<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>

Automated LC-MS Sample Cleanup Using Turbulent Flow Chromatography

<h3><strong>Part 4: Going beyond 4D to improve analytical performance for targeted quantitative analysis</strong></h3><p><strong>This is the fourth in a multi-part blog series highlighting the key attributes and impressive benefits of the Thermo Scientific Stellar mass spectrometer—the first-of-its-kind instrument designed and optimized for highly multiplexed targeted quantitation, ideally suited for discovery verification. By delivering robust analytical methods and dramatically improved turnaround time, this solution helps labs boost capacity and differentiate themselves to generate more revenue. For additional background, see blog </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/article/5077"><strong>Part 1</strong></a><strong>, </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/article/5086"><strong>Part 2 </strong></a><strong>and </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/article/5416"><strong>Part 3</strong></a><strong> here and stay tuned for more blogs on our website.</strong></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Why_You_Need_a_Verification_Class_Mass_Spectrometer_Going_Beyond_4d_to_Improve_Analytical_Performance_for_Targeted_Quantitative_Analysis_125258804e.jpg" alt="Thermo Fisher Scientific: Why You Need a Verification-Class Mass Spectrometer: Going Beyond 4d to Improve Analytical Performance for Targeted Quantitative Analysis." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Why_You_Need_a_Verification_Class_Mass_Spectrometer_Going_Beyond_4d_to_Improve_Analytical_Performance_for_Targeted_Quantitative_Analysis_125258804e.jpg 245w," sizes="100vw" width="1200" height="600"></p><p>Analytical specificity is one of the most critical requirements for successful targeted quantitative analysis. Assigning measured data to diagnostic product ions from the analyte of interest increases the confidence in resulting measurement determining the analyte expression level, copy number, or absolute amount in each sample, as well as across an entire study. Using empirically determined values for liquid chromatography (LC) and mass spectrometry (MS) provides specific information that collectively increases data processing. This orthogonal information comes in the form of <strong>1) </strong>chromatographic retention times and peak shapes; <strong>2) </strong>precursor <i>m/z</i> value; <strong>3)</strong> MS/MS product ions; and <strong>4)</strong> MS/MS product ion distribution profiles, which can be stored to form spectral libraries that are used to not only process LC-MS<sup>n</sup> data but build confident targeted data acquisition methods.</p><h3><strong>4D parameter determination: Sufficient or not?</strong></h3><p>Previous publications touted utilization of four-dimensional (4D) parameter determination to confidently create and process untargeted and targeted data. Using LC coupled to a trapped ion mobility QTOF (timsTOF) mass spectrometer, each analyte is annotated by four empirical measurements across all study samples: 1) measured retention time; 2) ion mobility as measured by its collision cross section (CCS); 3) precursor <i>m/z</i> value; and 4) presence of corresponding product ions. The assumption is that the orthogonal selectivity achieved by UHPLC separation and ion mobility resolution relative to the precursor isolation is sufficient to differentiate a specific analyte from co-eluting isobaric and isomeric ions and that resulting product ions are only attributed to the isolated precursor. <a target="_blank" rel="noopener noreferrer" href="https://arxiv.org/pdf/2111.03134">Adding CCS values can help accommodate for some variability</a> but requires more work by the researcher to accurately determine the variance associated with ion mobility. <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/1885960_lcms_179_lipidomics_short_gradient_ebook_rev_01_ed630faf92/1885960-lcms-179-lipidomics-short-gradient-ebook-rev-01.pdf">At no point are the product ion ratios used as an additional dimension for verification</a>.</p><p><strong>A smart addition: product ion ratio determination</strong><br>Product ion ratio determination, however, has been used as the gold standard for qualitative data analysis for SRM/MRM acquisition for decades. Despite quantitative methods on triple quadrupole mass spectrometers acquiring data for only two or three product ion transitions, the inclusion of the resulting product ion ratio is used to qualitatively verify that the signal measured per SRM transition is attributed to the analyte of interest. This concept has been included in the targeted quantitative studies performed using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1149"><strong>Thermo Scientific Stellar mass spectrometer (MS)</strong></a>, significantly increasing analytical performance for a wide range of molecules.</p><p>To increase the quantitative selectivity and specificity needed for confident data acquisition, the proposed solution combines the chromatographic separation capabilities of the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products?category=40&amp;search=vanquish"><strong>Thermo Scientific Vanquish UHPLC system </strong></a>with the innovative PRM acquisition on the<strong> Stellar mass spectrometer </strong>to go beyond data processing confidence.&nbsp; Additionally, the proposed method leverages intelligent data acquisition to perform RT alignment reducing the need to apply additional post-acquisition data processing steps.&nbsp; This blog covers the differentiation for each of these steps while presenting an important 5<sup>th</sup> dimension—extending PRM data analysis to the MS<sup>3</sup> level.</p><h3><strong>Dimension #1: Leveraging 1,500 bar UHPLC separation to drive orthogonal selectivity</strong></h3><p>Using the<strong> </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Thermo Scientific Vanquish Neo</strong></a> and<strong> </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/744"><strong>Horizon UHPLC</strong></a><strong> systems</strong>, researchers can harness higher backpressure capabilities covering a wide range of flow rates from nanoflow to analytical flow rates—increasing peak capacity while driving higher utilization rates than HPLC systems with only 1,000 bar of backpressure. T<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products?category=40&amp;search=vanquish"><strong>he Vanquish UHPLC systems</strong></a> also deliver reproducible performance over the course of longer studies such as populational health.</p><p><strong>Going beyond the first dimension</strong>: Including the Adaptive RT routine enables LC mapping to assign true retention time values to each analyte with narrower retention time windows. The Adaptive RT routine works for small and large molecules, from single-cell to bulk analysis, and bridges method development between longer discovery gradients and faster targeted quantitation gradients without the need for spiked RT standards.&nbsp; The advantage is that the retention time alignment for the study is reliably performed during data acquisition, not processing.</p><h3><strong>Dimension #2: Introduction of targeted analytes</strong></h3><p>Following UHPLC separation and ionization, targeted analytes (precursors) are introduced into the MS and moved through the ion flight path to the detector. The quadrupole mass filter (termed isolating quadrupole or Q1) has an RF/DC offset to transmit a narrow <i>m/z</i> range centered on the target precursor <i>m/z</i> value. The mass range used for precursor ion filtering is <i>ca.</i> 1 to 2 Th depending on the mass spectrometer. Leveraging precursor isolation following chromatographic separation increases the target analyte selectivity relative to co-eluting compounds.</p><p><strong>Going beyond the second dimension:</strong> The Stellar mass spectrometer’s QR5 Plus quadrupole mass filter uses hyperbolic-surfaced quadrupole rods that improve ion transmission efficiency across a wider precursor <i>m/z</i> range. Unit resolution settings are 0.7 Th at the baseline—significantly better than other quadrupole mass spectrometers using 1.2 to 2 Th (almost 2-3x wider), which can compromise quantitative performance.</p><h3><strong>Dimension #3: Acquiring PRM data from more product ions</strong></h3><p>The<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1149"><strong> Stellar mass spectrometer </strong></a>acquires PRM data which is comprised of full scan MS<sup>2</sup> spectra per scan event relative to SRM/MRM acquisition. Acquiring data for many more product ions per unit time increases the specificity of the resulting measurement. It also enables post-acquisition data processing methods to determine specific product ions used for quantitation without having to update the experimental method and re-analyze samples.</p><p><strong>Going beyond the third dimension:</strong>&nbsp; The Stellar mass spectrometer combines the unique capabilities of dual ion packet management with ion accumulation outside of the ion trap to boost quantitative performance.&nbsp; Simultaneously managing two different ion packets enables longer accumulation times without significantly compromising the PRM acquisition rates which becomes imperative when performing quantitative measurements at the LOD and LOQ levels.</p><h3><strong>Dimension #4: Leveraging the full scan MS<sup>2</sup> spectrum and multiple product ions to evaluate the product ion ratios compared to a reference spectrum</strong></h3><p>As mentioned above, ion ratio calculations are used in validated quantitative methods to ensure selectivity relative to the matrix or background interference per product ion.</p><p><strong>Going beyond the fourth dimension:</strong> What, where and how you perform ion accumulation differentiates the effectiveness of each mass spectrometer. The Stellar MS first filters for the targeted precursor <i>m/z</i> value, then accumulates product ions in an ion-routing multipole (as has been done on Thermo Scientific Orbitrap mass spectrometers for over a decade).&nbsp; Performing tandem MS in this order maximizes sensitivity for low-level product ions to maintain accurate ion ratio analysis. Finally, incorporating dynamic AGC automates the accumulation time regardless of precursor ion flux. (Reference: <a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1101/2024.06.04.597431">Plubell et al. BioRxiv</a>)</p><h3><strong>Dimension #5: Addressing sensitivity disrupters</strong></h3><p>Targeted quantitation for specific analytes using MS<sup>2</sup> acquisition may have co-eluting isomeric/isobaric ions potentially disrupting quantitative sensitivity (signal-to-noise limitation).&nbsp; Two options to pursue would be modifying LC gradients or increasing the tandem MS level to MS<sup>3</sup>. Elongating the LC gradient decreases sample throughput yet still may not remove all background interferences. The Stellar MS, on the other hand, can implement MS<sup>3</sup> acquisition with exceptionally fast acquisition speeds (up to 40 Hz) to maintain target capacity and the number of data points per LC peak.</p><p><strong>Going beyond the fifth dimension</strong>:&nbsp;In addition to the unique MS<sup>3</sup> acquisition speed, the Stellar MS implements dynamic AGC to maximize spectral quality across a wider dynamic range, as well as the ability to perform either HCD or CID at each MS<sup>n</sup> level. Finally, introduction of Adaptive RT to confidently manage scheduled retention time windows ensures tMS3 methods can succeed for increased target capacity using faster LC gradients.</p><blockquote><p>For more information, explore the <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-systems/orbitrap-lc-ms/stellar-mass-spectrometer.html">Stellar mass spectrometer</a> and <a target="_blank" rel="noopener noreferrer" href="https://assets.thermofisher.com/TFS-Assets/CMD/brochures/eb-003672-lsms-stellar-2024-year-in-review-eb003672-na-en.pdf">download our new 2024 year in review ebook</a>.</p><p><strong>Visit us on </strong><a target="_blank" rel="noopener noreferrer" href="https://www.linkedin.com/showcase/72003132/admin/dashboard/"><strong>LinkedIn:</strong></a><strong> </strong>#StellarMassSpectrometer #Vanquish #UHPLC</p></blockquote><section><blockquote><h5><strong>Dr. Scott Peterman</strong></h5><div>Scott Peterman, Ph.D., is Senior Product Marketing Manager for Life Science Mass Spectrometry of the Chromatography and Mass Spectrometry Division of Thermo Fisher Scientific.</div></blockquote></section>

Why You Need a Verification-Class Mass Spectrometer: Going Beyond 4d to Improve Analytical Performance for Targeted Quantitative Analysis

News from LabRulezLCMS Library - Week 22, 2025

Folin-Ciocâlteu, RP-HPLC (reverse phase-high performance liquid chromatography), and LC-MS (liquid chromatography-mass spectrometry) provide complementary information for describing cider (Malus spp.) apple juice

<p><strong>At the forefront of global anti-doping efforts, the Laboratoire Anti-Dopage Français (LADF) plays a critical role in ensuring fair play and integrity in elite sports. We spoke with Dr. Magnus Ericsson, Director of LADF and a leading expert in analytical chemistry, to explore how the lab detects banned substances, manages high-throughput workflows, and leverages advanced Thermo Fisher Scientific technologies to stay ahead of constantly evolving challenges in anti-doping science.</strong></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Inside_Laboratoire_Anti_Dopage_Francais_LADF_An_Interview_with_Director_Dr_Magnus_Ericsson_6aca8272d5.jpg" alt="Thermo Fisher Scientific: Inside Laboratoire Anti-Dopage Français (LADF): An Interview with Director Dr. Magnus Ericsson" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Inside_Laboratoire_Anti_Dopage_Francais_LADF_An_Interview_with_Director_Dr_Magnus_Ericsson_6aca8272d5.jpg 245w," sizes="100vw" width="1024" height="512"></p><article><div><h3><strong>Screening and confirmation: A rigorous two-step approach</strong></h3><p>Every year, LADF analyzes tens of thousands of biological samples using a workflow aligned with World Anti-Doping Agency (WADA) guidelines. This two-step process—screening and confirmation—forms the backbone of modern doping analysis.<br><br>During the screening phase, high-throughput, non-targeted assays detect a broad spectrum of compounds. This aligns with recent advancements in mass spectrometry that allow LC-HRAM (high-resolution accurate mass) systems to scan for hundreds of substances in a single run, ensuring rapid and comprehensive coverage of the WADA Prohibited List <sup>(1)</sup>.<br><br>Suspicious samples then undergo confirmation testing using validated targeted methods that meet WADA’s stringent sensitivity and specificity criteria. LADF employs the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/485"><strong>Thermo Scientific TSQ 9610 Triple Quadrupole GC-MS/MS system</strong></a> for this task. Introduced in 2023, this triple quadrupole instrument has already supported the analysis of over 40,000 urine samples, ensuring reliable confirmatory data.<br><br><i>“The TSQ 9610 mass spectrometer has helped us to improve our workflow in the lab,”</i> says Dr. Ericsson. <i>“We started using it in 2023 and today we have analyzed more than 40,000 samples… with great success.”</i><br><br>Implementation of <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/77"><strong>Thermo Scientific TraceFinder software</strong></a> has also enabled seamless software continuity with LADF’s existing LC-MS and GC-MS platforms—minimizing training needs and ensuring consistent operations.</p><h3><strong>Unlocking historical insights with retrospective analysis</strong></h3><p>Modern anti-doping labs benefit not just from real-time detection but also from retrospective analysis, enabled by HRAM technology. LADF leverages the high-resolution <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/403"><strong>Thermo Scientific Orbitrap Exploris 120 mass spectrometer</strong></a> to re-mine stored HRAM data and search for newly -banned substances.<br><br>This capability aligns with a broader trend in doping control. HRAM instruments now routinely provide resolution &gt;60,000 FWHM and mass accuracy &lt;2 ppm, allowing researchers to revisit past datasets and identify emerging doping agents without reanalyzing physical samples (1).<br><br><i>“Working with high-resolution mass spectrometry, we have the possibility to go back and search in previously analyzed data,” </i>Dr. Ericsson explains.<br><br>Retrospective analysis is becoming increasingly vital as WADA continues to expand its list of monitored substances.</p><h3><strong>Speeding up turnaround times without sacrificing accuracy</strong></h3><p>During major competitions, laboratories are under intense pressure to deliver results rapidly. LADF tackles this challenge using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/742"><strong>Thermo Scientific Vanquish Duo UHPLC</strong></a> paired with the Orbitrap Exploris 120 mass spectrometer, enabling parallel workflows and multiplexed analyses in 96-well formats.<br><br><i>“We are able to save maybe a couple of hours of time. And this is a huge benefit for us,”</i> notes Dr. Ericsson.<br><br>Recent advances support this approach. New UHPLC and HRAM technologies allow scan-to-scan polarity switching at &gt;1 Hz, making it possible to detect a wide array of acidic and basic substances simultaneously—significantly speeding up comprehensive screening workflows <sup>(1)</sup>.</p><h3><strong>Building toward a one-stop shop</strong></h3><p>LADF aims to become a true “one-stop shop” for anti-doping services—mirroring Thermo Fisher Scientific’s role as their trusted, all-in-one partner for laboratory technologies by consolidating their analytical infrastructure under a single provider.<br><br><i>“It’s nice to have a one-stop shop… which means that you work mostly with one major provider,” </i>says Dr. Ericsson.<br><br>Thermo Fisher Scientific has delivered leading technologies for the analysis of performance-enhancing drugs and other prohibited substances for more than a quarter century. In line with its commitment to advance the field, the technologies the company offers bolster the analytical arsenal of doping control laboratories, enabling them to provide multiple perspectives to enhance the reliability of results.<br><br>This strategic alignment not only reduces system fragmentation and compatibility issues but also enables rapid method implementation and consistent training across staff. Such standardization is key as doping tests grow more complex, involving both small molecules and peptide-based substances.</p><h3><strong>Looking ahead: The future of anti-doping analysis</strong></h3><p>As doping methods evolve, so must detection technologies. LADF continues to invest in instruments that deliver robustness, low maintenance, and ultra-sensitivity.<br><br><i>“It’s the sensitivity and the selectivity… and the possibility to increase the selectivity by doing, for instance, different MS/MS experiments,”</i> says Dr. Ericsson.<br><br>The industry trend supports this need. New approaches like stable isotope-labeled (SIL) internal standards, supercritical fluid chromatography (SFC), and top-down proteomics with Thermo Scientific Orbitrap instruments are being developed to quantify complex peptides and detect gene doping or biologics <sup>(1)</sup>.<br><br>In addition, growing concerns around unintentional doping—via contaminated supplements, food, or even environmental exposure—are pushing labs to adopt even higher sensitivity assays and more advanced data interpretation protocols <sup>(1)</sup>.<br><br>With a clear vision and cutting-edge technology, LADF is not only keeping pace with modern anti-doping demands but also setting a gold standard for scientific excellence in sport. Discover <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/forensics/antidoping.html">Thermo Fisher Scientific’s anti-doping solutions</a> and <a target="_blank" rel="noopener noreferrer" href="https://view.highspot.com/viewer/be96860291ab6345fc58cc95d9bc3156">watch Dr. Ericsson’s complete testimonial here.</a></p><h3><strong>Additional resources</strong></h3><ul><li>Video – <a target="_blank" rel="noopener noreferrer" href="https://www.youtube.com/watch?v=-8zRtsRkAcU">Mass Spectrometry Enables Top WADA Lab to Beat the Cheats: Athlete Doping Control</a></li><li>BBC Video – <a target="_blank" rel="noopener noreferrer" href="https://www.bbc.com/storyworks/connecting-the-dots/thermo-fisher">How can technology maintain sports integrity?</a></li><li>Testimonial – <a target="_blank" rel="noopener noreferrer" href="https://www.youtube.com/watch?v=mi1VHutyqPA">LCH Ludovic Bailly-Chouriberry Testimonial video for TSQ Altis Plus MS</a></li><li><a target="_blank" rel="noopener noreferrer" href="https://assets.thermofisher.com/TFS-Assets/CMD/Technical-Notes/tn-000304-ms-testosterone-human-serum-faims-tn000304-en.pdf">TN000304 – Analysis of testosterone from human serum using FAIMS technology</a></li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/tn_001896_gc_ms_gc_ms_ms_tsq_9610_steroids_urine_tn001896_na_en_d1fd813050/tn-001896-gc-ms-gc-ms-ms-tsq-9610-steroids-urine-tn001896-na-en.pdf">TN001896 – Staying ahead of regulations for the analysis of steroids in urine with GC-MS/MS</a></li></ul><blockquote><p><strong>Visit us on&nbsp;</strong><a target="_blank" rel="noopener noreferrer" href="https://www.linkedin.com/showcase/72003132/admin/dashboard/"><strong>LinkedIn:</strong></a>&nbsp;#Antidoping, #LADF, #WADA, #SportsIntegrity</p></blockquote></div></article><section><blockquote><h4><strong>Ema Ruzic</strong></h4><p>Vertical Marketing Manager, Chromatography and Mass Spectrometry Division (CMD)</p></blockquote></section>

Inside Laboratoire Anti-Dopage Français (LADF): An Interview with Director Dr. Magnus Ericsson

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 29th September 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application note by <strong>Agilent Technologies </strong>and posters by<strong> Shimadzu / AOAC, Thermo Fisher Scientific </strong>and <strong>Waters Corporation / AOAC!</strong></p><h3><strong>1. Agilent Technologies: Comparison of Dual Sorbent Solid Phase Extraction for PFAS Applications</strong></h3><p><strong>Using dual-phase Agilent </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Bond+Elut+PFAS+WAX"><strong>Bond Elut PFAS WAX/ Carbon S SPE</strong></a><strong> cartridges for US EPA Method 1633</strong></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_1633_wax_carbon_s_spe_comparison_5994_8291en_agilent_8bdc559ad8.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Many laboratories have opted to combine polymeric weak anion exchange (WAX) and graphitized carbon black (GCB) into single solid phase extraction (SPE) cartridges to streamline sample preparation and facilitate automation for the determination of Per- and Polyfluoroalkyl Substances (PFAS) in environmental samples. This modification is acceptable under Section 1.5 of US EPA Method 1633, if the method's quality control metrics are met.1 The Agilent PFAS WAX and Carbon&nbsp;S sorbents are specifically manufactured for PFAS applications and are lot-tested to ensure low PFAS residue and maximum recovery.2,3 Packing these sorbents into standard 6 mL SPE cartridges with low PFAS residue frits makes them ideally suited for automated methods requiring both WAX extraction and carbon matrix reduction. The extraction performance of the dual-phase Agilent Bond Elut PFAS WAX/Carbon&nbsp;S SPE cartridges are comparable to other commercial cartridges. This ensures seamless integration into existing workflows while assuring optimal performance for PFAS applications.</p><h4><strong>Experimental&nbsp;</strong></h4><p>Extraction recoveries using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Bond+Elut+PFAS+WAX"><strong>Bond Elut layered 200 mg PFAS WAX (top)/50 mg Carbon S (bottom) SPE cartridges</strong></a> (part number 5610-2237) were compared to two other commercial 200 mg WAX/50 mg GCB dual-phase cartridges (Table 1). Four replicate extractions were performed with each sorbent, except for benchmark B, where only two replicates were extracted. The target compounds included the 40 listed in Method 1633, spiked at a low-level concentration of 4 ng/L in 250 mL of reagent water. Target recoveries were quantified using 24 isotope-labeled extracted internal standards (EIS). Extractions were carried out using automated SPE. Method details were described in a previous application note.4</p><h4><strong>Conclusion&nbsp;</strong></h4><p>Dual-phase Agilent Bond Elut PFAS WAX/Carbon S SPE cartridges are specifically manufactured for PFAS applications, with rigorous lot testing to ensure PFAS cleanliness and recovery. They enable efficient streamlined sample preparation and automation for EPA Method 1633. PFAS target and extracted internal standards recoveries are comparable to other dual-phase SPE cartridges, facilitating easy integration into existing EPA Method 1633 workflows.</p><h3><strong>2. Shimadzu / AOAC: Analysis of Per- and Polyfluoroalkyl Substances (PFAS) in Drinking Water and Milk using LC-MS/MS coupled with Online-SPE Interface</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/aoac_2025_t009_835132523a.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Per- and Polyfluoroalkyl Substances (PFAS) are a chemical group of organic fluorinated compounds, and perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) are representative compounds. They have been used in applications such as water repellents, surface treatment agents, fire extinguishers, and coatings. PFAS are known to be widely present in the environment and wildlife due to their stable structure. Concerns about human exposure through diet have led various countries to conduct investigations into food contamination by PFAS.</p><p>We have examined a quantitative analysis method for 43 PFAS in tap water, drinking water, and milk, and developed a pretreatment and analysis method that realized labor and time savings using LC-MS/MS and automatic pretreatment equipment (Fig.1). For extraction from milk, the QuEChERS method was used with reference to the FDA method.</p><h4><strong>Experimental</strong></h4><ul><li><strong>Automatic pretreatment equipment: </strong>SPL-W100 (AiSTI SCIENCE)</li><li><strong>LC-MS/MS:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-8060RX"><strong>LCMS-8060RX</strong></a> (Shimadzu)</li></ul><h4><strong>Conclusion</strong></h4><ul><li>LC-MS/MS methods were developed to analyze 43 PFAS in 11 minutes using automatic pretreatment, saving time and labor.</li><li>We conducted recovery tests by adding samples to tap water, drinking water, and milk, and achieved the LOQ set by EPA regulations and AOAC criteria for all compounds.</li><li>The quantitative values of the four main components in tap water were PFOA 0.00109 <span>μ</span>g/kg, PFNA 0.00044 <span>μ</span>g/kg, PFHxS 0.0004 <span>μ</span>g/kg and PFOS 0.00063 <span>μ</span>g/kg. PFAS was not detected above the detection limit in drinking water and milk.</li></ul><h3><strong>3. Thermo Fisher Scientific: High-Throughput and Highly Selective Quantitative Lipidomics with the Stellar Mass Spectrometer – A Novel Hybrid Nominal Mass Instrument</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_unil_stellar_lipidomics_metsoci_2025_po_en_730b1c19fd.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The increasing prevalence of metabolic disorders underscores the need for robust, high-throughput clinical lipid panels and lipidomics methods to quantify lipid species comprehensively, with high precision and selectivity . Structurally related lipids, with varying fatty acid composition, were associated with distinct metabolic consequences and proven to have different biological roles. Thereby, measuring individual lipid species with highest selectivity possible is crucial for corroboration of clinical utility including the improved risk prediction and diagnostics. We present an advanced methodology leveraging the unique capabilities of the new Stellar mass spectrometer. This nominal mass instrument addresses current limitations in specificity and throughput by enabling fast acquisition parallel reaction monitoring, and revolutionizing lipidomics workflows by delivering unprecedented specificity and quantitation. This system combines a quadrupole and a dual cell linear ion trap that significantly improves the ion accumulation efficiency and scan speed. This allows for the acquisition of full MS2 spectra including multiple transitions, thus improving the annotation specificity by resolving isomeric lipids and structurally similar species. This unique capacity of Stellar MS positions it as a practical solution for translational research, biomarker discovery and clinical lipidomics where rapid, sensitive and selective lipid quantitation is essential.</p><h4><strong>Materials and Methods&nbsp;</strong></h4><h5><strong>Sample Preparation&nbsp;</strong></h5><p>Dried UltimateSPLASH ONE internal standard mixture (100 µL) was reconstituted in 25 µL of NIST human plasma SRM 1950 followed by the addition of 125 µL of isopropanol for lipid extraction. The supernatant was then transferred to LC vials for LC-MS analysis. Linearity assessment: different volumes of Avanti Research UltimateSPLASH ONE internal standard mixture (0.5, 1, 5, 10, 50, 100, and 500 µL) were evaporated to dryness, followed by the reconstitution with 25 µL NIST Plasma and 125 µL of isopropanol for lipid extraction.&nbsp;</p><h5><strong>Data Acquisition&nbsp;</strong></h5><p>Plasma lipid extracts were separated on a ACQUITY Premier BEH Amide column (1.7um, 100 mm x 2.1 mm I.D., Waters) and analyzed using a targeted LCMS lipidomics approach on <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/742"><strong>Thermo Scientific Vanquish Duo UHPLC system</strong></a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1149"><strong>Stellar mass spectrometer</strong></a> (Figure 1) 1 . This method was built from a well-established selected reaction monitoring (SRM) method that we Converted to a parallel reaction monitoring (PRM) method by using only the unique precursors. As there are many isomeric lipids sharing the same mass, converting the method for the Stellar reduced 1,019 (579 positive mode; 440 negative mode) SRM precursors to 524 (233 positive mode; 291 negative mode) PRM precursors.</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>By integrating LipidCreator with Stellar MS, we expanded on an already thorough lipid workflow by increasing the number of targeted lipids (&gt;50%) and transitions (&gt;3/molecule) enabling higher confidence in lipid identification&nbsp;</li><li>Multiple transitions per precursor, combined with fast scan speeds, enhanced both the specificity and accuracy of lipid quantification, particularly for isomeric species.&nbsp;</li><li>Employing both HCD and CID simultaneously allowed for more robust characterization of sphingomyelins seen in the 2-3 transitions per species.&nbsp;</li><li>This high throughput, targeted approach addresses key limitations and provides a efficient platform for biomarker discovery&nbsp;</li><li>Also, look for our other poster showing a high-throughput targeted MS3 approach has been optimized on the Stellar MS, for the semi-quantification of TG species in human plasma.</li></ul><h3><strong>4. Waters Corporation / AOAC: From Coop to Carton: A Study of PFAS in Backyard &amp; Store-Bought Eggs Using Automation and LC-MS/MS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009037_6848187630.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Consumers often view backyard chicken eggs as a healthier alternative to store-bought eggs. However, environmental factors such as contaminated soil, water, feed, and bedding may expose backyard chickens to per- and polyfluoroalkyl substances (PFAS). This study set out to compare PFAS levels in eggs from backyard flocks with those in cage-free eggs purchased from grocery stores. The challenge was to analyze whole egg—a dense protein- and fat-rich matrix—efficiently and reproducibly. To address this, an automated sample preparation workflow was developed, reducing analyst involvement, minimizing variability, and ensuring robust results.</p><h4><strong>Methods</strong></h4><p>The workflow combined automated extraction (CEM EDGE) with automated solid-phase extraction (PromoChrom SPE-03) using dual-phase <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/215"><strong>Oasis GCB/WAX cartridges</strong></a> designed for PFAS. Key steps included:</p><ul><li>Homogenizing whole eggs and spiking with internal standards.</li><li>Automated alkaline extraction cycles followed by nitrogen-assisted concentration.</li><li>SPE cleanup with GCB/WAX cartridges to remove matrix interferences.</li><li>Analysis by LC-MS/MS using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>Waters ACQUITY Premier system</strong></a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/554"><strong>Xevo TQ Absolute mass spectrometer</strong></a>.</li></ul><p>This approach enabled preparation in less than 15 minutes per sample, while the SPE system processed up to eight samples simultaneously in under 70 minutes. Altogether, the workflow provided consistent recoveries across a broad range of PFAS, including EU-regulated compounds such as PFOA, PFOS, PFNA, and PFHxS.</p><h4><strong>Conclusions</strong></h4><p>Automated sample preparation and SPE enabled reproducible, high-throughput analysis of PFAS in whole eggs—a challenging matrix. Results showed that backyard eggs generally contained higher PFAS concentrations and a wider variety of compounds than store-bought eggs, reflecting greater environmental exposure. In contrast, grocery store eggs contained certain PFAS precursors, suggesting possible legacy contamination. The method proved robust for both regulated and emerging PFAS, with recoveries in the acceptable 70–130% range. This workflow offers laboratories a reliable, future-proof solution for PFAS monitoring in foods, helping to ensure consumer safety and regulatory compliance.</p>

News from LabRulezLCMS Library - Week 40, 2025

<p><strong>Mineral oil hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) have moved from niche laboratory concerns to central topics in food safety, regulatory policy, and analytical science.</strong></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_MOSH_MOAH_Analysis_Technology_Regulation_and_the_Road_Ahead_2_f79d1ed4ee.jpg" alt="Thermo Fisher Scientific: MOSH/MOAH Analysis - Technology, Regulation, and the Road Ahead" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_MOSH_MOAH_Analysis_Technology_Regulation_and_the_Road_Ahead_2_f79d1ed4ee.jpg 245w," sizes="100vw" width="1200" height="600"></p><p>These compounds—originating from sources such as environmental pollution, lubricants, processing aids, and migration from packaging materials—can enter the food chain and accumulate in both raw ingredients and finished products.</p><ul><li><strong>MOSH</strong> are saturated hydrocarbons, which can accumulate in human tissues but are generally considered of lower toxicological concern.</li><li><strong>MOAH</strong> contain aromatic rings, including polycyclic structures; certain high-ring MOAH are suspected to have genotoxic and carcinogenic properties, making them a priority for regulatory control.</li></ul><p>Growing public awareness, coupled with scientific research and legislative pressure, is pushing the food industry toward more robust monitoring and testing.</p><h4><strong>The evolving regulatory landscape</strong></h4><p>For years, MOSH/MOAH testing lacked consistent rules across jurisdictions. Different countries and organizations used their own limits and methods, creating confusion for global supply chains. Over the last decade, several important steps have brought the field closer to harmonization:</p><h5><strong>2017 – EN 16995 (CEN)</strong></h5><ul><li>The first standardized method for quantifying MOSH and MOAH in foodstuffs using LC-GC-FID technology.</li></ul><h5><strong>2023 – JRC Guidelines v2</strong></h5><ul><li>Expanded scope to include food contact materials, with refinements in sample preparation and measurement.</li></ul><h5><strong>2024 – ISO 20122:2024</strong></h5><ul><li>A dedicated standard for fats and oils, integrating clean-up procedures alongside LC-GC-FID to improve accuracy.</li></ul><h5><strong>Ongoing – EURL/ISO initiatives</strong></h5><ul><li>Collaborative efforts including interlaboratory studies, method refinement, and the potential adoption of GC×GC–MS for enhanced selectivity and molecular insight.</li></ul><p>A major development still in progress is the <strong>EU’s draft regulation for maximum residue limits for MOAH</strong>. Expected after 2024, it could introduce strict, enforceable thresholds across the single market, forcing a step-change in testing capacity and method validation.</p><h4><strong>Analytical challenges in MOSH/MOAH testing</strong></h4><p>Although standardized methods exist, MOSH/MOAH analysis is not a straightforward “plug-and-play” process. Laboratories face several persistent challenges:</p><h5><strong>Complex sample matrices</strong></h5><ul><li>Edible oils, processed foods, and packaging extracts contain a mix of natural compounds such as carotenoids, terpenes, and squalene. These can overlap chromatographically with MOSH/MOAH peaks, making quantification more difficult.</li></ul><h5><strong>False positives and overestimation</strong></h5><ul><li>Non-MOSH/MOAH compounds can mimic the target analytes, especially in less selective detection modes, leading to inflated results.</li></ul><h5><strong>Low detection limits</strong></h5><ul><li>Many regulations demand quantification in the low mg/kg range. Achieving this requires both clean sample extracts and highly sensitive analytical instrumentation.</li></ul><h5><strong>Reproducibility across labs</strong></h5><ul><li>Differences in sample handling, clean-up techniques, and instrument tuning can lead to significant interlaboratory variation, complicating compliance and enforcement.</li></ul><p>These challenges mean that achieving <strong>accuracy, repeatability, and regulatory compliance </strong>requires optimized workflows that combine precision sample preparation with advanced chromatographic techniques.</p><h4><strong>A modern workflow: from sample to result</strong></h4><p>State-of-the-art MOSH/MOAH workflows are typically built around an <strong>LC-GC-FID</strong> platform supported by automated sample preparation. This integration reduces human error, improves throughput, and delivers reproducible results.</p><h5><strong>Step 1: saponification</strong></h5><p>Fats can overwhelm LC columns, limiting injection volumes and obscuring MOSH/MOAH peaks. Saponification removes these fats, enabling:</p><ul><li>Larger injection volumes.</li><li>Clearer chromatographic baselines.</li><li>Lower quantitation limits without compromising peak integrity.</li></ul><h5><strong>Step 2: epoxidation</strong></h5><p>For MOAH analysis, carotenoids, terpenes, and other naturally occurring compounds must be removed. Epoxidation—now most commonly performed using PFA reagents—cleans up these interferences while maintaining the integrity of aromatic hydrocarbons.</p><h5><strong>Step 3: evaporation and concentration</strong></h5><p>By concentrating the hexane extract after saponification, laboratories can:</p><ul><li>Achieve lower detection limits.</li><li>Improve recovery from challenging matrices such as palm stearates.</li></ul><h5><strong>Step 4: alu oxide clean-up</strong></h5><p>Adding an alumina oxide clean-up step can substantially improve MOSH quantification in the presence of n-alkanes. This step is matrix-dependent and should be avoided if n-alkanes are absent to prevent bias.</p><h5><strong>Step 5: fraction collection for advanced analysis</strong></h5><p>When further identification is required—such as distinguishing between mineral oil hydrocarbons and plasticizers (POSH)—fraction collection followed by <strong>GC×GC-MS</strong> analysis can provide a deeper chemical fingerprint.</p><h4><strong>Beyond “how much”: the role of GC×GC-MS</strong></h4><p>Conventional LC-GC-FID answers the fundamental question: <i>How much MOSH or MOAH is present in the sample?</i></p><p>But it cannot always explain the <strong>source</strong> or the <strong>chemical nature</strong> of the detected hydrocarbons.</p><p><strong>This is where GC×GC-MS adds value:</strong></p><ul><li><strong>Source tracing </strong>– Identifies whether contamination originates from packaging, processing equipment, or environmental exposure.</li><li><strong>Structural characterization</strong> – Distinguishes low-ring MOAH (less concerning) from high-ring MOAH (more concerning toxicologically).</li><li><strong>False positive elimination</strong> – Confirms the identity of suspect peaks, reducing the risk of misreporting.</li></ul><p>By combining <strong>FID for precise quantification</strong> with <strong>MS for molecular identification</strong>, GC×GC-MS enables both regulatory compliance and investigative insight.</p><h4><strong>The role of chromeleon software in MOSH/MOAH analysis</strong></h4><p>Modern analytical systems rely heavily on software to ensure speed, traceability, and accuracy. Chromeleon software offers:</p><ul><li><strong>Unified control</strong> of LC, GC, and sample preparation hardware from a single interface.</li><li><strong>Automated workflow setup</strong> – In just a few clicks, vial positions, injection types, and processing methods are assigned.</li><li><strong>Integrated quality checks</strong> – Internal standard verification and retention time monitoring are built-in.</li><li><strong>Customizable, regulatory-ready reports</strong> – Exportable in PDF, CSV, XML, and other formats without external spreadsheets.</li></ul><p>The result is streamlined operation, reduced analyst intervention, and consistent compliance with good laboratory practice (GLP) requirements.</p><h4><strong>Looking ahead</strong></h4><p>With upcoming EU regulations likely to set strict MOAH limits, and with continued scientific scrutiny of MOSH accumulation, the demand for high-quality testing will only increase.</p><p><strong>Key trends shaping the future of MOSH/MOAH analysis include:</strong></p><ul><li><strong>Wider adoption of GC×GC-MS</strong> for confirmation and source identification.</li><li><strong>Greater automation</strong> in sample preparation to increase throughput and reproducibility.</li><li><strong>Regulatory harmonization</strong>, which will help reduce discrepancies between international markets.</li><li><strong>Lower detection thresholds</strong>, requiring even more sensitive and selective methods.</li></ul><p>For laboratories, the challenge is twofold: staying ahead of compliance requirements while building capacity for high-volume, high-accuracy testing. Those that invest in <strong>robust, automated, and harmonized workflows</strong> now will be better positioned to meet both current and future demands.</p><blockquote><p><strong>Acknowledgement: </strong>Jorn Hofsteenge, SampleQ, Breda, The Netherlands</p></blockquote>

MOSH/MOAH Analysis: Technology, Regulation, and the Road Ahead

Article

Product

Events

Webinars

Application

Academy

Video

Poster

Scientists

Plastics

Environment

Food

Water

Health

Presentation

Scientific article

Interview

Toxicology

Popularization

Science and research

Software

Covid-19

Career

Laboratories

Various

Zaměření

Type of News

Focus

A unique company dedicated to serving science helping our customers drive productivity and accelerate results. Through our premier brands – Thermo Scientific, Applied Biosystems, Invitrogen, Fisher Scientific and Unity Lab Services.

Thermo Fisher Scientific

Everything from the world of analytical chemistry in one place. We connect people in solving their problems. At Labrulez you will find all the necessary information easily, quickly and clearly. Stop searching and start finding.

LabRulez

Bruker at ADLM 2026

Beyond ASMS — A Waters Innovation Road Show

Waters Corporation at ADLM 2026

PFAS & Our Planet: Textiles and Materials

Column Chemistry Compass: Navigating the Agilent HPLC and UHPLC Column Landscape

Empowering Omics Research Through Integrated Workflows and Strategic Collaboration