Lithium-ion batteries (LIBs) have transformed energy storage technology, driving innovations for products we use in everyday life such as smartphones and even electric vehicles. But what makes these batteries so efficient? A key component is the electrolyte solution, a complex mix that’s crucial for battery performance. GC-MS or gas chromatography-mass spectrometry is an essential tool in analyzing these electrolyte mixtures and the development of increased efficiency and longer-lasting batteries.<figure class="image"><img style="aspect-ratio:1024/551;" src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Electrifying_Insights_How_GC_MS_is_Powering_Lithium_Ion_Battery_Analysis_29d144ea28.jpg" alt="Thermo Fisher Scientific: Electrifying Insights: How GC-MS is Powering Lithium-Ion Battery Analysis." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Electrifying_Insights_How_GC_MS_is_Powering_Lithium_Ion_Battery_Analysis_29d144ea28.jpg 245w," sizes="100vw" width="1024" height="551"></figure><h4>Why Analyze Electrolytes?</h4>Electrolyte solutions are the essence of lithium-ion batteries, impacting:<ul><li>Performance: The right mix ensures faster charging and longer battery life.</li><li>Safety: Accurate composition prevents overheating and potential hazards.</li><li>Lifespan: Understanding degradation helps design components that last longer.</li></ul>Getting the electrolyte mix right is vital for efficient, safe, and durable batteries.However, analyzing electrolytes is complex and comes with a number of challenges:<ol><li>Complex Mixture: Electrolytes consist of various organic solvents, additives, and degradation products. This complexity requires sophisticated technology to separate and identify components.</li><li>Heat Sensitivity: Components like LiPF6 can degrade at high temperatures, creating new compounds that complicate analysis.</li><li>Trace Additives: Some additives are present in low concentrations but play a critical role in battery performance. Detecting these components demands highly sensitive methods.</li><li>Degradation Products: Battery cycling produces byproducts that can interfere with the main components. It’s like trying to find a book in a disorganized library.</li></ol>This is where GC-MS becomes an essential analytical tool. This powerful technique provides a detailed look into the composition of LIB electrolytes. The analysis follows a number of steps:<ul><li>Sample Prep: LIB electrolyte samples are diluted in dichloromethane and centrifuged to remove interfering salts.</li><li>GC Separation: Samples are run through a gas chromatograph which uses a programmed temperature ramp ensures all components are separated within a 23-minute window.</li><li>MS detection: After separation, the mass spectrometer operating in full scan and selected ion monitoring (SIM) provides detailed qualitative and quantitative data.</li></ul>Figure 1 shows the difference in selectivity between full scan and SIM mode. Vinylene carbonate is not detected in full scan at a 1 to 500 dilution due to the lack of selectivity and interference in full scan acquisition. However, by using SIM the ions of interest are isolated in the quadrupole increasing selectivity and allowing vinylene carbonate to be quantified at a low level.<figure class="image"><img style="aspect-ratio:881/694;" src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Electrifying_Insights_How_GC_MS_is_Powering_Lithium_Ion_Battery_Analysis_Figure_1_Full_scan_and_SIM_acquisition_of_vinylene_carbonate_in_cycled_LIB_electrolyte_at_1_500_dilution_6803793369.jpg" alt="Thermo Fisher Scientific: Figure 1. Full scan and SIM acquisition of vinylene carbonate in cycled LIB electrolyte at 1:500 dilution." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Electrifying_Insights_How_GC_MS_is_Powering_Lithium_Ion_Battery_Analysis_Figure_1_Full_scan_and_SIM_acquisition_of_vinylene_carbonate_in_cycled_LIB_electrolyte_at_1_500_dilution_6803793369.jpg 198w," sizes="100vw" width="881" height="694"></figure>GC-MS brings several advantages to electrolyte analysis:<ul><li>Precise Separation: Achieves excellent separation of multiple components, ensuring accurate readings without co-elution issues.</li><li>High Sensitivity: Detects even trace amounts of additives—down to 0.021 mg/L.</li><li>Broad Range: Handles a wide concentration range, analyzing both major and minor components in one go.</li><li>Degradation Insights: Reveals compositional shifts in cycled electrolytes, providing clues about the aging process of batteries.</li></ul><div><div><h4>Why this analysis is important?</h4>Understanding the detailed composition and changes in LIB electrolytes is crucial. It helps researchers and manufacturers fine-tune battery designs for enhanced performance, safety, and durability. While the analysis can be complex, the insights gained are invaluable.So next time you charge your device remember the sophisticated science behind that battery. Tools like GC-MS are enabling battery technological advances to be made, ensuring the future of battery technology.<blockquote>For full details on this analysis<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_001124_gc_ms_isq_7610_li_battery_electrolyte_an001124_na_en_4df8612386/an-001124-gc-ms-isq-7610-li-battery-electrolyte-an001124-na-en.pdf">&nbsp;</a><a target="_blank" rel="noreferrer noopener" aria-label="read the full application note. - open in a new tab" data-uw-rm-ext-link="" uw-rm-external-link-id="https://assets.thermofisher.com/tfs-assets/cmd/application-notes/an-001124-gc-ms-isq-7610-li-battery-electrolyte-an001124-na-en.pdf$readthefullapplicationnote."><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_001124_gc_ms_isq_7610_li_battery_electrolyte_an001124_na_en_4df8612386/an-001124-gc-ms-isq-7610-li-battery-electrolyte-an001124-na-en.pdf">read the full application note.</a></a> For further details on how GC-MS can power your analysis, <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/mass-spectrometry/gas-chromatography-mass-spectrometry-gc-ms/gc-ms-systems/single-quadrupole-gc-ms.html">visit our website.</a><h5>Visit us on <a target="_blank" rel="noreferrer noopener" aria-label="LinkedIn: - open in a new tab" data-uw-rm-ext-link="" uw-rm-external-link-id="https://www.linkedin.com/showcase/72003132/admin/dashboard/$linkedin:"><a target="_blank" rel="noopener noreferrer" href="https://www.linkedin.com/showcase/72003132/admin/dashboard/">LinkedIn:</a></a> #LithiumIonBatteries #GCMS #BatteryMaterialAnalysis</h5><section><h4 data-uw-rm-heading="level" role="heading" aria-level="2">Adam Ladak</h4><div itemprop="description">Adam Ladak is the global product marketing manager for GC quadrupole mass spectrometry at Thermo Fisher, based in the UK. He started his career working in a contracting testing lab analyzing sports supplements and horse feed for prohibited substances. He has over 20 years of experience in the analytical testing industry and has worked for leading instrument manufacturers in various roles from an application specialist to a global marketing role focused on food and environmental testing. Adam is passionate about utilizing our GCMS instrumentation to meet the customer needs and solve real world problems.</div></section></blockquote></div></div>

Electrifying Insights: How GC-MS is Powering Lithium-Ion Battery Analysis

During the manufacture of pharmaceuticals, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=45&amp;search=1%2C+4-Dioxane">1, 4-Dioxane</a> is used as a cleansing agent. It is also a byproduct of plastic manufacturing. The most likely exposure to 1, 4-Dioxane is at an industrial site. However, if any 1, 4-Dioxane is released into the environment during manufacturing there is a potential for it to migrate into ground water. The fact that 1, 4-Dioxane is so miscible in water makes degradation of the chemical challenging. Ethanol, on the other hand, has been a popular gasoline additive. Since it burns more quickly and completely than gasoline, emissions from car exhaust are decreased. The downside of this is underground storage tank leakage and fuel spills cause ground water and drinking water to be contaminated with both the fuel and the ethanol additive. Since ethanol is also very miscible in water, the detection of ethanol contamination in water can be difficult.&nbsp;There have been several innovations that help overcome the obstacles of detecting 1, 4-Dioxane and Ethanol. The first one is the SIM mode of the mass spectrometer. This mode allows better detection of hard to extract compounds. Furthermore, mass spectrometers are now equipped to run SIM/Scan, this not only helps detect more difficult compounds, but also enables the detection of an extensive list of <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=45&amp;search=USEPA+Method+8260">USEPA Method 8260</a> compounds without having to run the samples twice. Advancements in purge and trap sampling have also facilitated better detection of these compounds. Most effective in this has been the ability to heat the samples. However, there are drawbacks to better detection. The most problematic of these is the tendency of 1, 4-Dioxane and Ethanol to “stick” to the glass ware. This susceptibility has caused many headaches in environmental labs.&nbsp;This application note will investigate seven variations of <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=45&amp;search=purge+and+trap">purge and trap</a> sampling. The data will then be evaluated in order to recommend the optimum purge and trap sampling parameters for your lab.<h4>Experimental:&nbsp;</h4>The sampling system used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Evolution concentrator</a> affixed with a Vocarb 3000 trap. The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler</a> equipped with the syringe option was employed as the autosampler. The separation and analysis were performed by an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890A+Gas+Chromatograph">Agilent 7890A Gas Chromatograph (GC)</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975C+Mass+Spectrometer">5975C inert XL Mass Spectrometer (MS).</a> The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=7&amp;search=Rxi-624+Sil+MS">Restek Rxi-624 Sil MS</a> 30m x 0.25mm x 1.4µm column. The purge and trap and GC/MS parameters used for this study are listed below.<h5>Purge and Trap Parameters</h5><ul><li>Concentrator: EST Encon Evolution</li><li>Trap type: Vocarb 3000</li><li>Valve oven temperature: 150 °C</li><li>Transfer line temperature: 150 °C</li><li>Trap temperature: 35 °C</li><li>Moisture Reduction Trap (MoRT) temperature: 39 °C</li><li>Purge time: 11 min</li><li>Purge flow: 40 mL/min</li><li>Dry purge: Ambient temperature, 40 mL/min, 1.0 min</li><li>Desorb pressure: 5 psi (with control ON)</li><li>Desorb time: 0.5 min</li><li>Desorb preheat delay: 10 sec</li><li>Desorb temperature: 250 °C</li><li>MoRT bake temperature: 210 °C</li><li>Bake temperature: 260 °C</li><li>Sparge vessel bake temperature: 40 °C for 3 min, ramp to 100–110 °C, hold</li><li>Bake time: 6 min</li><li>Bake flow: 85 mL/min</li></ul><h5>Auto-Sampler (EST Centurion WS):</h5><ul><li>Sample type: Water</li><li>Sample volume: 5 or 10 mL</li><li>Internal standard volume: 5 µL</li></ul><h5>GC/MS Parameters</h5><ul><li>System: Agilent 7890A GC / 5975C inert XL MS</li><li>Inlet: Split mode, 220 °C, 40:1 split ratio, 12.153 psi head pressure</li><li>Column: Restek Rxi-624Sil MS, 30 m × 0.25 mm × 1.4 µm</li><li>Oven program: 45 °C (1 min) → ramp 15 °C/min → 220 °C, hold 1.33 min (total run ~14 min)</li><li>Column flow rate: 1 mL/min helium</li><li>Total flow: 44 mL/min</li><li>Source temperature: 230 °C</li><li>Quadrupole temperature: 150 °C</li><li>Transfer line temperature: 180 °C</li><li>Scan range: m/z 35–300, 5.2 scans/sec</li><li>SIM ions:<ul><li>45, 46 (0.7–3.49 min)</li><li>58, 88 (3.5–14 min)</li></ul></li><li>Solvent delay: 0.7 min</li></ul>For each parameter iteration, see the text below, a calibration curve was established with a linear range of 0.5 to 200ppb using standards from Restek. After each of the prescribed curves was determined; Method Detection Limits (MDLs), precision and accuracy and carryover studies were performed. A series of seven low level standards were run in order to establish MDLs per 40CFR Part 136, Appendix B. Next, seven replicate samples of the 50ppb standard were run in order to establish the precision and the accuracy of the experimental parameters. Finally, a series of four 50ppb standards were run with each standard followed by three blanks. The amount of carryover was then analyzed in the first blank. The data from each parameter variation was compiled and compared in order to determine the optimum conditions for this analysis. An average of the results for each analysis condition is listed in Table 1.<h5>Purge and Trap Sampling Test Parameters</h5><ul><li>Baseline: 5 mL traditional sparger, room temp purge, 110 °C sparge bake</li><li>Iteration A: 5 mL traditional sparger, 40 °C purge, 110 °C sparge bake</li><li>Iteration B: 5 mL traditional sparger, 60 °C purge, 110 °C sparge bake</li><li>Iteration C: 5 mL traditional sparger, 40 °C purge, no sparge bake</li><li>Iteration D: 40 mL vial, 10 mL purge volume, 40 °C purge, no sparge bake</li><li>Iteration E: 5 mL fritless bulbless sparger, 40 °C purge, 110 °C sparge bake</li><li>Iteration F: 5 mL fritless bulbless sparger, 40 °C purge, no sparge bake (Iteration E used the patented Water/Soil prep mode)</li></ul><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_4_Averaged_Results_Summary_306dcbfde6.jpg" alt="EST Analytical: Table 1 Averaged Results Summary" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_4_Averaged_Results_Summary_306dcbfde6.jpg 245w," sizes="100vw" width="1493" height="351">The primary compounds of interest for the study were Ethanol and 1, 4-Dioxane. For this reason, the data for these compounds was compiled separately in order to better distinguish the benefits or detriment of each purge and trap parameter set. The experimental results of the precision and percent recovery studies are displayed in Tables 2 and 3.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_5_Ethanol_and_1_4_Dioxane_Precision_at_50ppb_3a195e1acb.jpg" alt="EST Analytical: Table 2 Ethanol and 1, 4-Dioxane Precision at 50ppb" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_5_Ethanol_and_1_4_Dioxane_Precision_at_50ppb_3a195e1acb.jpg 245w," sizes="100vw" width="1316" height="236"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_6_Ethanol_and_1_4_Dioxane_Percent_Recovery_at_50ppb_cb12616f47.jpg" alt="EST Analytical: Table 3 Ethanol and 1, 4-Dioxane Percent Recovery at 50ppb" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_6_Ethanol_and_1_4_Dioxane_Percent_Recovery_at_50ppb_cb12616f47.jpg 245w," sizes="100vw" width="1318" height="234">For the carryover studies, Ethanol and 1, 4-Dioxane were examined along with the carryover of 1, 2, 4- Trichlorobenzene, Naphthalene and 1, 2, 3-Trichlorobenzene. The reason the heavier compounds were included in this study was a concern that changing the sampling parameters may help the Ethanol and 1, 4-Dioxane carryover, but harm the carryover of the heavier compounds of interest. Table 4 shows a listing of the carryover results, in parts per billion, while Figure 1 displays the percent carryover of the different purge and trap experimental parameters for just the Ethanol and 1, 4-Dioxane.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_7_Carryover_in_First_Blank_after_a_50ppb_Standard_7d2bc81626.jpg" alt="EST Analytical: Table 4 Carryover in First Blank after a 50ppb Standard" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_7_Carryover_in_First_Blank_after_a_50ppb_Standard_7d2bc81626.jpg 245w," sizes="100vw" width="1332" height="426"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_1_Ethanol_and_1_4_Dioxane_Percent_Carryover_after_a_50ppb_Standard_Graphic_f57c981913.jpg" alt="EST Analytical: Figure 1 Ethanol and 1, 4-Dioxane Percent Carryover after a 50ppb Standard Graphic" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_1_Ethanol_and_1_4_Dioxane_Percent_Carryover_after_a_50ppb_Standard_Graphic_f57c981913.jpg 245w," sizes="100vw" width="1358" height="787">After all the studies were completed, two purge and trap parameter variations showed the best precision, percent recovery, and carryover while meeting the USEPA Method 8260 linearity and response factor requirements. An abbreviated listing of the results for these two iterations are shown in Table 5.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_8_Results_of_the_Water_Extraction_and_the_Fritless_Bulbless_Sparge_Vessel_With_Sparge_Bake_Studies_9b71ec4951.jpg" alt="EST Analytical: Table 5 Results of the Water Extraction and the Fritless - Bulbless Sparge Vessel With Sparge Bake Studies" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_8_Results_of_the_Water_Extraction_and_the_Fritless_Bulbless_Sparge_Vessel_With_Sparge_Bake_Studies_9b71ec4951.jpg 161w," sizes="100vw" width="1256" height="1221"><h4>Conclusions:&nbsp;</h4>All seven purge and trap parameter iterations passed the USEPA Method 8260 requirements for linearity and method detection limits. The problem with some of the experimental parameters was found in the carryover and precision and accuracy studies. The carryover using the traditional sparge vessel showed a large amount of carryover for the Ethanol and 1, 4-Dioxane. Since the carryover was so high, the precision and accuracy data suffered. The Fritless/Bulbless sparge vessel, on the other hand, displayed much lower carryover for the Ethanol and 1, 4-Dioxane especially when the patented sparge bake was not used. However, the 1, 2, 4-Trichlorobenzene, Naphthalene and 1, 2, 3-Trichlorobenzene carryover after the 50ppb standard was above the lower limit of the curve.&nbsp;Thus, the sparge bake would be recommended in order to limit the carryover of the heavier compounds. The optimum purge and trap parameters proved to be the patented water extraction technique. This technique provided linearity and method detection limits that met the USEPA Method 8260 requirements, while providing excellent precision and accuracy data. During water extraction, the sample is transferred to an empty 40ml vial and then purged in the soil station of the Centurion. The “fresh” vial provides a clean sparge vessel for every sample thus limiting carryover for both the Ethanol and 1, 4-Dioxane and for the heavy compounds. This lack of carryover aided in providing optimum precision and accuracy and carryover results and would be the recommended method for examining these troublesome compounds.

Optimization of 1,4-Dioxane and Ethanol Detection Using USEPA Method 8260

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.<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"><article><div><h3>Screening and confirmation: A rigorous two-step approach</h3>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. 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 (1). 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">Thermo Scientific TSQ 9610 Triple Quadrupole GC-MS/MS system</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. “The TSQ 9610 mass spectrometer has helped us to improve our workflow in the lab,” says Dr. Ericsson. “We started using it in 2023 and today we have analyzed more than 40,000 samples… with great success.” Implementation of <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/77">Thermo Scientific TraceFinder software</a> has also enabled seamless software continuity with LADF’s existing LC-MS and GC-MS platforms—minimizing training needs and ensuring consistent operations.<h3>Unlocking historical insights with retrospective analysis</h3>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">Thermo Scientific Orbitrap Exploris 120 mass spectrometer</a> to re-mine stored HRAM data and search for newly -banned substances. 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). “Working with high-resolution mass spectrometry, we have the possibility to go back and search in previously analyzed data,” Dr. Ericsson explains. Retrospective analysis is becoming increasingly vital as WADA continues to expand its list of monitored substances.<h3>Speeding up turnaround times without sacrificing accuracy</h3>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">Thermo Scientific Vanquish Duo UHPLC</a> paired with the Orbitrap Exploris 120 mass spectrometer, enabling parallel workflows and multiplexed analyses in 96-well formats. “We are able to save maybe a couple of hours of time. And this is a huge benefit for us,” notes Dr. Ericsson. 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 (1).<h3>Building toward a one-stop shop</h3>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. “It’s nice to have a one-stop shop… which means that you work mostly with one major provider,” says Dr. Ericsson. 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. 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.<h3>Looking ahead: The future of anti-doping analysis</h3>As doping methods evolve, so must detection technologies. LADF continues to invest in instruments that deliver robustness, low maintenance, and ultra-sensitivity. “It’s the sensitivity and the selectivity… and the possibility to increase the selectivity by doing, for instance, different MS/MS experiments,” says Dr. Ericsson. 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 (1). 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 (1). 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><h3>Additional resources</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>Visit us on&nbsp;<a target="_blank" rel="noopener noreferrer" href="https://www.linkedin.com/showcase/72003132/admin/dashboard/">LinkedIn:</a>&nbsp;#Antidoping, #LADF, #WADA, #SportsIntegrity</blockquote></div></article><section><blockquote><h4>Ema Ruzic</h4>Vertical Marketing Manager, Chromatography and Mass Spectrometry Division (CMD)</blockquote></section>

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

<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=45&amp;search=USEPA+Method+524.2">USEPA Method 524.2</a> calls for purge and trap sampling coupled with a Gas Chromatograph (GC) and Mass Spectrometer (MS) for separation and analysis. It has an extensive list of compounds and requires lower detection limits due to its use in drinking water testing. A 20% relative standard deviation for compound response factors is required across the calibration curve while the calibration check standard analytes have to be within 30% of the expected concentration. Currently, this method calls for a 5mL or 25mL purge volume and a four minute desorb time. These method requirements can pose a challenge for the analyst due to the amount of moisture that is created.&nbsp;The negative effects of the increased water vapor include instability of the chromatography, band eluting and poor peak shape to name a few. A side effect of this instability is sample re-runs and lost laboratory productivity. In addition, a common practice for mitigating moisture is increasing the GC inlet split rate. This poses yet another difficulty as the increased split rate can result in reduced sensitivity. EST Analytical’s eight port valve in the Evolution purge and trap concentrator aids in limiting the water exposure because the water management of the system is not part of the desorb pathway. This feature also enables laboratories to use a smaller split ratio at the GC inlet thus increasing sensitivity.<h4>Experimental:&nbsp;</h4>The sampling system used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Evolution purge and trap concentrator</a> and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler</a>. The concentrator was affixed with a Vocarb 3000 trap and connected to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890A">Agilent 7890A GC</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975C">5975C inert XL MS</a>. The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=7&amp;search=Restek+Rxi-624+Sil+MS">Restek Rxi-624 Sil MS</a> 30m x 0.25mm x 1.4µm column. The purge and trap and GC/MS parameters used for this study are listed below.<h5>Purge and Trap Parameters</h5><ul><li>Concentrator: EST Evolution</li><li>Trap type: Vocarb 3000</li><li>Valve oven temperature: 130 °C</li><li>Transfer line temperature: 130 °C</li><li>Trap temperature: 35 °C</li><li>Moisture Reduction Trap (MoRT) temperature: 39 °C</li><li>Purge time: 11 min</li><li>Purge flow: 40 mL/min</li><li>Dry purge Temp.: Ambient</li><li>Dry Purge Flow: 40mL/min</li><li>Dry Purge Time: 1.0 min &nbsp;</li><li>Desorb pressure Control: ON</li><li>Desorb Pressure: 5psi</li><li>Desorb time: 4 min</li><li>Desorb preheat delay: 15 sec</li><li>Desorb temperature: 250 °C</li><li>MoRT bake temperature: 210 °C</li><li>Bake temperature: 260 °C</li><li>Sparge vessel bake temperature: 110 °C</li><li>Bake time: 6 min</li><li>Bake flow: 70 mL/min</li></ul><h5>Auto-Sampler (EST Centurion WS):</h5><ul><li>Sample type: Water</li><li>Water volume: 25 mL</li><li>Internal standard volume: 5 µL</li></ul><h5>GC/MS Parameters</h5><ul><li>System: Agilent 7890A GC / 5975C inert XL MS</li><li>Inlet: Split mode, 220 °C, 40:1 split ratio, 12.153 psi head pressure</li><li>Column: Restek Rxi-624Sil MS, 30 m × 0.25 mm × 1.4 µm</li><li>Oven program: 45 °C (1 min) → ramp 15 °C/min → 220 °C, hold 1.33 min (total run ~14 min)</li><li>Column flow rate: 1 mL/min helium</li><li>Total flow: 44 mL/min</li><li>Source temperature: 230 °C</li><li>Quadrupole temperature: 150 °C</li><li>Transfer line temperature: 180 °C</li><li>Scan range: m/z 35–300, 5.2 scans/sec</li><li>Solvent delay: 0.7 min</li></ul>A calibration curve was established with a linear range of 0.25 to 40µg/L using the USEPA Method 524.2 standards from Restek. After the curve was determined, method detection limits were ascertained by running a series of seven replicate 0.25 µg/L standards and calculated using the procedure outlined in 40 CFR Part 136 Appendix B. Finally, seven 20 µg/L standards were examined in order to verify the precision and accuracy of the analysis. The results of this study are displayed in Tables 1 and 2 while Figure 1 presents a 20 µg/L standard GC/MS chromatogram.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_3_Compound_Linearity_and_Response_Factor_Table_f63b77844f.jpg" alt="EST Analytical: Table 1 - Compound Linearity and Response Factor Table" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_3_Compound_Linearity_and_Response_Factor_Table_f63b77844f.jpg 153w," sizes="100vw" width="1104" height="1126"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_4_MDL_and_Precision_and_Percent_Recovery_Table_27572600f0.jpg" alt="EST Analytical: Table 2 - MDL and Precision and Percent Recovery Table" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_4_MDL_and_Precision_and_Percent_Recovery_Table_27572600f0.jpg 186w," sizes="100vw" width="1358" height="1143"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_1_20mg_L_Standard_Chromatogram_7ff795984b.jpg" alt="EST Analytical: Figure 1 - 20 µg/L Standard Chromatogram" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_1_20mg_L_Standard_Chromatogram_7ff795984b.jpg 245w," sizes="100vw" width="1431" height="789"><h4>Conclusions:&nbsp;</h4>This study demonstrated the effectiveness of the Evolution/Centurion purge and trap sampling system. The results passed all of the USEPA Method 524.2 criteria for both linearity and detection limits. Since the Evolution bypasses the water management trap during the four minute desorb process, the amount of water effecting the experiments was limited. Furthermore, the forty to one split ratio at the GC inlet provided excellent detection limits as the system was more sensitive to the low level standard requirements of the method. The lower split rate has an added benefit of reducing laboratory helium consumption when setting it against other system’s higher split ratios. Finally, the precision and percent recovery results showed the reliability of the system in producing accurate experimental findings.

USEPA 524.2 Method Validation Using the Evolution Purge and Trap Concentrator and the Centurion WS Autosampler

Analysis of field samples in environmental laboratories can sometimes be complicated by how contaminated or “hot” the sample is. Many times “hot” samples have to be diluted in order to verify the level of contamination in the sample. The process of diluting samples is a time consuming process that can sometimes lead to human error when calculations are incorrect. A further problem is the loss of volatile organic compounds as the sample vial needs to be opened in order to perform the dilution.&nbsp;This poster will examine the benefits of automated dilutions. Since the syringe option of this system has the unique ability to dilute samples from two times to 400 times the original concentration, this study will examine the precision and accuracy for an array of dilutions in this comprehensive range. The dilution data will be compared to a manually prepared 50ppb calibration standard in order to determine the accuracy of the results. The precision will be established by examining four sequential dilutions and the percent relative standard deviation of the compounds’ respective area counts. Furthermore, in order to demonstrate the linearity of the dilutions, a calibration curve will be presented using the automated dilution option to prepare 200ppb standards for a calibration range of 0.5ppb (400x) to 200ppb (1x).<h4>Discussion&nbsp;</h4>Environmental laboratories often have to dilute field samples due to the analytes of interest having concentrations over the highest calibration level of the curve. In order to dilute these samples, the vial has to be opened and a portion of the sample has to be diluted manually and re-analyzed. Opening the vial can compromise the integrity of the sample as volatiles are lost when the seal of the vial is broken.&nbsp;EST Analytical has developed a syringe feature for the Centurion Autosampler that can dilute samples up to 400 times the original concentration. This feature is fully programmable and the sample vial does not have to be compromised in order to dilute the sample because the dilution process is automated. The sealed vial can be placed in the sample tray while the Centurion does all of the work.&nbsp;<h4>Experimental&nbsp;</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler</a> was configured with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">Encon Evolution concentrator</a>. A Vocarb 3000 (K) trap was installed in the Evolution. Finally, the sampling system was connected to a GC/MS for sample analysis. The GC column employed for this study was an Rxi-624Sil MS 30m x 0.25mm x 1.4µm. Dilution Factors, Purge and Trap, and GC/MS parameters are listed below.<h5>Standard Concentration &amp; Dilution Factors</h5><ul><li>100ppb: 2x</li><li>250ppb: 5x</li><li>500ppb: 10x</li><li>2.5ppm: 50x</li><li>5ppm: 100x</li><li>10ppm: 200x</li><li>20ppm: 400x</li></ul><h5>Purge and Trap Parameters</h5><ul><li>Concentrator: EST Encon Evolution</li><li>Trap type: Vocarb 3000</li><li>Valve oven temperature: 150 °C</li><li>Transfer line temperature: 150 °C</li><li>Trap temperature: 35 °C</li><li>Moisture Reduction Trap (MoRT) temperature: 39 °C</li><li>Purge time: 11 min</li><li>Purge flow: 40 mL/min</li><li>Dry purge Temp.: Ambient</li><li>Dry Purge Flow: 40mL/min</li><li>Dry Purge Time: 1.0 min &nbsp;</li><li>Desorb pressure Control: ON</li><li>Desorb Pressure: 5psi</li><li>Desorb time: 0.5 min</li><li>Desorb preheat delay: 5 sec</li><li>Desorb temperature: 260 °C</li><li>MoRT bake temperature: 230 °C</li><li>Bake temperature: 265 °C</li><li>Sparge vessel bake temperature: 120 °C</li><li>Bake time: 8 min</li><li>Bake flow: 40 mL/min</li></ul><h5>GC/MS Parameters</h5><ul><li>System: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890%2F5975">Agilent 7890/5975</a></li><li>Inlet: Split mode, 200 °C, 40:1 split ratio, 12.153 psi head pressure</li><li>Column: Rxi-624Sil MS 30m x 0.25mm I.D. 1.4µm film thickness</li><li>Oven program: 45 °C (1 min) → ramp 18 °C/min → 220 °C, hold for 0.3 min</li><li>Column flow rate: 1 mL/min helium</li><li>Total flow: 44.0 mL/min</li><li>Source temperature: 230 °C</li><li>Quadrupole temperature: 150 °C</li><li>Transfer line temperature: 180 °C</li><li>Scan range: m/z 35–265, 3.12 scans/sec</li><li>Solvent delay: 0.7 min</li></ul>A 9 point calibration curve was manually prepared and run from 0.5 to 200ppb with standards ordered from Restek. After a linear calibration curve was established, a 50ppb calibration standard was run to establish instrument response for the compounds being analyzed. Next, a series of dilutions were run and compared with the initial 50ppb calibration standard. Each dilution factor was run four times with blanks in between. The final concentration of each dilution was 50ppb. The precision and accuracy of the dilutions are listed in Tables 4 and 5 and Figures 1 and 2 display the chromatograms of two of the dilutions.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_1_Overlay_of_50ppb_1_X_and_2500ppb_50x_Standards_29d90b4107.jpg" alt="EST Analytical: Figure 1 - Overlay of 50ppb (1X) and 2500ppb (50x) Standards" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_1_Overlay_of_50ppb_1_X_and_2500ppb_50x_Standards_29d90b4107.jpg 245w," sizes="100vw" width="1023" height="383"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_2_Overlay_of_50ppb_1_X_and_10000ppb_200x_Standards_7f939589b9.jpg" alt="EST Analytical: Figure 2 - Overlay of 50ppb (1X) and 10000ppb (200x) Standards" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_2_Overlay_of_50ppb_1_X_and_10000ppb_200x_Standards_7f939589b9.jpg 245w," sizes="100vw" width="1073" height="383"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_4_Experimental_Results_2x_5x_10x_and_50x_dilutions_d81be1942f.jpg" alt="EST Analytical: Table 4 - Experimental Results (2x, 5x, 10x, and 50x dilutions)" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_4_Experimental_Results_2x_5x_10x_and_50x_dilutions_d81be1942f.jpg 150w," sizes="100vw" width="1173" height="1220"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_5_Experimental_Results_100x_200x_and_400x_dilutions_f29762c72e.jpg" alt="EST Analytical: Table 5 - Experimental Results (100x, 200x and 400x dilutions)" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_5_Experimental_Results_100x_200x_and_400x_dilutions_f29762c72e.jpg 124w," sizes="100vw" width="972" height="1226">Finally, a nine point calibration curve was run by setting up the system to do the dilutions. The curve was run using nine 40ml vials filled to volume with a 200ppb calibration standard and doing serial dilutions on the standards. For example, the 200ppb was diluted 400x for the 0.5ppb standard, 200x for the 1.0ppb standard, etc. See Table 6 for the curve dilutions and Table 7 for the curve linearity and compound responses.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_6_Syringe_Curve_Dilutions_4237e1d568.jpg" alt="EST Analytical: Table 6 Syringe Curve Dilutions" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_6_Syringe_Curve_Dilutions_4237e1d568.jpg 245w," sizes="100vw" width="785" height="381"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_7_Automated_Dilution_Curve_Results_356126f34f.jpg" alt="EST Analytical: Table 7 Automated Dilution Curve Results" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_7_Automated_Dilution_Curve_Results_356126f34f.jpg 138w," sizes="100vw" width="927" height="1050"><h4>Conclusions&nbsp;</h4>The Centurion WS with the syringe option displayed remarkable precision and accuracy from as low as the 2x dilution to as high as 400x dilution. On the whole, the average precision of the instrument was less than 5%RSD while the overall accuracy was 90% to 110%. The system also is capable of curve automation with the average %RSD of below 10% for a 9 point curve from 0.5ppb to 200ppb. The automated dilution feature of the Centurion WS with the syringe option would enable laboratories to run samples more efficiently and the since the samples would not need to be compromised in order to perform dilutions, the accuracy of the experimental results would improve.

Automated Dilutions Using the Centurion Autosampler

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Automated Dilutions Using the Centurion Autosampler

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