<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 22nd July 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p>
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<h4>👉 <a href="https://gcms.labrulez.com/library"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></a></h4>
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<p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p>
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<p>This week we bring to you poster presentations from <a href="https://gcms.labrulez.com/events/568"><strong>ASMS 2024</strong></a> by <strong>LECO</strong>, <strong>Agilent Technologies</strong>, and <strong>Thermo Fisher Scientific</strong>! And as a bonus two application notes from <strong>Shimadzu</strong> and <strong>Thermo Fisher Scientific</strong>.</p>
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<p>💡 <strong>+ 100 ASMS posters and presentations <a href="https://gcms.labrulez.com/library?mainauthorItems=284">available in the LabRulezGCMS library</a></strong> (unique search and filtering)</p>
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<h4><strong>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></strong></h4>
<ul>
<li>poster - ASMS 2024</li>
</ul>
<p><strong>Introduction:</strong> 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.</p>
<p><strong>Conclusions:</strong> The Pegasus BTX GC(GCxGC)-TOFMS with a novel Long-Lifetime Ion Detector has demonstrated the following performance characteristics:</p>
<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><strong>2. Thermo Fisher Scientific: <a href="https://gcms.cz/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></strong></h4>
<ul>
<li>poster - ASMS 2024</li>
</ul>
<h5><strong>Abstract</strong></h5>
<p><strong>Purpose:</strong> 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.</p>
<p><strong>Methods:</strong> 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.</p>
<h5><strong>Conclusions</strong></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 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.</li>
</ul>
<h4><strong>3. Agilent Technologies: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/po_142_utilizing_hydrogen_pesticides_food_gc_ms_po142_asms2024_en_7ed0951b93.pdf">Analyzing Nitrosamines with Hydrogen Carrier Gas: GC/MS/MS Analysis of Nitrosamines in Sartan Drugs</a></strong></h4>
<ul>
<li>Poster Reprint - ASMS 2024</li>
</ul>
<p><strong>Introduction:</strong> The limited availability of helium has been a concern, leading to a growing interest in switching to alternative carrier gases like hydrogen. Hydrogen offers several advantages over helium1 , including faster run times and improved chromatographic resolution. Helium is commonly used as a carrier gas for analyzing nitrosamine impurities in pharmaceuticals. However, there are concerns that nitrosamines may react with hydrogen, forming unwanted byproducts. To ensure that using hydrogen as a carrier gas does not impact spectral quality, we evaluated its suitability for analyzing eight impurities:</p>
<ul>
<li>N-nitrosodimethylamine (NDMA),</li>
<li>N-nitrosomethylethylamine (NMEA),</li>
<li>N-nitrosodiethylamine (NDEA),</li>
<li>N-nitroso-ethylisopropylamine (NEIPA),</li>
<li>N-nitrosodiisopropylamine (NDIPA),</li>
<li>N-Nitrosodipropylamine (NDPA),</li>
<li>N-nitrosodi-n-butylamine (NDBA),</li>
<li>N-Nitrosopiperidine (NPIP).</li>
</ul>
<p>Hydrogen carrier gas was used with the 7000E and 7010 Series GC/TQ systems equipped with the HydroInert and HES ion sources respectively, assessing spectral quality, linearity, repeatability, recovery, and compliance with nitrosamine analysis regulations.</p>
<p>MassHunter 13 software suite provided the tools for data acquisition and processing to be performed under a unified compliance environment. OpenLab Electronic Content Management (ECM) XT includes native tools to facilitate compliance, including the ability to create users with affiliated permissions, the generation of audit trails, and remote data storage.</p>
<p><strong>Conclusions:</strong></p>
<ul>
<li>The 7000E and 7010 Series GC/TQ systems equipped with the HydroInert and HES, respectively, exhibited exceptional performance in determining eight nitrosamine drug impurities in sartan drug products and substances using hydrogen carrier gas.</li>
<li>The method was validated at 30 ppb with acceptable recovery and long-term repeatability. </li>
<li>The 7010 Series GC/TQ system enabled a smooth switch between helium and hydrogen carrier gas without compromising the performance of the methods. </li>
<li>Both the HydroInert and the HES sources facilitated achieving the necessary detection limits for the tested impurities.</li>
</ul>
<h4><strong>4. Agilent Technologies: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/po_142_utilizing_hydrogen_pesticides_food_gc_ms_po142_asms2024_en_7ed0951b93.pdf">Analysis of Essential Oils Using a Comprehensive GCxGC with a Reverse Flow Modulator Combined with High Resolution GC/MS</a></strong></h4>
<ul>
<li>Poster Reprint - ASMS 2024</li>
</ul>
<p><strong>Introduction:</strong> Essential oils are typically analyzed to determine their chemical composition contributing to flavor and quality as well as to evaluate their authenticity and identify adulterants. Essential oils are often complex samples with high number of volatile and semi-volatile components that include many isomers with highly similar spectra and close Retention Indices (RIs) when separated on a single column. Hence, a comprehensive GCxGC approach is preferable to achieve an appropriate chromatographic separation for this sample matrix. In this study we used comprehensive GCxGC coupled to a high-resolution accurate mass GC/MS to identify the essential oil  components. Here we also investigate approaches for comparison of the complex GCxGC essential oil data.</p>
<p><strong>Conclusions:</strong></p>
<ul>
<li>Several comprehensive GCxGC configurations and method using the high-resolution GC/Q-TOF and RFM were developed and optimized using a diesel sample. </li>
<li>Essential oils were analyzed using the optimized GCxGC approach, and the workflows for compound identification and statistical analysis were evaluated.</li>
</ul>
<h4><strong>5. Shimadzu: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/an_01_00746_en_e14cf49b7b.pdf">Greenhouse Gas Analyzer</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>User Benefits:</strong></p>
<ul>
<li>Simultaneously measures the 3 main greenhouse gases: CH₄, CO₂, and N₂O.</li>
<li>Offers short analysis cycle times and is equipped with an AOC-6000 Plus syringe injection system to analyze large numbers of samples.</li>
<li>Uses nitrogen as a carrier gas for lower running costs.</li>
</ul>
<p><strong>Introduction:</strong> Greenhouse gases are a major cause of climate change, and carbon dioxide, (CO₂), methane (CH₄), and nitrous oxide (N₂O) are considered the 3 primary greenhouse gases. Although CO₂ accounts for the majority of greenhouse gas emissions followed by CH₄, reducing CH₄ emissions is considered important because CH₄ has a warming effect that is more than twenty times greater than CO₂. At the United Nations Climate Change Conference (COP26) in November 2021, over 100 countries joined the Global Methane Pledge, which pledges by 2030 to reduce global CH₄ emissions by 30 % compared to 2020 levels. The Greenhouse Gas Analyzer is a gas chromatography system that has been developed by Shimadzu in collaboration with the National Agriculture and Food Research Organization (NARO) (Fig. 1). Measuring levels of CH₄, CO₂, and N₂O simultaneously in a single sample is difficult, but the Greenhouse Gas Analyzer has been designed to do this simultaneously, which reduces analytical errors and improves the sampling speed, giving researchers a valuable tool in reducing greenhouse gas emissions.</p>
<p>This Application News describes using the Greenhouse Gas Analyzer to simultaneously measure CO₂, CH₄, and N₂O levels.</p>
<p><strong>Conclusion:</strong> The Greenhouse Gas Analyzer can simultaneously measure 3 greenhouse gases in atmospheric air in a single analysis. Each analysis by the Greenhouse Gas Analyzer is performed in 8 minutes with an analysis cycle time of 10 minutes.</p>
<h4><strong>6. Thermo Fisher Scientific: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/an_002695_gc_triplus_rsh_smart_sample_prep_environ_an002695_na_en_77a5aa2300.pdf">An automated approach for the analysis of VOCs in drinking and surface water by using the TriPlus RSH SMART VOC Sample Prep Station</a></strong></h4>
<ul>
<li>Application - Environmental</li>
</ul>
<p><strong>Goal:</strong> The aim of this study is to demonstrate the suitability of the Thermo Scientific™ TriPlus™ RSH SMART VOC Sample Prep Station for the analysis of volatile organic compounds (VOCs) in drinking and surface water by using a fully automated sample preparation workflow.</p>
<p><strong>Keywords:</strong> Automated sample preparation, TriPlus RSH SMART Sample Prep Station, volatile organic compounds, VOCs, drinking water, surface water, gas chromatography, TRACE 1610 GC, single quadrupole mass spectrometry, ISQ 7610 GC-MS.</p>
<p><strong>Conclusions:</strong> The results of these experiments demonstrate that the automated sample preparation capability of the TriPlus RSH SMART VOC Sample Prep Station coupled to the ISQ 7610 GC-MS system provides an ideal solution for water testing laboratories looking to improve productivity and deliver confident results.</p>
<ul>
<li>Static headspace is a convenient solventless extraction technique for volatiles in water with almost no sample preparation required. </li>
<li>Unattended operations of up to 210 samples can be achieved with the automated calibration dilution and ISTD addition workflows.</li>
<li>The automated addition of fresh reagent just before the incubation increases the stability of ISTD/surrogates mix, therefore improving the accuracy of the quantitation of target analytes during data reprocessing.</li>
<li>The TriPlus RSH SMART VOC Sample Prep Station ensures increased sample integrity for highly reliable quantitative analysis, and reduced errors or possible cross-contaminations, maximizing the productivity of the laboratory. Additionally, it allows saving valuable analyst time and improving safety by limiting the user’s exposure to toxic chemicals. </li>
<li>The integrated control for both autosampler and GC-MS in a single CDS ensures a streamlined automated workflow from on-line sample preparation to sequence setup, data acquisition, and reporting. </li>
<li>Suitability of headspace sampling for analysis of VOCs was demonstrated with R2  &gt; 0.990, RRF %RSD &lt; 20%, and calculated amount within 20% of the spiked concentration. </li>
<li>Inter-day reproducibility was demonstrated by running three batches of samples bracketed with QCs. Average absolute peak area %RSD across the entire evaluation period was &lt;20%, the QC calculated amount was within 20% of the expected value, and the calculated recovery was within 70–130%, with the only exception of 1,2-dibromo-3-chloropropane for which the % recovery was 132. </li>
<li>Reliable quantitative analysis was achieved for drinking water samples and surface water samples analyzed in three different batches across six working days. All the sample results were compliant with the thresholds set by the current EU regulation.</li>
</ul>


News from LabRulezGCMS Library - Week 30, 2024

<p><strong>Christmas are time of the year to celebrate and reflect on the year gone by, and to catch up with friends or family (or both). What better way to do it, than over your favourite drink (alcoholic or not). Coming from Scotland, my go-to festive tipple has always been Whisky (yes, that’s the way we spell it).&nbsp;</strong></p><p>A drink with such popularity, complexity and let’s be honest – some high price tags! Walk through any airport and marvel at the choice on offer and of course some eye watering prices. It’s a revered spirit with a history as rich as its flavor, has always been synonymous with tradition, craftsmanship, and quality. However, the increasing demand for premium whisky has led to a surge in adulteration practices, posing significant challenges for consumers and producers alike.&nbsp;</p><p>In this blog, we delve into the intricacies of whisky adulteration and explore how cutting-edge technology, specifically the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/472"><strong>Thermo Scientific Orbitrap Exploris GC 240 mass spectrometer</strong></a>, is revolutionizing the fight against counterfeit whisky and ensuring your Christmas cheer is genuine.</p><figure class="image"><img style="aspect-ratio:1024/512;" src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_The_Spirit_of_Christmas_Ensuring_the_Quality_and_Authenticity_of_Whisky_3_33aa2173ac.jpg" alt="Thermo Fisher Scientific: The Spirit of Christmas - Ensuring the Quality and Authenticity of Whisky" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_The_Spirit_of_Christmas_Ensuring_the_Quality_and_Authenticity_of_Whisky_3_33aa2173ac.jpg 245w," sizes="100vw" width="1024" height="512"></figure><h3 id="h-understanding-whisky-adulteration" data-uw-rm-heading="level" role="heading" aria-level="2"><strong>Understanding whisky adulteration</strong></h3><p>Whisky adulteration can take several forms, each compromising the integrity of the spirit.</p><ol><li><strong>Artificial Whisky Creation: </strong>This involves mixing various chemicals to mimic the flavor and aroma of genuine whisky. The absence of safety controls over the quality and concentration of these chemicals raises health concerns.</li><li>&nbsp;Bottles may be falsely labelled with more expensive brands or incorrect maturation periods. This type of adulteration often involves adding artificial colours or using heat to accelerate the aging process, giving the appearance of a well-aged whisky without the time investment.</li></ol><p>For the consumer its hard, or even impossible, to distinguish between a budget blended whisky and a genuinely aged single malt whisky. Furthermore, how could you tell if a whisky had been aged for 10 years or 25 years (apart from the higher price). You can see the economic motivation for the whisky fraudster.</p><h3 id="h-the-role-of-advanced-technology"><strong>The role of advanced technology</strong></h3><p>To combat these sophisticated adulteration techniques, a robust and precise analytical approach is essential. The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/472"><strong>Orbitrap Exploris GC 240</strong></a>, combined with <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/order/catalog/product/36SP03M5"><strong>headspace solid-phase microextraction (SPME Arrow)</strong></a><strong> </strong>via the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/422"><strong>Thermo Scientific TriPlus RSH SMART Autosampler</strong></a>, offers a powerful solution for the comprehensive characterization of whisky.</p><h3 id="h-workflow-for-finding-the-differences"><strong>Workflow for finding the differences</strong></h3><p>The workflow shown in figure 1 for differential analysis of whisky using the <strong>Orbitrap Exploris GC 240 mass spectrometer</strong> is straightforward yet highly effective:</p><ol><li><strong>Sample Preparation:</strong> Whisky samples (100 µl) are aliquoted directly into vials and mixed with water (900 µl). After heating, SPME Arrow was used to sample from the vial headspace, which allows for efficient extraction of volatile compounds.</li><li><strong>Chemical Profiling: </strong>The samples are analyzed in EI full scan at 120,000 mass resolving power (FWHM m/z 200) using the Orbitrap Exploris GC 240. This provides comprehensive high-resolution and accurate mass data that enables the detection of subtle differences in the chemical profiles of different whisky samples.</li><li><strong>Data Analysis: </strong>The data is processed using <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/mass-spectrometry/liquid-chromatography-mass-spectrometry-lc-ms/lc-ms-software/multi-omics-data-analysis/compound-discoverer-software.html"><strong>Thermo Scientific Compound Discoverer software</strong></a>, which incorporates a high-resolution accurate mass flavor and fragrance library. This facilitates the identification of compounds and comparison between samples.</li></ol><figure class="image"><img style="aspect-ratio:602/257;" src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_The_Spirit_of_Christmas_Ensuring_the_Quality_and_Authenticity_of_Whisky_2_dbdc69f6e0.jpg" alt="Thermo Fisher Scientific: Figure 1. Workflow from left to right showing how from data acquisition in full scan we move from peak detection, to identifying unique components in a sample, to finally making a compound identification." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_The_Spirit_of_Christmas_Ensuring_the_Quality_and_Authenticity_of_Whisky_2_dbdc69f6e0.jpg 245w," sizes="100vw" width="602" height="257"></figure><h3 id="h-case-study-identifying-adulteration"><strong>Case study: identifying adulteration</strong></h3><p>In the study reported in application note 003094: “Non-targeted analysis of whisky using <strong>SPME Arrow</strong> and <strong>Orbitrap Exploris GC 240 mass spectrometer</strong>”, the differential analysis of whisky samples revealed significant insights (figure 2). The principal component analysis plot for whiskies of different age statement shows clear chemical differences between the samples. We can dive deeper into the data to see what compounds drive that difference. For instance, comparing sample 2 and sample 3 the results highlighted compounds unique to sample 2, such as higher levels of 2,3 – methyl-1-butanol and Furfural. These compounds are typically associated with Scotch malt whisky and indicate a longer and different maturation process, suggesting that sample 2 is a genuine aged whisky compared to sample 3.</p><figure class="image"><img style="aspect-ratio:602/350;" src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_The_Spirit_of_Christmas_Ensuring_the_Quality_and_Authenticity_of_Whisky_9d095fe6dc.jpg" alt="Thermo Fisher Scientific: Figure 2. Principal component analysis loading plot of whisky samples based on identified chemical profile from Compound Discoverer software." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_The_Spirit_of_Christmas_Ensuring_the_Quality_and_Authenticity_of_Whisky_9d095fe6dc.jpg 245w," sizes="100vw" width="602" height="350"></figure><h3 id="h-ensuring-quality-and-authenticity"><strong>Ensuring quality and authenticity</strong></h3><p>As the whisky market continues to grow, the importance of ensuring quality and authenticity cannot be overstated. Advanced analytical technologies like the <strong>Orbitrap GC-MS</strong> provide a <strong>powerful tool</strong> in the fight against whisky adulteration. By leveraging these technologies, producers can uphold the tradition and integrity of whisky, ensuring that every bottle delivers the genuine experience that consumers expect and deserve.</p><p>Whether you are a whisky enthusiast or a producer, understanding and utilizing these advanced technologies is key to preserving the heritage and quality of this beloved spirit.</p><p>So cheers, or as we say in Scotland “Slàinte Mhath” to authenticity and innovation in the world of whisky!</p><blockquote><section><h4><strong>Dominic Roberts</strong></h4><div itemprop="description">Dominic Roberts has been closely involved with the Thermo Scientific GC Orbitrap MS since its launch in 2015. He started at Thermo Fisher Scientific as a Senior Applications Specialist for the product and is currently the GC Orbitrap MS Product Marketing Manager. Dominic is an experienced analytical chemist and mass spectrometrist with more than 20 years of experience using state-of-the-art analytical systems. He has worked in both a regulatory and industrial environment with GC–MS and LC–MS systems to investigate a variety of chemicals in food, biological, and environmental samples.</div></section></blockquote>

The Spirit of Christmas: Ensuring the Quality and Authenticity of Whisky

<h3><strong>Too much interfering matrix? Discover how to streamline your daily LC-MS analysis with turbulent flow chromatography.</strong></h3><p><strong>Sample preparation is a critical step in liquid chromatography-mass spectrometry (LC-MS) analysis to achieve quantitative accuracy and precision. Directly injecting crude samples into your instrument without prior cleanup to remove interfering compounds can clog the flow path, damage your detector, and negatively impact your analyses through a “matrix effect.”</strong></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Automated_LC_MS_Sample_Cleanup_Using_Turbulent_Flow_Chromatography_c7647c2c50.jpg" alt="Thermo Fisher Scientific: Automated LC-MS Sample Cleanup Using Turbulent Flow Chromatography." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Automated_LC_MS_Sample_Cleanup_Using_Turbulent_Flow_Chromatography_c7647c2c50.jpg 245w," sizes="100vw" width="1024" height="512"></p><p>Common approaches to clean up samples and suppress the matrix effect include simple dilution and centrifugation to extensive extraction techniques. The common scope of all these procedures is to minimize the possible contamination of your LC-MS system but, more importantly, to reduce to a minimum the interference of unrelated sample components on the detection and quantification of your analytes of interest.</p><p>A point to note is the preparation method you choose often depends on the complexity of your sample. For instance, samples for clinical research applications or toxicology tend to have high levels of interfering matrix and require a more sophisticated clean-up approach.&nbsp; Let’s dive into what a matrix effect is, the impacts on your LC-MS data, and an effective method called turbulent flow chromatography you can use to clean complex samples.<sup>1</sup></p><h3 id="h-what-exactly-is-matrix-effect"><strong>What exactly is matrix effect?</strong></h3><p><strong>Any chemical entity in your sample capable of coeluting or interacting with analytes of interest can generate matrix effect, ultimately impacting the integrity of your data.</strong></p><p>Interfering matrix compounds come from endogenous and exogenous sources, but biological samples like blood or serum, and food and environmental extracts inherently have higher levels of interfering compounds.</p><p>Some examples of interfering matrix compounds include ion-suppressing salts, proteins, lipids, compounds capable of ion-pairing interactions, and polymers.</p><h3 id="h-how-does-matrix-effect-impact-your-lc-ms-data"><strong>How does matrix effect impact your LC-MS data?</strong></h3><p>Because matrix compounds interfere with the detection and quantitation of your target analytes, the effects ultimately lead to an <strong>under- or overestimation in analyte quantification.</strong></p><p>In the case of LC-MS, the matrix effect triggers ion suppression<sup>2</sup>, which happens when compounds from the sample matrix inhibit charge transfer from the ion source to your target analytes – a prime example is electrospray ionization, where the detection relies on efficient charge transfer to analytes.</p><p>Analytes and matrix components will naturally compete for the available charge from the MS ion source. And when compounds of your sample matrix are present in higher concentrations than your analytes, these unwanted molecules can capture more of the charge, leaving fewer ions available for charge transfer to your analytes.</p><p><strong>Hence suppression of charge transfer to your analytes leads to poor accuracy and limits of detection and quantitation.</strong></p><h3 id="h-sample-preparation-methods-to-remove-interfering-matrix"><strong>Sample preparation methods to remove interfering matrix</strong></h3><p>Using the example of ion suppression, you can see how eliminating the competition for charge transfer between matrix components and analytes through proper sample cleaning is essential to developing a method with quantitative accuracy.</p><p><strong>Solid-Phase Extraction (SPE) and Liquid-Liquid Extraction (LLE) are techniques used to clean samples before LC-MS analysis.</strong><sup> 3,4</sup></p><ul><li>In <strong>SPE</strong>, a liquid sample is loaded onto a column packed with a solid adsorbent material. The analytes of interest are retained on the adsorbent material while unwanted matrix components are washed away. The retained analytes are then eluted using a solvent. This approach is typically developed on a specific panel of target analytes.</li><li><strong>LLE </strong>is based on the differential solubility of analytes between two immiscible solvents; once a partition equilibrium is reached, the enriched solvent is separated and, usually, evaporated to dryness and reconstituted in a solvent compatible with LC-MS.</li></ul><p>Regardless of the <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/chromatography/chromatography-learning-center/chromatography-consumables/sample-prep.html"><strong>sample preparation</strong></a> approach you decide to use, these manual procedures are imprecise, time-consuming, and labor-intensive—even a quick and easy cleanup is subject to human errors like improper pipetting or sample mix-up.</p><h3 id="h-automated-online-sample-cleanup-for-efficient-sample-preparations"><strong>Automated online sample cleanup for efficient sample preparations</strong></h3><p>To overcome the bottlenecks and risks of manual approaches, automated sample cleanup is gaining popularity, thanks to much less human intervention combined with better speed and analytical reproducibility.</p><p><strong>Online SPE</strong>&nbsp;is an improvement over manual ones, where the extraction process integrates directly with your LC system. The sample is automatically injected onto an extraction cartridge, cleanup occurs, and your extracted sample transfers directly to the MS instrument (flow injection analysis) or to an analytical column for further separation and detection.</p><p><strong>Turbulent flow chromatography</strong> (TurboFlow) is a more advanced online sample cleanup approach combining the aspects of the <strong>chemical affinity of SPE with size exclusion chromatography </strong>(SEC).<sup>5</sup></p><h3 id="h-how-does-turbulent-flow-chromatography-work"><strong>How does turbulent flow chromatography work?</strong></h3><p>TurboFlow separates low molecular weight molecules from high molecular weight matrix components using a specialized sample extraction column on LC systems (<strong>Figure 2</strong>).</p><p><strong>Here’s a detailed look at how TurboFlow works</strong>:</p><ol><li>Your sample is directly injected into a <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/order/catalog/product/CH-952434"><strong>TurboFlow column</strong></a> (typically large<strong> &gt; 50 µm particle size </strong>with macropores).</li><li>The sample flows through the column at high linear velocities, creating turbulence to enhance the interaction between the sample components and the stationary phase.</li><li>Low molecular weight molecules diffuse into the pores faster than high molecular weight components and quickly flush to waste. Only the small molecules with an affinity for the particle chemistry bind to the internal pore surfaces.</li><li>A change in mobile phase composition elutes the small molecules bound by the TurboFlow column for further separation and detection.</li></ol><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Automated_LC_MS_Sample_Cleanup_Using_Turbulent_Flow_Chromatography_3_a261253a52.jpeg" alt="Thermo Fisher Scientific: Figure 1. Illustration showing how turbulent flow chromatography works." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Automated_LC_MS_Sample_Cleanup_Using_Turbulent_Flow_Chromatography_3_a261253a52.jpeg 245w," sizes="100vw" width="1024" height="512"></p><h3 id="h-benefits-of-turbulent-flow-chromatography-for-sample-preparation-over-spe"><strong>Benefits of turbulent flow chromatography for sample preparation over SPE</strong></h3><p>While both TurboFlow and online SPE streamline and automate the sample preparation process, TurboFlow has key differences and advantages to consider (Figure 2).</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Automated_LC_MS_Sample_Cleanup_Using_Turbulent_Flow_Chromatography_4_221b9dda9b.jpg" alt="Thermo Fisher Scientific: Figure 2. TurboFlow vs. SPE for sample cleanup." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Automated_LC_MS_Sample_Cleanup_Using_Turbulent_Flow_Chromatography_4_221b9dda9b.jpg 245w," sizes="100vw" width="700" height="410"></p><ol><li><strong>TurboFlow provides a cleaner sample compared to SPE</strong><ul><li>The more efficient dual mode of action (chemical affinity plus SEC)</li><li>The elution performed by a strong solvent plug potentially reduces the transfer of residual matrix components to your MS</li></ul></li><li><strong>A cleaner sample means</strong><ul><li>Reduced ion suppression, leading to increased sensitivity</li><li>Less mass spectrometer contamination</li><li>Extended analytical column lifespan</li><li>Faster analytical gradients</li></ul></li></ol><p>Moreover, the opportunity to modulate the strength of the mobile phase reaching the analytical column allows for better analyte focusing on the head of the column, significantly improving your chromatography.</p><h3 id="h-streamline-your-daily-lc-ms-analysis-with-turboflow-technology"><strong>Streamline your daily LC-MS analysis with TurboFlow technology</strong></h3><div style="grid-template-columns:auto 60%;"><div><p>Automated sample cleanup using <a target="_blank" rel="noreferrer noopener" aria-label="online TurboFlow technology - open in a new tab" data-uw-rm-ext-link="" uw-rm-external-link-id="https://assets.thermofisher.com/tfs-assets/cmd/brochures/br-74120-lc-ms-transcend-uhplc-systems-br74120-en.pdf$onlineturboflowtechnology"><a target="_blank" rel="noopener noreferrer" href="https://assets.thermofisher.com/TFS-Assets/CMD/brochures/br-74120-lc-ms-transcend-uhplc-systems-br74120-en.pdf"><strong>online TurboFlow technology</strong></a></a> is a rapid and efficient sample preparation approach that considerably improves method accuracy, reliability, and sensitivity.<br><br>Adopting this technology can even enhance the competitiveness of your laboratory by allowing faster results, lower costs per sample, and improved reproducibility and MS sensitivity.</p><figure class="image"><img style="aspect-ratio:700/410;" src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Automated_LC_MS_Sample_Cleanup_Using_Turbulent_Flow_Chromatography_2_0a20492c6a.jpg" alt="Thermo Fisher Scientific: Figure 3. Transcend TLX TurboFlow UHPLC System." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Automated_LC_MS_Sample_Cleanup_Using_Turbulent_Flow_Chromatography_2_0a20492c6a.jpg 245w," sizes="100vw" width="700" height="410"></figure><blockquote><p><a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/chromatography/liquid-chromatography-lc/hplc-uhplc-systems/transcend-turboflow-tlx-systems.html"><strong>Learn how TurboFlow can ease your lab’s daily LC-MS analysis of complex matrices today</strong></a><strong>.</strong></p></blockquote><article aria-label="Automated LC-MS Sample Cleanup Using Turbulent Flow Chromatography"><div><blockquote><p><strong>Visit us on </strong><a target="_blank" rel="noreferrer noopener" aria-label="LinkedIn: - open in a new tab" data-uw-rm-ext-link="" uw-rm-external-link-id="https://www.linkedin.com/showcase/72003132/admin/dashboard/$linkedin:"><a target="_blank" rel="noopener noreferrer" href="https://www.linkedin.com/showcase/72003132/admin/dashboard/"><strong>LinkedIn:</strong></a></a> #TurbulentflowChromatography #lcms #IonSuppression</p></blockquote></div></article><section><blockquote><h4>Dan Kalu Appulage</h4><p>Dr. Dan Kalu Appulage is a Product Management Specialist in the HPCS business unit at Thermo Fisher Scientific. He holds a Ph.D. in Analytical Chemistry, an M.A., and B.S. in Chemistry. His professional background includes expertise in product management, LCMS method development, and teaching. Dan is passionate about education and loves sharing his knowledge and experiences with others. Outside of work, Dan enjoys playing volleyball and traveling with his family.</p></blockquote></section></div></div>

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