<p><strong>In the week of July 7, the following webinars await you in the field of liquid phase and especially HPLC and LC/MS.</strong></p><blockquote><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></p><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>4 500 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. SCIEX: SCIEX OS software transforms your workflows</strong></h5><ul><li>Tuesday, July 8, 2025, 19:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5268">Registration</a></li></ul><p>In this webinar, we will dive deeper into the advanced features of SCIEX OS software, including automated compound optimization, method editors, and more.</p><h5><strong>2. Agilent Technologies: Cutting through pesticide residues and heavy metals</strong></h5><ul><li>Wednesday, July 9, 2025, 06:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/4868">Registration</a></li></ul><p>This webinar focuses on pesticides and heavy metals detection, along with performing elemental speciation in dairy products by LC/MS/MS, GC/MS/MS, and ICP-MS techniques.</p><h5><strong>3. Phenomenex: HPLC Mysteries Unveiled: Solving Retention Time and Resolution Challenges</strong></h5><ul><li>Wednesday, July 9, 2025, 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5224">Registration</a></li></ul><p>Facing issues with HPLC retention or resolution? Join this session to explore retention principles, void time, and strategies to optimize or troubleshoot your LC methods.</p><h5><strong>4. Agilent Technologies: Peptide Analysis and Purification: From Fundamentals to Advanced Techniques</strong></h5><ul><li>Wednesday, July 9, 2025, 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5296">Registration</a></li></ul><p>Join the live webinar for a comprehensive overview of peptide analysis, designed for both emerging scientists and seasoned professionals.</p><h5><strong>5. SCIEX: SCIEX OS software: custom calculations for confident data analysis</strong></h5><ul><li>Wednesday, July 9, 2025, 11:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5297">Registration</a></li></ul><p>Explore calculated columns in SCIEX OS software—create custom fields, apply tailored formulas, and validate results for flexible, accurate, and confident data analysis in the lab.</p><h5><strong>6. Thermo Fisher Scientific: Data to Discovery: Orbitrap Astral for Small Molecules</strong></h5><ul><li>Wednesday, July 9, 2025, 15:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5234">Registration</a></li></ul><p>Join us for an expert-led panel discussion showcasing the power of the Orbitrap Astral mass spectrometer in small molecule research.</p><h5><strong>7. Waters Corporation: Fundamentals and Applications of Dynamic Light Scattering (DLS) for Biotherapeutic Development</strong></h5><ul><li>Wednesday, July 9, 2025, 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5111">Registration</a></li></ul><p>This webinar will introduce the fundamentals of DLS and explore its practical applications in biopharmaceutical workflows.</p><h5><strong>8. Thermo Fisher Scientific: Ion Chromatography: Practical Tips and Techniques for Every User</strong></h5><ul><li>Wednesday, July 9, 2025, 17:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5279">Registration</a></li></ul><p>Join us for an informative webinar focused on optimizing the operation of your ion chromatography (IC) system.</p><h5><strong>9. Metrohm: Amplifying the Invisible: Advanced Spectroelectrochemistry with EC-SERS</strong></h5><ul><li>Wednesday, July 9, 2025, 19:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5285">Registration</a></li></ul><p>Learn how Raman spectroelectrochemistry empowers time-resolved redox analysis by combining spectroscopy with electrochemistry—featuring SERS and real-world research applications.</p><h5><strong>10. Thermo Fisher Scientific: MOSH MOAH Analysis Made Clear: Strategies for Diverse Matrices</strong></h5><ul><li>Thursday, July 10, 2025, 08:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5305">Registration</a></li></ul><p>Join our upcoming webinar to learn from our experts about advanced MOSH/MOAH analysis techniques designed to tackle diverse matrices with exceptional efficiency and precision.</p><h5><strong>11. Phenomenex: Enhancing Productivity Using Flash Chromatography: Strategies and Techniques</strong></h5><ul><li>Thursday, July 10, 2025, 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5287">Registration</a></li></ul><p>Explore flash chromatography basics, TLC method development, HILIC for polar analytes, and how to transfer HPLC methods for efficient preparative purification workflows.</p>

Webinars LabRulezLCMS Week 28/2025

<p><strong>In the week of July 7, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.</strong></p><blockquote><p><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></p><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>4 500 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. Wasson-ECE Instrumentation: Introduction to the Micro GC, Use of Autosamplers with the uGC</strong></h5><ul><li>Tuesday, July 8, 2025, 21:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5304">Registration</a></li></ul><p>Do you know about Wasson-ECE’s MicroGCs? Join us for an introduction to Micro-GCs and their use with autosamplers.</p><h5><strong>2. Agilent Technologies: Cutting through pesticide residues and heavy metals</strong></h5><ul><li>Wednesday, July 9, 2025, 06:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4868">Registration</a></li></ul><p>This webinar focuses on pesticides and heavy metals detection, along with performing elemental speciation in dairy products by LC/MS/MS, GC/MS/MS, and ICP-MS techniques.</p><h5><strong>3. Separation Science: From Peaks to Insights: Navigating Environmental Analysis with Weck Laboratories using GC/MS/MS Instrumentation</strong></h5><ul><li>Wednesday, July 9, 2025, 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5259">Registration</a></li></ul><p>Discover the benefits of using triple quadrupole GC/MS in high-throughput environmental testing workflows.</p><h5><strong>4. Metrohm: Amplifying the Invisible: Advanced Spectroelectrochemistry with EC-SERS</strong></h5><ul><li>Wednesday, July 9, 2025, 19:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5285">Registration</a></li></ul><p>Learn how Raman spectroelectrochemistry empowers time-resolved redox analysis by combining spectroscopy with electrochemistry—featuring SERS and real-world research applications.</p><h5><strong>5. Thermo Fisher Scientific: MOSH MOAH Analysis Made Clear: Strategies for Diverse Matrices</strong></h5><ul><li>Thursday, July 10, 2025, 08:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5305">Registration</a></li></ul><p>Join our upcoming webinar to learn from our experts about advanced MOSH/MOAH analysis techniques designed to tackle diverse matrices with exceptional efficiency and precision.</p><h5><strong>6. Agilent Technologies: Surface Measurement and Beyond – Nondestructive Testing with Handheld FTIR and SORS Raman Spectroscopy</strong></h5><ul><li>Thursday, July 10, 2025, 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5298">Registration</a></li></ul><p>Join us for an engaging webinar! Agilent portable SORS Raman and FTIR systems are simplifying in situ chemical analysis.</p>

Webinars LabRulezGCMS Week 28/2025

<p><strong>In the week from July 7, the following webinars await you in the field of atomic and molecular spectroscopy and spectrometry</strong></p><blockquote><p><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></p><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>4 500 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. Milestone: How to Enhance Ash Content Determination with Microwave Ashing</strong></h5><ul><li>Tuesday, July 8, 2025, 16:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5283">Registration</a></li></ul><p>Join us for a live webinar dedicated to the challenges of traditional ash content determination and the advantages of adopting microwave ashing.</p><h5><strong>2. Bruker: Spatiotemporal Imaging with Light-Sheet Microscopy: Having Your Cake and Eating It Too</strong></h5><ul><li>Tuesday, July 8, 2025, 18:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5274">Registration</a></li></ul><p>Discover how FCS can be used in light-sheet microscopes—without customization—to analyze molecular behavior in biofilms, drosophila, and zebrafish at high speed and sensitivity.</p><h5><strong>3. Agilent Technologies: Cutting through pesticide residues and heavy metals</strong></h5><ul><li>Wednesday, July 9, 2025, 06:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/4868">Registration</a></li></ul><p>This webinar focuses on pesticides and heavy metals detection, along with performing elemental speciation in dairy products by LC/MS/MS, GC/MS/MS, and ICP-MS techniques.</p><h5><strong>4. Metrohm: Amplifying the Invisible: Advanced Spectroelectrochemistry with EC-SERS</strong></h5><ul><li>Wednesday, July 9, 2025, 19:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5285">Registration</a></li></ul><p>Learn how Raman spectroelectrochemistry empowers time-resolved redox analysis by combining spectroscopy with electrochemistry—featuring SERS and real-world research applications.</p><h5><strong>5. Agilent Technologies: Surface Measurement and Beyond – Nondestructive Testing with Handheld FTIR and SORS Raman Spectroscopy</strong></h5><ul><li>Thursday, July 10, 2025, 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5298">Registration</a></li></ul><p>Join us for an engaging webinar! Agilent portable SORS Raman and FTIR systems are simplifying in situ chemical analysis.</p><h5><strong>6. Agilent Technologies: Tips and Tricks Workshop on ICP-OES: Smarter Method Development</strong></h5><ul><li>Thursday, July 10, 2025, 20:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/3160">Registration</a></li></ul><p>Techniques on how to achieve the best sensitivity and detection limits through tuning techniques and strategies.</p>

Webinars LabRulezICPMS Week 28/2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 7th July 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you posters by <strong>Agilent Technologies / ASMS, Shimadzu / ASMS, </strong>presentation by<strong> Liège University / MDCW </strong>and technical note by<strong> Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Analysis of Allergens in Fragrance Samples Using a Comprehensive GCxGC in Combination with a High-Resolution Mass Spectrometry&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_gc_gc_7250_allergens_asms_2025_mp_353_en_agilent_3459141f12.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Fragrances are highly complex mixtures that combine natural and synthetic components. Analytical separation of these samples on a single GC column results in coelution of isomers and structurally similar compounds which produce similar spectral fragmentation patterns. This significantly complicates identification and quantitative analysis of individual components of the fragrances. Here we demonstrate a power of a comprehensive GCxGC approach combined with high resolution MS for identification and quantitative analysis of 64 allergens in fragrances. With added confidence in compound identification provided by accurate mass, this approach also streamlines a non-targeted analysis of the fragrances to determine their composition.</p><h4><strong>Experimental</strong></h4><p>The samples were separated on an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC"><strong>8890 GC</strong></a> using a comprehensive GCxGC configuration with a reverse flow modulator (RFM). The non-polar/mid-polar column set was used and comprised of a 20m x 0.1mm x 0.1um DB-1ms column (100% Dimethylpolysiloxane) coupled to a 5m x 0.25mm x 0.15um DB-17ms column (equivalent to (50%-phenyl)- methylpolysiloxane). Optimized instrumental parameters are shown in Table 1.</p><p>The data were acquired using the high-resolution <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7250+GC%2FQ-TOF"><strong>7250 GC/Q-TOF</strong></a> at data rate of 50 Hz. For compound identification the Unknown Analysis tool of <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Quantitative+Analysis"><strong>MassHunter Quantitative Analysis</strong></a> software version 12.1 and the GC Image software version 2024 R3 were used. The linear retention indices (RIs) were used to increase confidence in compound identification. Statistical analysis was performed in Mass Profiler Professional (MPP) software version 15.1.</p><h4><strong>Results and Discussion</strong></h4><h5><strong>GCxGC Configuration&nbsp;</strong></h5><p>A GCxGC RFM method was developed to achieve an optimal chromatographic separation of all the allergens while also ensuring adequate sensitivity and carrier gas flow to the MS. GCxGC RFM setup included two detectors: the Q-TOF MS and the FID. The configuration provided an optimal flow to the MS of 1.3 mL/min (11.8% of total flow) maintaining a constant split between FID and MS throughout the entire oven temperature ramp. The configuration is shown in Figure 2.</p><h4><strong>Conclusions</strong></h4><ul><li>Allergens in fragrance samples have been analyzed using comprehensive GCxGC combined with the highresolution GC/Q-TOF and RFM.&nbsp;</li><li>Fragrances with different types of aroma were analyzed using the GCxGC/HRMS combined with statistical analysis to identify the major differentiating compounds that may contribute to the particular type of scent.</li></ul><h3><strong>2. Liège University / MDCW: Coupling of Vac-HS-SPME and GC×GC-qMS for simultaneous 5-HMF quantification and volatile profiling in honey</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/FL_01_Honey_Eggermont_D_c3a35d2053.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The presentation by D. Eggermont et al. explores a novel analytical approach for assessing honey quality and authenticity. The method focuses on the simultaneous quantification of 5-hydroxymethylfurfural (5-HMF)—a key marker of honey freshness, heat exposure, and compliance with EU regulations—and the untargeted profiling of semi-volatile organic compounds (sVOCs).</p><p>The core of the method is <strong>vacuum-assisted headspace solid-phase microextraction (Vac-HS-SPME)</strong>, which improves extraction efficiency for low and semi-volatiles by reducing gas-phase resistance and accelerating mass transfer. This is followed by <strong>comprehensive two-dimensional gas chromatography coupled with quadrupole mass spectrometry (GC×GC-qMS)</strong>, enabling high-resolution separation and detection of both derivatised 5-HMF and various sVOCs such as benzaldehyde, furfuralcohol, phenylethanol, and menthofuran.</p><p><strong>Instrumentation used in the method includes:</strong></p><ul><li><strong>SPME fiber:</strong> DVB/CAR/PDMS (1 cm)</li><li><strong>Thermal desorption and focusing:</strong> Markes and SepSolve</li><li><strong>GC×GC system: </strong>Shimadzu platform with apolar × polar column set</li><li><strong>Mass spectrometer:</strong> Quadrupole MS operated in SIM mode for targeted 5-HMF quantification and full scan for volatile profiling</li></ul><p>The method was rigorously validated (LoQ 4.7 µg/g, LoD 1.6 µg/g, recovery 98%, precision RSD 21%) and compared against HPLC-UV as the official method, showing comparable results with lower sample amounts and fewer preparation steps. Additionally, the technique aligns with green analytical chemistry principles due to its miniaturization, low solvent use, and energy efficiency. This makes it a promising tool for routine honey analysis and food quality control.</p><h3><strong>3. Shimadzu / ASMS: Advancing PFAS Detection in Drinking Water: GC-MS as a Complementary Technique to LC-MS for Closing PFAS Mass Balance</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_25_WP_133_fcfd7e41b2.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Analysis of per- and polyfluoroalkyl substances (PFAS) in the environment is pivotal. There are several standardized PFAS methods, such as EPA 533, 537.1 8327, 1633, OTM-45 and OTM 50. Most of these methods are based on Liquid Chromatography/Mass Spectrometry (LC/MS) techniques. However, LC/MS is not suitable to analyze all PFAS compounds because of the diverse physico-chemical properties of chemicals within the PFAS family. Gas Chromatography/Mass Spectrometry (GC/MS) as a complementary technique can address volatile PFAS compounds that are challenging to analyze by LC/MS. In this study, a Head-Space Solid Phase Microextraction Triple Quadrupole Gas Chromatography/Mass Spectrometry analytical method is used to analyze PFAS in drinking water. This technique has advantages of analyzing volatile PFAS in water with minimum sample preparation procedure.</p><h4><strong>Methods</strong></h4><p>A volatile PFAS analysis method was developed on a Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8040"><strong>GCMS-TQ8040</strong></a> NX with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=AOC-6000+Plus"><strong>AOC-6000 Plus</strong></a> multifunctional autosampler equipped with a solid phase microextraction (SPME) module (Figure 1).&nbsp;</p><p>Thirteen PFAS target compounds were included in the Multiple Reaction Monitoring (MRM) method. The PFAS chemical classes were perfluoroalkyl iodides (PFIs), (n:2) fluorotelomer iodides (FTIs), (n:2) fluorotelomer acrylates (FTACs), (n:2) fluorotelomer methacrylates (FTMACs), (n:2) fluorotelomer alcohols (FTOHs) and perfluoroalkane sulfonamides (FASAs). Internal standards (IS) FTOHs, FASAs and FTAC mass-labelled compounds were added to each vial prior to extraction. Concentrations of the target compounds were calculated using isotope dilution.&nbsp;</p><p>An internal calibration curve was prepared in 10 mL of reagent water at concentrations of 2000, 1000, 500, 100, 50, 10, 2.5 and 1 ng/L. The IS were spiked at 100 ng/L to each calibrator. Sodium Chloride (NaCl) was added to each vial to achieve a final salinity concentration of 2% NaCl (w/v). These calibrators were vortex for 30 seconds and then placed on the AOC-6000 Plus autosampler rack for analysis.</p><p>The optimized parameters of the HSSPME GC/MS method for the targeted PFAS are listed in table 1. Quantifier and qualifier ions for each PFAS target are listed in table 2. The associated internal standard used for each compound is also listed in table 2.&nbsp;</p><p>A laboratory control sample (LCS) was analyzed to determine the general performance of the method in a clean matrix. Drinking water analyzed in the study were from a private well and an utility with surface water as its source.</p><h4><strong>Conclusion</strong></h4><p>This study demonstrated the satisfactory performance of a HS-SPME GC/MS/MS method to measure PFAS in drinking water. The PFAS family is vast, comprising thousands of different compounds across various chemical classes. Due to this diversity, multiple analytical instruments are necessary to effectively analyze PFAS. While LC-MS is widely recognized for its ability to analyze many PFAS compounds, it is not always practical for measuring certain PFAS. This has led to a gap in the environmental mass balance, especially when it comes to measuring volatile PFAS compounds. Fortunately, unlike LC-MS, GC-MS is well-suited for analyzing volatile PFAS compounds. GC-MS complements LC-MS-based PFAS methods, providing a more comprehensive analytical solution. By expanding the PFAS target list, GC-MS helps close gaps in the PFAS environmental mass balance. The method used in this study demonstrated quantitative capability in analyzing nanogram per liter PFAS compounds in an LCS and matrix influenced drinking water samples.</p><h3><strong>4. Thermo Fisher Scientific: Method transfer to the EXTREVA ASE Accelerated Solvent Extractor&nbsp;</strong></h3><ul><li>Technical note (White paper)</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/wp_001751_sp_extreva_ase_method_transfer_wp001751_en_c7884e1151/wp-001751-sp-extreva-ase-method-transfer-wp001751-en.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=EXTREVA+ASE"><strong>EXTREVA™ ASE™</strong></a> Accelerated Solvent Extractor (Figure 1) is a system based on many proprietary technologies including gas-assisted solvent extraction and parallel accelerated solvent extraction. This fully automated system combines the extraction and evaporation capabilities in one instrument, and it can be conveniently used for extracting and concentrating/evaporating extracts from up to 16 solid and semi-solid samples per batch (i.e., 4 sequences of 4 sample cells in parallel). The EXTREVA ASE system combines elevated temperatures and pressurized gas with liquid solvents to achieve fast and efficient collection of analytes from various matrices. The system can use up to six different extraction solvents (or mixtures of them) and extract up to four cells in parallel. The gas-assisted solvent extraction comprises delivering a mixture of extraction solvents and nitrogen gas to the stainless-steel cell to reach the working pressure of 200 psi (~14 bar). The combined effect of temperature and pressure greatly increases the efficiency of the extraction process, significantly reducing the amount of time and solvent required for extraction when compared to traditional techniques such as Soxhlet. The enrichment/concentration process starts immediately after the completion of the extraction step without any analyst interaction, if no offline cleanup of extract needed. The extracts can be evaporated to dryness or concentrated in 2 mL vials to volumes as low as 0.3 mL, with the final volume controlled by artificial intelligence machine vision (Figure 2). Succinctly, the EXTREVA ASE system automates extraction, in-cell clean up, and evaporation, which frees up the analyst’s time for other, more demanding tasks.</p><p>A schematic diagram of the EXTREVA ASE Accelerated Solvent Extractor is shown in Figure 2. This white paper describes the method transfer from a Thermo Scientific™ Dionex™ ASE 350 Accelerated Solvent Extractor to the EXTREVA ASE system, and provides instructions for new EXTREVA ASE system methods.</p><h4><strong>Which options to choose for a particular application?&nbsp;</strong></h4><p>The EXTREVA ASE system workflows comprise three main options: extraction only, evaporation only, or extraction and evaporation combined (integrated) depending on the option of the instrument.&nbsp;</p><p><strong>1. Extraction only:</strong> No evaporation. After extraction, the analyst may perform an offline cleanup, and, subsequently, perform sample enrichment. If evaporation is performed after cleanup, the analyst needs to manually load cells and evaporation bottles back onto the EXTREVA ASE system as per the evaporation workflow below.&nbsp;</p><p><strong>2. Evaporation only:</strong> Evaporation has two modes of operation: evaporation to dryness or evaporation to a fixed volume. When evaporating to a fixed volume, the minimum and maximum volumes are 0.3 and 1.6 mL, respectively. When evaporating to dryness, automatic end point detection is not available; therefore, the analyst needs to optimize evaporation conditions, such as temperature, vacuum and nitrogen gas flow, in order to complete this process in the minimum amount of time while meeting analysis requirements.&nbsp;</p><p><strong>3. Extraction and evaporation combined (integrated):</strong> Extraction followed by evaporation either to dryness (such as fat extraction) or fixed volume (such as PAH, OCP, and PCB) can be pursued based on the need of a particular application or target analytes.</p>

News from LabRulezGCMS Library - Week 28, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 7th July 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 / ASMS, Thermo Fisher Scientific / ASMS </strong>and<strong> Waters Corporation / ASMS!</strong></p><h3><strong>1. Agilent Technologies: Rapid and Sensitive Analysis of Antifungal Agents in Human Serum Using the Agilent 6475 LC/TQ</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_antifungal_human_serum_5994_8338en_agilent_89f89cb4dc.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In addition to minimizing drug-related toxicity, TDM has been hailed as a key step to prevent the emergence of drug resistance. The growing number of invasive fungal infections creates a ripple effect on the rapid advancement of TDM for antifungal agents. Increasing evidence confirms the critical role of TDM in preventing and treating antifungal infections.1 The RECIPE ClinMass TDM kit system for antimycotics in serum (Munich, Germany) was used on a 6475 LC/TQ for the analysis of eight antifungal agents. This application note demonstrates the evaluation and validation of the RECIPE TDM kit, covering sensitivity, linearity, and robustness across five consecutive days (n =&nbsp;5). Quick and simple sample preparation was implemented, providing high-throughput monitoring of antifungal agents in biological&nbsp;samples.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation</strong></h5><ul><li><strong>Liquid Chromatography System&nbsp;</strong><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=Agilent+1290+Infinity+II"><strong>Agilent 1290 Infinity II</strong></a> High-Speed Pump&nbsp;</li><li>Agilent 1290 Infinity II Multisampler&nbsp;</li><li>Agilent 1290 Infinity II Multicolumn Thermostat&nbsp;</li></ul></li><li><strong>Mass Spectrometry System&nbsp;</strong><ul><li>Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=6475+LC%2FTQ"><strong>6475 LC/TQ &nbsp;</strong></a></li><li>Agilent Jet Stream Technology Ion Source (AJS)</li></ul></li></ul><h5><strong>Method&nbsp;</strong></h5><p>The optimization of multiple reaction monitoring (MRM) transitions for analytes and ISTDs was carried out using Auto MRM Optimizer in the Agilent MassHunter acquisition software to provide optimal sensitivity and selectivity. Data were processed using the Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=MassHunter+Qualitative+Analysis+software"><strong>MassHunter Qualitative Analysis software</strong></a>, version B.12, and Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=MassHunter+Quantitative+Analysis+software"><strong>MassHunter Quantitative Analysis software</strong></a>, version B.12.</p><h4><strong>Results and discussion&nbsp;</strong></h4><p>Figure 2 shows the chromatograms of quantifier MRM transitions for the eight antifungal agents at the lowest calibration level. Six out of eight antifungal agents had good chromatographic separation across the run time. The retention times of two antifungals, posaconazole and hydroxy-itraconazole, were slightly overlapped. Despite this overlap, measurement integrity can still be maintained due to MRM selectivity.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A fast and sensitive analysis of eight antifungal agents in serum was validated on an Agilent 6475 triple quadrupole LC/MS. By employing a ready-to-use RECIPE ClinMass TDM kit, this method demonstrates accurate and precise quantitation of antifungal agents in biological samples. Additionally, the streamlined sample preparation method allows high throughput analysis of up to 350 samples per day.</p><h3><strong>2. Shimadzu / ASMS: Robustness Evaluation of PFAS Analysis in Soil Using 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/ASMS_25_WP_137_e932b391c7.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Per- and polyfluoroalkyl substances (PFAS) are widely used in various fields and industries. However, due to their structural stability and resistance to degradation, they accumulate in the environment and are suspected of being harmful to humans. PFAS in soil can accumulate in the human body via agricultural products, thus it is essential to develop sensitive and robust analytical methods for the detection of PFAS in soil with complex matrices.1 This study shows a robustness evaluation by adding 30 PFAS to a soil matrix and using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=LCMS-8060RX"><strong>LCMS-8060RX</strong></a> to measure these PFAS in the soil matrix 500 consecutive times.</p><h4><strong>Methods&nbsp;</strong></h4><p>For this analysis, LC-MS/MS equipped with a newly designed ESI source was used, and a delay column was installed between the mixer and the autosampler to inhibit the effects of PFAS contamination from the LC system. Six points calibration curves were built, and each calibration point was measured 3 times. A soil sample was prepared referring to part of the soil preparation procedures published by the National Agricultural and Food Research Organization. 2 Thirty PFAS compounds were spiked to the soil sample at 0.1 μg/L after pretreatment and 500 soil sample analyses were performed for the robustness evaluation. This sample contains more than 90% soil matrix. QC samples were also analyzed after every 20 injections of the soil samples.</p><h4><strong>Conclusion</strong></h4><p>The <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=LCMS-8060RX"><strong>LCMS-8060RX</strong></a> performed 500 consecutive measurements of 30 PFAS spiked to a soil matrix sample. The results showed good peak area repeatability, good peak shapes, and good recovery. The newly designed ESI source showed excellent robustness, and stable analysis was achieved over a long period, even for samples with complex matrices.</p><h3><strong>3. Thermo Fisher Scientific / ASMS: Evaluation of a modified Orbitrap Astral Mass Spectrometer for label-free quantitation of proteomic samples</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PO_439_ms_ASMS_25_Astral_Zoom_LFQ_po439_na_en_c1a0b2a11e.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The demand for high-throughput proteomics analysis of complex samples is continually increasing, focusing on greater analysis depth and improved precision and accuracy in quantitation. Label-free quantitation of very complex proteomic samples poses significant challenges for mass spectrometers, requiring faster and more efficient processing of eluting peptide ions and their fragments. The new Orbitrap Astral Zoom mass spectrometer addresses these challenges, offering a higher acquisition rate by improved ion optics switching times and faster ion transfer, higher sensitivity due to ion pre-accumulation, and enhanced spectral processing, leading to deeper coverage with higher confidence.</p><h4><strong>Materials and methods</strong></h4><h5><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Vanquish Neo</strong></a><strong>: Direct injection mode using 25cm x 75 μm ID Aurora Ultimate TS column (IonOpticks)&nbsp;</strong></h5><ul><li>High loads: 37min gradient; 4-45%B and injection-to-injection time 48min (30SPD)&nbsp;</li><li>Low loads: 20min gradient; 1-40%B and injection-to-injection time 28min (50SPD)&nbsp;</li></ul><h5><strong>Mass Spectrometer: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/836"><strong>Orbitrap Astra</strong></a><strong>l and </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom&nbsp;</strong></a></h5><ul><li>Orbitrap (MS1) and Astral (MS2) detectors&nbsp;</li><li>Orbitrap: 240K; m/z range 380-980; AGC 500%; max IT 5ms&nbsp;</li><li>NCE 25; Thermo Scientific FAIMS Pro Duo (low loads): -48V; gas 3.5 L/min</li><li>Astral: DIA; window size depending on loads (in the tables below); m/z 150-2000; AGC 800% (low loads) or 100% (high loads); max IT depending on load; cycle time: 0.6s&nbsp;</li></ul><h5><strong>Data Processing&nbsp;</strong></h5><ul><li>Spectronaut® v19.5 Direct DIA, 6 files (2 x 3 replicates) processed together for each load; all other settings were default&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1782"><strong>Thermo Scientific Proteome Discoverer software </strong></a>3.3.0.54, CHIMERYS 4.0.21</li><li>Human, E.coli, and Yeast FASTA (all w/o isoforms) from UniProt; normalization by Human FASTA</li></ul><h4><strong>Results (High Loads)</strong></h4><p>The new Orbitrap Astral Zoom mass spectrometer takes advantage of ion preaccumulation in the bent trap, increasing the effective MS2 injection time. Its reduced ion transfer overheads result in a higher MS2 acquisition rate of up to 270 scans per second. Additionally, an enhanced spectral processing algorithm was implemented to deconvolute overlapping spectral features in MS2, for better handling spectra with increased spectrum density.&nbsp;</p><p>Using Orbitrap Astral Zoom MS and Spectronaut® 19.5 software, there was a 12-17% increase in IDs at the precursor level, 10-15% at the peptide level (stripped sequence), and 4-9% at the protein groups level. With Proteome Discoverer software, the gain was 12-19% at the DIA precursor level, 12-17% at the peptide level, and 4-7% at the protein group level. The increase in identifications was primarily observed for low-abundant species. Orbitrap Astral Zoom mass spectrometer also yielded, on average, a 15% higher median number of MS2 data points per peak, while maintaining consistently high quantitation precision and accuracy at the MS2 level.</p><h4><strong>Conclusions</strong></h4><p>The novel Orbitrap Astral Zoom mass spectrometer demonstrates improved performance for qualitative and quantitative analysis of complex proteomics samples over a wide range of sample loads spanning four orders of magnitude, from 100 pg to 1µg.</p><h3><strong>4. Waters Corporation / ASMS: Investigating Fire Fighter and E-waste Handlers Exposure to PFAS Using Liquid Chromatography and Cyclic Ion Mobility Mass Spectrometry</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008883_21620a6293.pdf"><strong>Full PDF for download</strong></a></li></ul><p>PFAS are persistent environmental pollutants linked to health risks, including cancer. Monitoring their levels in human biofluids provides insight into exposure pathways. However, the analysis of PFAS isomers is technically challenging due to their structural similarity. To overcome this, the study employs <strong>LC coupled with cyclic ion mobility mass spectrometry (LC-cIM-MS)</strong> using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/202"><strong>Waters SELECT SERIES Cyclic IMS</strong></a>, which adds a new separation dimension for better specificity.</p><h4><strong>Methods</strong></h4><p>Serum samples from Ghanaian firefighters and E-waste workers were prepared using <strong>solid-phase extraction (SPE)</strong> on 96-well µElution plates. A <strong>22-minute reversed-phase LC gradient</strong> was used for separation. The <strong>Cyclic IMS system</strong>, with ion mobility resolution R~65 and 145, enabled non-targeted PFAS analysis, including the generation of <strong>collision cross section (CCS)</strong> values to support compound identification.</p><h4><strong>Results</strong></h4><ul><li>PFAS compounds such as <strong>PFOS, PFHxS, PFHpS, PFNA</strong>, and <strong>6:2 FTS</strong> were identified in real serum samples.</li><li>The <strong>cyclic IMS</strong> allowed for the separation of coeluting isobaric compounds, such as <strong>PFOS isomers</strong> and <strong>cholic acid biomarkers</strong>, minimizing false identifications (Figure 3).</li><li><strong>Figure 4</strong> lists CCS values and other parameters for PFAS standards and identified analytes from a firefighter serum sample.</li><li><strong>Figure 5</strong> shows ion mobility conformeric profiles for <strong>PFNA</strong>, enabling reliable identification even at low signal intensities.</li></ul><h4><strong>Conclusion</strong></h4><p>The LC-cIM-MS method:</p><ul><li>Significantly improves specificity in PFAS identification.</li><li>Enables both <strong>targeted and untargeted detection</strong> of known and unknown PFAS in complex human samples.</li><li>Can be a key part of future occupational and environmental exposure assessments.</li></ul>

News from LabRulezLCMS Library - Week 28, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 7th July 2025? Check out new documents from the field of spectroscopy/spectrometry and related techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT SPECTROSCOPY/SPECTROMETRY RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> libraries.</p></blockquote><p>This week we bring you brochure by <strong>Anton Paar, </strong>poster by<strong> Shimadzu / ASMS </strong>and application note by<strong> Thermo Fisher Scientific</strong>!</p><h3><strong>1. Anton Paar: Dynamic Shear Rheometers for Asphalt SmartPave</strong></h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/C92_IP_013_EN_K_Brochure_Smart_Pave_screen_dda7b47acc.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The <strong>SmartPave brochure</strong> introduces a family of dynamic shear rheometers (DSR) – <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=444&amp;search=SmartPave+92"><i><strong>SmartPave 92</strong></i></a>, <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=444&amp;search=SmartPave+102e"><i><strong>SmartPave 102e</strong></i></a>, and<a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=444&amp;search=+MCR+502e+Power"><strong> </strong><i><strong>MCR 502e Power</strong></i></a> – specifically developed for the demanding rheological characterization of asphalt binders and bitumen. These instruments meet international standards such as AASHTO, ASTM, DIN EN, and others, and support a wide temperature range, enabling tests for routine quality control, research, and advanced performance grading.</p><p>Each SmartPave system is equipped with innovative features like EC motors for high-precision torque control, <strong>Toolmaster™</strong> for automatic tool recognition, and <strong>TruRay™</strong> sample illumination. The Peltier-based temperature control – with heating from both above and below – ensures fast, accurate, and stable temperature conditions without water circulation. This allows fully dry operation, which is particularly important for repeatable and noise-free measurements.</p><p>The brochure outlines various standard and advanced testing methods, such as <strong>Superpave PG grading (AASHTO T315)</strong>, <strong>MSCR tests (AASHTO T350)</strong>, <strong>viscosity measurements (ASTM D4402)</strong>, and <strong>GTR-modified asphalt analysis</strong>. Advanced applications include DMA on solid asphalt, master curves, and low-temperature measurements down to –160 °C. The modular system supports multiple geometries including parallel-plate, cone-plate, and concentric-cylinder setups.</p><p>All systems operate with the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=444&amp;search=RheoCompass+software"><strong>RheoCompass® software</strong></a>, offering intuitive test design, automated calibration, standard operating procedures (SOPs), and customizable analysis. This makes SmartPave systems ideal for both routine lab use and advanced asphalt R&amp;D, offering unmatched performance, ease of use, and compliance with global asphalt testing standards.</p><h3><strong>2. Shimadzu / ASMS: Arsenic Speciation in Rice and Rice Products using LC-ICP-MS: A Sensitive and Reliable Approach by Shimadzu&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_2025_THP_065_99cfe0ebbb.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Arsenic toxicity is a major public health concern, particularly in drinking water, leading to strict regulatory limits worldwide. While total arsenic has traditionally been measured, its toxicity largely depends on its chemical form with inorganic species Arsenite and Arsenate (As(III) and As(V)) being highly toxic and carcinogenic, and organic forms monosodium methyl arsenate (MMA) and disodium methyl arsenate (DMA) displayed in fig. 1, considered less harmful. Speciation analysis is therefore essential for accurate risk assessment.&nbsp;</p><p>Rice and rice-based products are of particular concern, as rice can efficiently accumulate inorganic arsenic from the environment. In response, the European Union established maximum residue levels (MRLs) for inorganic arsenic in rice under Commission Regulation (EU) 2015/1006, highlighting the need for precise speciation.&nbsp;</p><p>To address this, advanced techniques like liquid chromatography coupled with inductively coupled plasma mass spectrometry (LC-ICPMS) are employed. LC-ICPMS provides high sensitivity and specificity for arsenic species determination, ensuring regulatory compliance and protecting consumer health.&nbsp;</p><p>This study presents the effective use of Shimadzu’s <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=LC-ICPMS-2050+LF"><strong>LC-ICPMS-2050 LF</strong></a> system for arsenic speciation in rice and related products.</p><h4><strong>Methods and Materials</strong></h4><p>All standard stock solutions are prepared as specified in the LC-ICP-MS Method Package for Arsenic Speciation Analysis Type-2 by Shimadzu, Japan. Seven levels of mixed calibration standards are prepared and injected for the quantification of arsenic species. Calibration curves are generated using the external standard calibration method with a 1/l weighted regression. All samples are prepared in duplicate to verify method performance. Additionally, two spiked samples containing only inorganic arsenic standards are included to evaluate the extraction efficiency of the method.&nbsp;</p><p>The Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=ICPMS-2050+LF"><strong>ICPMS-2050 LF</strong></a>, coupled with the Nexera LC series (Fig. 2), manufactured by Shimadzu Corporation, Japan, is used to separate and quantify the different arsenic species present in the samples.</p><h4><strong>Conclusion&nbsp;</strong></h4><ul><li>The extraction procedure employed effectively ensures the recovery of inorganic and organic arsenic species from various sample types, including both raw and processed materials.&nbsp;</li><li>A highly sensitive method based on hyphenated techniques, specifically LC-ICPMS, is developed for the speciation and quantification of arsenic using the Shimadzu ICPMS-2050 LF coupled with a Nexera inert LC system.</li></ul><h3><strong>3. Thermo Fisher Scientific: EDXRF analysis of coal fly ash as loose powders Ling Yok Ung, Application Specialist</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/edxrf_analysis_of_coal_fly_ash_as_loose_powders_an41971_en_2960bf7ad9.pdf"><strong>Full PDF for download</strong></a></li></ul><p>All the waste that remains after coal is burned, often in a coalfired power station, is referred to as coal ash. Coal ash may contain lead, mercury, arsenic and many other heavy metals. Fly ash and bottom ash are two subcategories of coal ash, typically separated based on particle size.&nbsp;</p><p>More than half of coal leftovers are fly ash, the most abundant and well-known component. Particles of fly ash, the lightest type of coal ash, “fly” up into a power plant’s exhaust stacks because they are so light. About 99 % of the ash are captured by filters inside the stacks, which draw it in with opposing electrical charges. Fly ash can be recycled. The fine particles are a perfect material for wallboard and concrete because they bond together and solidify, especially when combined with water.&nbsp;</p><p>But fly ash from coal is also a dangerous industrial solid waste. The natural environment and human health are seriously threatened by its excessive worldwide production, inappropriate disposal methods, underutilization, and lack of knowledge about its inherent risks. Therefore, a method that is quick, precise, and accurate, is required to quantify coal fly ash. Many companies use X-ray fluorescence spectrometry (XRF) as a preferred technology for process and quality control since it is a proven analytical approach that can accurately assess the chemical composition of materials with limited sample preparation.</p><h4><strong>Instrumentation&nbsp;</strong></h4><p>The <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1209"><strong>Thermo Scientific™ ARL™ QUANT’X EDXRF Spectrometer</strong></a> is equipped with a Silicon Drift Detector (SDD) and a 50 Watt Rh or Ag target X-ray tube which is air cooled with a maximum excitation v The Thermo Scientific™ ARL QUANT’X™ EDXRF Spectrometer is equipped with the following features: and radiation of heat in our atmosphere; N2 and O2 which are present in much higher concentrations do not have this same characteristic effect. Atmospheric CO2 levels increase the temperature of the surface of our planet, simultaneously excess CO2 is dissolved into the oceans gradually lowering the water’s pH, thus making the seas more acidic.&nbsp;</p><ul><li>Silicon drift detector (SDD): The SDD remains the performance benchmark for all energy dispersive detectors. The large active area of 30 mm² enables effective capture of characteristic element X-rays emitted by the sample.&nbsp;</li><li>50 W Rh or Ag target X-ray tube: Air-cooled with a maximum excitation voltage of 50 kV.&nbsp;</li><li>Nine primary beam filters: Designed to optimize the peak-to-background signals for all elements from F to Am.&nbsp;</li><li>10-Position auto-sampler with spinner: Allows for unattended analysis of multiple samples.</li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>This application note shows the suitability of the ARL QUANT’X EDXRF Spectrometer for the analysis of coal fly ash samples. This compact instrument allows for reliable and fast analysis of coal fly ash. Accuracy and repeatability results show that satisfactory results are obtainable for an analysis of loose powder in vacuum. This is a significant advantage for simple sample preparation while providing good accuracy &amp; precision.</p>

News from LabRulezICPMS Library - Week 28, 2025

<p><strong>A pressurized liquid extraction and GC/MS (PLE-GC/MS) method was developed for quantifying seven model contaminants in recycled HDPE, selected based on EFSA and FDA recommendations. The method showed low detection limits, good repeatability, and high accuracy. Extraction was optimized using acetone at 100 °C for 6 min.</strong></p><p>This method was applied in a challenge test to evaluate an innovative HDPE recycling process using limonene for polymer dissolution and precipitation. The results confirmed high cleaning efficiency, demonstrating both the effectiveness of the recycling process and the suitability of the PLE-GC/MS method for such evaluations.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986"><strong>Pressurized liquid extraction and GC/MS determination of model contaminants in HDPE - Application to recycling of post-consumer polyolefins using limonene</strong></a></h4><p>Javier Blázquez-Martín, Jorge García-Barrasa, María Teresa Tena&nbsp;</p><p>Journal of Chromatography A, Volume 1745, 2025, 465749</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1016/j.chroma.2025.465749">https://doi.org/10.1016/j.chroma.2025.465749</a></p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/"><strong>CC-BY 4.0</strong></a></h6></blockquote><p><strong>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.</strong></p><p>World plastic production reached 400.3 million tonnes in 2022. Of the total, the production of polyolefins from fossil sources accounted for 45.2 %. The most produced polyolefins were polypropylene (PP) and polyethylene (PE: linear low density (LLDPE), low density (LDPE), medium density (MDPE) and high density (HDPE)) [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0001"><span>1</span></a>], with main applications in the packing industry [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0002"><span>2</span></a>].</p><p>Of the 17.9 million tonnes of post-consumer packaging waste collected in the European Union in 2020, 46 % was recycled, 37 % was used for energy recovery and 17 % ended up in landfills [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0003"><span>3</span></a>]. This metric cannot be applied to polyolefins and is mainly due to the high recyclability of poly(ethylene terephthalate) (PET). HDPE recycling rates fall to 10 to 15 % in Europe [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0004"><span>4</span></a>]. As for other polymers (LDPE, PP and PS), recycling is limited as well [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0004"><span>4</span></a>].</p><p>A wide variety of extraction methods has been proposed for extracting additives and contaminants from plastics, such as total dissolution [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0022"><span>22</span></a>], solvent extraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0022"><span>22</span></a>], supercritical fluid extraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0023"><span>23</span></a>], pressurized liquid extraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0023"><span>[23]</span></a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0024"><span>[24]</span></a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0025"><span>[25]</span></a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0026"><span>[26]</span></a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0027"><span>[27]</span></a>] or microwave-assisted extraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0028"><span>28</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0029"><span>29</span></a>]. Pressurized liquid extraction is a technique that achieves higher efficiencies and lower operating times by using organic solvents at high pressures, allowing working with temperatures higher than the selected solvent's boiling point, which increases the diffusion and desorption of compounds from the polymer, as well as increasing compound solubility.</p><p>The analysis of the PE extracts has been carried out by gas chromatography/mass spectrometry (GC/MS) [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0022"><span>22</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0025"><span>25</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0026"><span>26</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0028"><span>28</span></a>], GC with a flame ionization detector (FID) [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0025"><span>25</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0026"><span>26</span></a>] or a thermoionic selective detector (TSD) [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0026"><span>26</span></a>], headspace solid phase microextraction and GC/MS [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0022"><span>22</span></a>], liquid chromatography (LC) with UV–Vis [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0023"><span>23</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0024"><span>24</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0027"><span>27</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0029"><span>29</span></a>] and MS detection [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0024"><span>24</span></a>]. GC is the preferred technique for volatile and low molecular weight compounds. Due to the volatile nature of some compounds of interest, and to allow a simultaneous detection, GC/MS was chosen for this study.</p><p>The aim of this work was to develop, optimize and validate a PLE and GC/MS-based method for the determination of seven model contaminants (proposed by the EFSA), as well as to demonstrate the cleaning efficiency of a recycling process intended for PE from different waste sources based on the dissolution-precipitation method with limonene by analysing artificially contaminated HDPE samples in a challenge test. The development of this method is of utmost importance since, to our knowledge, there are no validated procedures published for surrogates of challenge tests.</p><h4><strong>2. Materials and methods</strong></h4><h5><strong>2.4. FTIR characterization</strong></h5><p>FTIR characterization was performed to determine whether treated and untreated HDPE presented differences in its characteristic bands, as well as to determine the presence of residual limonene after the treatment. To carry out the measurements, a Perkin-Elmer FTIR spectrometer (Waltham, MA, USA) equipped with an ATR accessory was used. Resolution of 4 cm<sup>-1</sup>, 4 scans per measurement and room temperature were the selected conditions. Vibrational bands for HDPE and limonene have been assigned according to Da Silva and Wiebeck [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0031"><span>31</span></a>] and Schulz et al. [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0032"><span>32</span></a>] and can be found in Table S1 of the supplementary material.</p><h5><strong>2.5. Pressurized liquid extraction</strong></h5><p>A Dionex ASE 200 pressurized liquid extractor (Sunnyvale, CA, USA) with a solvent controller was used for the extraction process. 0.5 g of PC-HDPE flakes were placed into 11 mL extraction cells with sea sand filling up the void volume inside the cells. Extractions were carried out at 10.3 MPa (1500 psi) using acetone as solvent. Temperature varied from 60 to 100 °C, setting an upper limit below HDPE's melting point (120–130 °C) to prevent polymer melting. The extraction time varied from 2 to 10 min. The use of one, two, three and four extraction cycles was studied as well. The flush volume was 60 % and purge time was set at 60 s. A preheating step of 5 min was used. Acetone extracts containing the surrogates were transferred into volumetric flasks and made up with acetone to 50 mL after the addition of 1.25 mL of an internal standard solution. Aliquots of each extract were filtered through a 0.22 µm nylon syringe filter prior to GC analysis.</p><h5><strong>2.6. Chromatographic conditions</strong></h5><p>An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC"><strong>Agilent 8890 gas chromatograph </strong></a>coupled to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=5977B"><strong>Agilent 5977B single quadrupole mass spectrometer</strong></a> and an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7693A+autosampler"><strong>Agilent 7693A autosampler</strong></a> were used for GC analysis. The chromatographic column was an Agilent HP-5 ms (30 m x 250 µm x 0.25 µm) with a 5 % phenyl 95 % dimethylpolysiloxane phase.</p><p>The oven program started at 35 °C, holding for 0.5 min before raising the temperature to 60 °C at a rate of 10 °C min<sup>-1</sup>. Temperature was raised again to 280 °C at a rate of 70 °C min<sup>-1</sup> and maintained for 1.8 min.</p><div><p>Injection was done at 380 °C with an Agilent 5190–2293 4 mm I.D. liner in splitless-split mode (0.05 min in splitless mode). The carrier gas was helium at 1.0 mL min<sup>-1</sup>. MS detection was carried out by electronic impact, with an ionization source heated at 230 °C with a voltage of 70 eV. The quadrupole temperature was 150 °C. Chromatograms were registered in SIM mode. Chromatographic parameters for each compound are listed in <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#tbl0001"><span>Table 1</span></a>.</p><h4><strong>3. Results and discussion</strong></h4><h5><strong>3.1. GC/MS determination of surrogates</strong></h5><p>The analyte separation by GC was studied using surrogate standard solutions prepared in three different solvents: isopropanol, acetone and diethyl ether. Isopropanol was chosen first as it had been previously used for pressurized liquid extraction of additives in polyethylene [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0024"><span>24</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0025"><span>25</span></a>]. In addition, it is considered as a green solvent [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0033"><span>33</span></a>], but it was discarded because it has a higher boiling point than chloroform and, therefore, interfered with its detection.</p><p>Diethyl ether and acetone proved to be better candidates as they did not interfere with the detection of any of the surrogates. However, diethyl ether's lower boiling point led to the evaporation of standard solutions even under cooling conditions, so acetone was chosen to prepare the surrogate solutions for the GC/MS analysis. Acetone is considered a green solvent as well [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0033"><span>33</span></a>].</p><div><p>Due to the extensive range of boiling points (from 62 °C for chloroform to 443 °C for methyl stearate), both a high injection temperature (380 °C) and a low oven start temperature (35 °C) were needed. A non-polar low-bleed column was used to carry out the separation. A chromatogram of a solution containing 1000 µg <span>L</span><sup>-1</sup> of each surrogate in acetone is shown in <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#fig0001"><span>Fig. 1</span></a>. <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#tbl0001"><span>Table 1</span></a> shows the model contaminants, their physical properties and the chromatographic parameters for its detection.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Journal_of_Chromatography_A_Volume_1745_2025_465749_Fig_1_GCMS_SIM_chromatogram_of_a_standard_solution_containing_1_000_g_L_1_of_each_surrogate_53d33c9fd8.jpg" alt="Journal of Chromatography A, Volume 1745, 2025, 465749: Fig. 1. GC/MS SIM chromatogram of a standard solution containing 1,000 µg L-1 of each surrogate. 1: chloroform. 2: deuterated toluene. 3: toluene. 4: deuterated chlorobenzene and chlorobenzene. 5: methyl salicylate. 6: phenyl cyclohexane. 7: deuterated benzophenone and benzophenone. 8: methyl stearate." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Journal_of_Chromatography_A_Volume_1745_2025_465749_Fig_1_GCMS_SIM_chromatogram_of_a_standard_solution_containing_1_000_g_L_1_of_each_surrogate_53d33c9fd8.jpg 245w," sizes="100vw" width="1501" height="900"></p></div><h5><strong>3.4. Recycling method based on dissolution-precipitation</strong></h5><p>The analytical method developed was used in the evaluation of the cleaning efficiency of a recycling method based on the dissolution-precipitation of post-consumer HDPE using limonene as the dissolution solvent which is a greener alternative to the commonly used toluene or xylene. The addition of an antisolvent to precipitate the polymer was deemed unnecessary, as the polymer precipitated by cooling down the mixture.</p><p>Both the PC-HDPE flakes and the recycled polymer were characterized by FTIR. Attention was put to find characteristic signals of the polymer and residual solvents. Of the PC-HDPE samples analysed, only HDPE characteristic bands were found. For the ultra-cleaned HDPE, the characteristic bands of the polymer were found along bands for limonene, which meant that residues of the solvent remained after the ultra-cleaning method.</p><p>To ensure the absence of any residues of limonene in the precipitated polymer, a drying step was carried out. A soft temperature of 40 °C was chosen to prevent the polymer from degrading. Aliquots of a treated sample being dried in an oven were taken at different time intervals and stored in closed glass vials at room temperature until characterization. The IR spectrum of each aliquot was registered to analyze the trends of limonene characteristic bands over time of drying.</p><div><p>The IR spectrums were registered six times for the aliquot taken at <i>t</i> = 0 h and three times for the rest of the aliquots. For each spectrum, the signal areas of limonene's characteristic bands were obtained. The variation of mean signal area over time is shown in Fig. S4 of the supplementary material. At 9 days, no signals were found. A comparison of spectrums of ultra-cleaned HDPE with 0 and 9 days of drying at 40 °C is shown in <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#fig0003"><span>Fig. 3</span></a>. No differences in HDPE bands were found between the contaminated and ultra-cleaned polymer.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/JO_6_BE_2_1_7fccd4305a.jpg" alt="Journal of Chromatography A, Volume 1745, 2025, 465749: Fig. 3. FTIR spectrums of ultra-cleaned just after cleaning (A) and after 9 days of drying at 40 °C (B). Band assignment can be found in Table S1 of the supplementary material." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_JO_6_BE_2_1_7fccd4305a.jpg 103w," sizes="100vw" width="987" height="1500"></p></div><h4><strong>4. Conclusions</strong></h4><p>A PLE-GC/MS method for the determination of seven model contaminants in post-consumer and recycled HDPE was optimized, validated and applied to the evaluation of a novel recycling method based on the dissolution and precipitation of PC-HDPE with limonene.</p><p>GC/MS allowed the quantification of the model contaminants in a single analysis, using acetone as solvent. LODs suitable for the low concentrations expected in the recycled material were achieved. The PLE conditions were optimized with a central composite design, with the compromise values allowing a fast and automated extraction process.</p><p>This method was applied to evaluate the cleaning efficiency of a novel recycling method using limonene, following EFSA recommendations to carry out a challenge test. High cleaning efficiencies were achieved for all surrogates, proving the suitability of limonene and the dissolution-precipitation process to recycle PC-HDPE.</p><p>Moreover, the proposed analytical method allowed an easy, fast analysis of HDPE samples both before and after recycling, regardless of original application of the material, proving its adequate use during the evaluation of other novel recycling methods, whether they are mechanical, chemical or alternative processes. Lastly, the use of green and bio-based solvents, lower temperatures and shorter analysis times reduced the impact on the environment.</p></div>

Pressurized liquid extraction and GC/MS determination of model contaminants in HDPE - Application to recycling of post-consumer polyolefins using limonene

Systematic method optimisation approach for small molecule imaging on the SELECT SERIES MALDI MRT - Drug mapping in fingerprints, a case study

Improved sampling strategy for high-performance materials: The introduction of the stethoscope cell for online-LASIL experiments

<p><strong>In the week of July 14, the following webinars await you in the field of liquid phase and especially HPLC and LC/MS.</strong></p><blockquote><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></p><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>4 500 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. Agilent Technologies: It's not the analytes you see. It's the ones you miss that count. Unveiling Next-Gen LC-Mass Detection</strong></h5><ul><li>Tuesday, July 15, 2025, 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5291">Registration</a></li></ul><p>Discover the Agilent InfinityLab Pro iQ Series—next-gen LC-mass detection for fast, confident analysis and streamlined workflows in pharma, biotech, food, and environmental labs.</p><h5><strong>2. 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Agilent Technologies: Recycled Plastics in Food Packaging: Testing and Standards in India’s rPET Mandate</strong></h5><ul><li>Wednesday, July 16, 2025, 07:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5306">Registration</a></li></ul><p>Explore India’s rPET packaging regulations and testing methods using GC/MS, ICP-MS, and LC/MS. Ensure safety and compliance in recycled plastics for food contact with expert insights and case studies.</p><h5><strong>5. Phenomenex: Chromatography Modes Explained: Dive into the Modes of Chromatography!</strong></h5><ul><li>Wednesday, July 16, 2025, 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5225">Registration</a></li></ul><p>This webinar offers new LC users a solid introduction to HPLC principles and chromatography modes, including reversed phase, HILIC, ion exchange, and size exclusion.</p><h5><strong>6. Waters Corporation: Expanding the mass spectrometry and informatics toolsets for comprehensive analysis of large RNA constructs</strong></h5><ul><li>Wednesday, July 16, 2025, 16:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5288">Registration</a></li></ul><p>Learn how Waters and MKI enable streamlined mass spectrometry of large RNA constructs with advanced enzymes, reagents, informatics, and tools for mapping and quality attribute analysis.</p><h5><strong>7. 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Webinars LabRulezLCMS Week 29/2025

Improved sampling strategy for high-performance materials: The introduction of the stethoscope cell for online-LASIL experiments

Systematic method optimisation approach for small molecule imaging on the SELECT SERIES MALDI MRT - Drug mapping in fingerprints, a case study

Pressurized liquid extraction and GC/MS determination of model contaminants in HDPE - Application to recycling of post-consumer polyolefins using limonene

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How is capillary electrophoresis being used to analyze DNA and RNA