre-concentrator combined with the TRACE 1610 GC equipped with the SCD detector and connected to an ISQ 7610 single quadrupole mass spectrometer provides a highly performing solution for selective and sensitive analysis of some critical hydrogen impurities in compliance with the requirements of the Chinese regulation.<ul><li>R2 values were ≥ 0.995 for all the investigated compounds with linear ranges from 0.1 to 10 nmol/mol for sulfur-containing compounds, from 1 to 400 nmol/mol for formaldehyde, and from 1 to 100 nmol/mol for organic halides, with RSD of response factors well below the acceptance limit of 30%.</li><li>LODs calculated as 3.143 × S0 resulted close to 0.01 nmol/mol for sulfur-containing compounds, 0.04 nmol/mol for formaldehyde, and between 0.06 and 0.095 nmol/mol for organic halides.</li><li>Peak area repeatability was &lt;12% for all the target analytes.</li></ul><h4>2. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00745_en_c333797ed9.pdf">Analysis of Diethylene Glycol in Glycerin Using Brevis GC-2050</a></h4><ul><li>Application</li></ul>User Benefits<ul><li>The compact Brevis GC-2050 allows for high-throughput analysis by increasing the number of operational units in the lab.</li><li>Despite its small size, the Brevis GC-2050 achieves uncompromised analytical performance, enabling the analysis of concentrated glycerin in compliance with pharmacopeial standards.</li></ul>IntroductionIn response to the issue of contamination in pharmaceuticals and toothpaste with diethylene glycol, certain parts of the Japanese Pharmacopoeia were revised through Ministry of Health, Labour and Welfare Notification No. 32 (February 21, 2008). In Application News G259 “Analysis of Diethylene Glycol in Glycerin,” a measurement example conforming to the pharmacopoeial requirements is introduced using GC-2010. While each country has its own official methods, this application conducted measurements on a Brevis GC-2050 under conditions where the Split/Splitless injection unit (SPL) temperature was set higher, taking into consideration that the sample component has a high boiling point, with reference to the Japanese Pharmacopoeia.ConclusionA sample was prepared for the analysis of concentrated glycerin as described in the Japanese Pharmacopoeia, and the analysis was conducted by the condition specified in the Japanese Pharmacopoeia. Good separation and reproducibility were confirmed.<h4>3. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ebook_gcms_faq_5994_7643en_agilent_d81a1e0189.pdf">GC and GC/MS Frequently Asked Questions</a></h4><ul><li>Guide</li></ul>Table of ContentsIn this eBook, you’ll find answers to the questions that Agilent technical experts hear most often from our GC and GC/MS customers. To instantly access the information you need, click the following links or use the navigation tabs at the bottom of each page.General Knowledge<ul><li>How does chromatography work?</li><li>Why is GC column polarity important?</li><li>What is the significance of GC column dimensions?</li><li>What are the basic principles and mechanisms of GC/MS?</li><li>How do chemical and electron impact ionization differ?</li><li>What is the difference between standard, mass spec, and Ultra Inert columns?</li><li>What is headspace and how does it work?</li><li>What is the difference between split and splitless?</li><li>How do I choose the right carrier gas for my detector?</li><li>What should I consider when using hydrogen as an alternate to helium carrier gas?</li><li>How does the Agilent HydroInert source preserve spectral fidelity with hydrogen carrier gas?</li><li>What solvent is best for liquid injection on GC/MS?</li></ul>Maintenance<ul><li>How often should I change columns?</li><li>How often should I change liners?</li><li>How do I check for leaks?</li><li>When should I replace the filaments?</li><li>Can preslit vial cap septa prevent septa leakage into the inlet or sample?</li><li>I use the MS with complex matrices every day. Should I tune daily or weekly?</li><li>What chemicals should I use to perform a standard instrument check?</li><li>When replacing and conditioning a column, should I install it into the MS?</li><li>How does JetClean maximize instrument uptime and productivity?</li><li>How do I prevent loss of column efficiency and resolution?</li></ul>Method Development and Optimization<ul><li>How do I develop methods in MRM/SRM mode?</li><li>How do I select an internal standard (ISTD) for my GC/MS analysis?</li><li>How do I select the right MSD for my sample or analytical requirements?</li><li>How do I choose the right mass spectrometer?</li><li>What are the rules of thumb for choosing an inlet liner?</li><li>What is a good approach for analyzing unknown compounds?</li><li>Can I quantify GC/MS results in either scan or SIM mode?</li></ul>Troubleshooting<ul><li>How do I improve peak shape?</li><li>How do I improve resolution?</li><li>How do I improve signal-to-noise levels?</li><li>What causes spiking and how do I avoid it?</li><li>What can cause a negative peak in GC/MS?</li><li>Where do ghost peaks come from?</li><li>What can cause split peaks, peak tailing, and drifting baselines?</li><li>Why is water difficult to observe in GC and how can it be quantified using GC?</li><li>How do I determine the source of contamination within my chromatograph?</li></ul><h4>4. LECO / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/295">Analytica</a>: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Cannabis_Characterization_BT_G_Cx_GC_SA_CK_ANALYTIKA_SA_24_LPSS_317_edc6c55493.pdf">Cannabis Characterization Using GC and GCxGC with Time-of-Flight Mass Spectrometry</a></h4><ul><li>Poster (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/295">Analytica</a>)</li></ul>Cannabis is a complex plant containing a variety of naturally occurring organic compounds in a wide range of concentrations, as well as xenobiotics (i.e., polyaromatic hydrocarbons, pesticides, etc.). Among these constituents, the cannabinoids, terpenes, and terpenoids are commonly recognized for their therapeutic properties. This plant has two main subspecies—Cannabis indica and Cannabis sativa—that can be differentiated by their different physical characteristics. Indica-dominant strains are short plants with broad, dark green leaves and have higher cannabidiol content than the sativa plants in which THC content is higher. Sativa-dominant strains are usually taller and have thin leaves with a pale green colour.The legalization of this drug has also led to an increasing amount of consumer products being infused with CBD, marketed and sold for medicinal and recreational purposes. Thus, it is imperative that we are able to determine its total composition as this is important in determining potency and medical effectiveness (Entourage Effect). In this study, we use GC with Time-of-Flight Mass Spectrometry (TOF-MS) to assist in the determination of its risks and benefits. This powerful tool provides chromatographic separation with high-quality deconvoluted mass spectral data allowing for comprehensive analysis, identification, and quantification of targeted and non-targeted analytes.ConclusionGCxGC-TOFMS facilitates compound identification, Library searches, and Mass ∆ calculations. Data was used to develop maps for quantitative analysis, cannabis classification, and sample comparison. Cannabis comparison via statistical processing was performed using ChromaTOF Tile (based on Fisher ratios) and could also perform PCA analysis.

News from LabRulezGCMS Library - Week 48, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 2nd December 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applications by Agilent Technologies and Thermo Fisher Scientific, a poster from AOAC by Shimadzu, and a poster from ASMS by LECO!<h4>1. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_terpene_cannabis_gc_fid_5994_7684en_agilent_1_2d2cf2f631.pdf">Fast Analysis of 22 Terpenes in Hemp and Cannabis with the Agilent 9000 Intuvo GC with FID using Hydrogen Carrier Gas</a></h4><ul><li>Application</li></ul>AbstractThis application note describes the procedure for the analysis of 22 common terpenes in cannabis and hemp using the Agilent Intuvo gas chromatograph (GC) and flame ionization detector (FID), with hydrogen carrier gas, and post column backflush. The GC injection‑to‑injection cycle time was 10 minutes allowing for six samples per hour. A group of 1,200 hemp samples were analyzed to test the robustness of the method, and to determine a maintenance schedule.IntroductionTerpenes are the main flavor and aromatic components of cannabis and hemp. Strains can be identified by their specific fingerprint for these terpenes. The abundance of particular terpenes may also indicate the character and usefulness of a particular strain. This identification also allows cultivators to monitor the consistency of their particular strains from one crop to the next, and to maintain better quality control. With ever‑increasing varieties of cannabis flowers and the number of individual tests performed, the overall speed of analysis time has become more important.Helium has been used as the carrier gas for most GC analyses. Recent limitations on its availability have added to the cost of testing. This application focuses on a fast and robust analysis of 22 of the most common terpenes found for strain identification, as well as providing information for labeling purposes. This application utilizes hydrogen carrier gas with flame ionization detection (FID) to help shorten the analysis time and therefore, keep the cost per sample down.ConclusionThis method proved to be a very robust, high throughput method with a GC cycle time of only 10 minutes (6 samples/hour). This study showed that the regular maintenance of changing liners, septa, and Guard Chips when needed, maintained retention time and curve stability. The use of backflushing helped keep the Guard Chip and inlet cleaner and minimized maintenance.All calibration curves showed great linear response across the concentration range, through all 12 calibration standards, as seen in Figure 3.Reminders can be set up using counters to alert the analyst when maintenance is needed according to the user's desired sample load. Being careful to install the liner in the same fashion helps to keep the tolerance of the CCV results within the ± 20% limits. It is noted and shown in Figure 4 that there may be additional terpenes present in samples that are not covered by the terpenes in the standards for this application. If this is of concern, a more encompassing standard may be used. Also, using a mass spectral detector may be more beneficial for the application.2 Other matrices may require a revised maintenance schedule.<h4>2. LECO / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/296">ASMS</a>: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/NIST_LIBRARY_MATCH_QUALITY_HRT_MMS_CF_ASMS_24_LPSS_320_90d3c6e8c9.pdf">Evaluation of the NIST Library Matching Quality of Mass Spectra Generated by the GC-HR-TOFMS with Multi-Mode Ionization Source</a></h4><ul><li>Poster (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/296">ASMS</a>)</li></ul>IntroductionComparison of electron ionization spectra against standardized libraries is a staple approach to compound identification in non-targeted GC-MS analysis. High-quality matches are central to the pace of, and confidence in, such analyses. Recent developments in gas chromatography high resolution mass spectrometry have progressed non-targeted analysis applications to a wide variety of studies. However, modern ion-optical design principles which allow gains in sensitivity and resolving power may inadvertently alter fragmentation patterns, which may in turn affect the reliability of automated comparisons against standard libraries. Thus, thorough evaluation and validation of the high-quality spectra matching to the standard libraries, like NIST, is necessary for comprehensive assessment of the promised benefits of new technologies.ConclusionsThis multi-mode ionization source, as assessed using these 207 diverse analytes, generates fragmentation patterns which align very well with the NIST spectral library. Across all analytes in standard solutions, the mean library match score was 935 and the standard deviation for this value was 24.2. Mean match scores were agreeable regardless of moieties present. Percent differences for MRPS #2 spiked into a Pu’er Tea and MRPS #8 spiked into a dietary supplement were - 3.75 % and -1.44 %, illustrating how the system can easily maintain spectral confidence even in complex matrices. Overall, this study suggests the electron ionization mode of this multi-mode ion source, in combination with its high-resolution time of flight mass analyzer, yields spectra in excellent agreement with the quadruple dominated NIST library.<h4>3. Shimadzu / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/292">AOAC</a>: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/aoac_2024_1_m034_5346b45c51.pdf">Qualification and Quantification of Residual Pesticides in Ginger by GCMS using Simultaneous Ultra-fast Scan and SIM</a></h4><ul><li>Poster (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/292">AOAC</a>)</li></ul>IntroductionInterest in food safety has grown, resulting in a trend of tightening global regulations for residual pesticides in produce. Selected Ion monitoring (SIM) in GC/MS is a common technique used for pesticide analysis while Scan mode is often used in non-targeted screening.This study demonstrates a SIM analysis of pesticides, including calibration and repeatability in ginger root matrix. In addition to targeted analysis, in this work we performed simultaneous untargeted analysis with Ultra-fast Scan analysis, maximizing the use of the GCMS-QP2050. NIST library search results are shown for untargeted components.ConclusionThe GCMS-QP2050 demonstrates sensitivity and reproducibility in analyzing pesticides in produce using SIM data obtained from simultaneous Scan/SIM analysis. Ultra-fast scan supports accurate identification of target compounds alongside SIM analysis without interference. Scan results provide MS spectrum patterns for identifying unknown compounds, assisting in non-target screening.<h4>4. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_002549_gc_ms_hesaver_h2safer_epa_1668_pcbs_an002549_na_en_4b122a7fbb.pdf">Environmental analysis of polychlorinated biphenyls (PCBs) at reduced running costs using hydrogen as carrier gas</a></h4><ul><li>Application</li></ul>GoalThe aim of this application note is to compare the performance of the Thermo Scientific™ TSQ™ 9610 triple quadrupole mass spectrometer coupled to the Thermo Scientific™ TRACE ™ 1610 GC with hydrogen versus helium as the carrier gas for the determination of polychlorinated biphenyls. For guidance on the analytical performance of the proposed method, acceptance criteria as per U.S. EPA Method 1668 were considered.IntroductionPolychlorinated biphenyls (PCBs) are a group of industrial organic chemicals consisting of carbon, hydrogen, and chlorine atoms. Due to their non-flammability, chemical stability, high boiling point, and electrical insulating properties, PCBs were used in hundreds of industrial and commercial applications including electrical, hydraulic equipment, plasticizers, plastics, rubber products, and dyes. The production of these compounds has been banned in the United States since 19771 because of their persistence in the environment and their tendency to enter the food chain and bioaccumulate in living organisms due to their lipophilicity.There are currently 209 known PCBs congeners that can be divided into two groups according to their structural and toxicological characteristics:<ul><li>Non-dioxin-like PCBs (non-DL-PCBs), which represent the majority of the PCB congeners, are characterized by a lower degree of toxicity.</li><li>Dioxin-like PCBs (DL-PCBs) include the 12 most toxic congeners (non‐ortho PCBs 77, 81, 126, 169 and mono‐ortho PCBs 105, 114, 118, 123, 156, 157, 167, 189), which have structures and toxicities similar to dioxins.</li></ul>DL-PCBs are classified as persistent organic pollutants (POPs), and they have been regulated under the Stockholm Convention for POPs since 2001.2 Following the Clean Water Act (CWA) in 1972, the United States Environmental Protection Agency (U.S. EPA) developed an analytical method, U.S. EPA Method 1668 and following revisions3 that can be applied for the determination of PCBs in wastewater, surface waters, soil, sediments, biosolids, and tissue matrices using gas chromatography coupled to high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS).3 However, recent advances in gas chromatography-triple quadrupole mass spectrometry allow for high sensitivity and selectivity, leading to the consideration of GC-MS/MS as a reliable tool for PCBs analysis.This application note reproduces the experiments described in a previously published application note,4 where polychlorinated biphenyls were analyzed using helium carrier gas. Here, helium was replaced by hydrogen. Additionally, the Thermo Scientific™ HeSaver-H2Safer™ carrier gas saving technology was applied. HeSaver-H2Safer technology offers a unique solution for laboratories to minimize carrier gas consumption during both standby and operational modes. When helium is used as carrier gas, the consumption can be drastically reduced without any changes to the analytical method or deterioration of performance. However, the Split-Splitless (SSL) injector modified to work in the HeSaver-H2 Safer mode can be used also in conjunction with hydrogen as a carrier gas, where the limited and fixed carrier gas flow allows for safe usage without the need to install additional sensors. At the same time, the hydrogen gas consumption is equally reduced and will lead to further cost savings, allowing laboratories to run their instrumentation longer on a single gas tank or using gas generators.SummaryThe HeSaver-H2Safer inlet allows laboratories full flexibility to select the carrier gas of choice between helium and hydrogen, while achieving a significant reduction of the consumption. With a simple upgrade to the standard Thermo Scientific™ iConnect SSL injector, the HeSaver-H2Safer inlet allows for the use of an inert and inexpensive gas for inlet pressurization, whereas the main carrier gas flow is limited to the column flow only.<ul><li>The use of hydrogen as carrier gas has been demonstrated as an alternative to helium for the analysis of PCBs, reducing the overall cost of running the laboratory.</li><li>The use of the HeSaver-H2Safer inlet reduces the amount of hydrogen going into the gas chromatography system such that safe operation is assured anytime, and no hydrogen sensor is needed inside the GC oven.</li><li>Hydrogen did not affect the linearity range; all compounds showed a linear response from 0.1 to 2000 ppb, with avarage R 2 &gt;0.999.</li><li>The TSQ 9610 triple quadrupole mass spectrometer provided excellent IDLs with hydrogen carrier gas, comparable to those obtained with helium.</li><li>The variation of ion ratios was less than 12% for all PCBs at 0.05 ppb.</li></ul>

News from LabRulezGCMS Library - Week 49, 2024

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!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you other document by Agilent Technologies and posters by Shimadzu / ASMS, Thermo Fisher Scientific / ASMS and Waters / ASMS!<h3>1. Agilent Technologies: Understanding Solvent Focusing Gas Chromatography and How it can be Optimized for Splitless Injections&nbsp;</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">Full PDF for download</a></li></ul>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.<h4>Sample preparation and solvent selection</h4>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;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.<h4>Conclusion&nbsp;</h4>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;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.<h3>2. Shimadzu / ASMS: PFAS in Bottled Water: A Simple Approach Using HS-SPME GC/MS/MS for Volatile Contaminant Analysis</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">Full PDF for download</a></li></ul>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.<h4>Methods</h4>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">GCMS-TQ8040 NX</a> with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=AOC-6000+Plus">AOC-6000 Plus</a> multifunctional autosampler equipped with a solid phase microextraction (SPME) module (Figure 1).&nbsp;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;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;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;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.<h4>Conclusion</h4>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.<h3>3. Thermo Fisher Scientific / ASMS: Large-scale targeted biomarker analysis of volatile organic compounds in breath by TD-GC-MS&nbsp;</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">Full PDF for download</a></li></ul>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.<h4>Materials and Methods</h4>Breath samples were collected using the ReCIVA® Breath Sampler and CASPER® air supply to reduce ambient contamination. Samples were analyzed with a Markes <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=7&amp;search=TD100xr+thermal+desorber">TD100xr thermal desorber</a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/18">Thermo Scientific Orbitrap Q Exactive GC-MS system</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">Chromeleon CDS software</a> in a secure, cloud-based enterprise environment.<h4>Results</h4>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.<h4>Conclusion</h4>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.<h3>4. Waters / ASMS: GC-APCI-MS/MS Analysis of Polychlorinated Dibenzo-p-dioxins and Furans to Revised US EPA1613 Guidelines</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008849_81ffe9aec9.pdf">Full PDF for download</a></li></ul>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.<h4>Materials and Methods</h4>Analysis was carried out using a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/55">Waters Xevo TQ-XS tandem quadrupole MS</a> 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">Agilent 8890 GC</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=8&amp;search=CIS-4+PTV">Gerstel CIS-4 PTV injector</a>, with autosampling via <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=PAL+3+RSI">PAL 3 RSI</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.<h4>Results</h4>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.<h4>Conclusion</h4>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.

News from LabRulezGCMS Library - Week 27, 2025

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European Symposium on Analytical Spectrometry (ESAS) 2026

2026 AOAC INTERNATIONAL Annual Meeting & Exposition

Shimadzu at 2026 AOAC Annual Meeting & Exposition

Correlating Mechanical and Chemical Properties: Introduction to Rheo-Raman for Polymers

From Legacy Workflows to Paperless Labs: Track Every Sample, Process, and Decision

Modern Methods for Faster Microbial Analysis