<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 30th June 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 other document 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: Agilent InfinityLab Assist Hub: Representing Advancements in Cybersecurity</strong></h3><ul><li>Other document (white paper)</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/wp_infinitylab_assist_cybersecurity_5994_8261en_agilent_310c5c9a6c.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>The laboratory as an operational technology (OT) environment: bridging the gap between OT and IT&nbsp;</strong></h4><p>Compared to connected industrial production environments, the connected laboratory environment closely aligns with an operational technology (OT) environment. OT is defined as "the practice of using hardware and software to control industrial equipment, and it primarily interacts with the physical world" (RedHAT, 2024).&nbsp;</p><p>In the classical Purdue reference model, established in the early 1990s to protect identities, information, and assets, the OT environment is clearly separated and secured from the information technology (IT)/enterprise environment.&nbsp;</p><p>The model only allows direct communication between adjacent levels. OT environments (lab environments) are necessary due to the long life cycles of the systems typically exposed to cybersecurity threats, with the mitigations listed in Table 1.&nbsp;</p><p>Addressing cybersecurity challenges in OT environments requires customized security strategies that incorporate both traditional IT security principles and specific measures for the physical operations they control.&nbsp;</p><p>Unlike some IT system components and devices where complete infrastructure replacement is common, lab devices are typically replaced gradually over years, sometimes even over&nbsp;decades.</p><p>The clear separation between OT and IT is becoming increasingly blurred due to new connectivity requirements, cloud functionality, and Industrial Internet of Things integration. This process, known as IT/OT convergence, is essential for achieving the next level of automation, such as Industry 4.0/5.0 or its counterparts, such as Pharma 4.0. The effectiveness of any new development will be evaluated based on how well it addresses cybersecurity within a converging IT/OT environment.</p><h4><strong>Standards and organizations&nbsp;</strong></h4><p>The diverse standards and organizations can be exemplified by the approaches taken in the U.S., Europe, and China. This summary aims to showcase the complexity of regulatory environments, and is not comprehensive. For specific situations, consulting with dedicated field experts is crucial.</p><h5><strong>Europe&nbsp;</strong></h5><p>European cybersecurity regulations prioritize privacy and data protection, with an emphasis on harmonizing standards across member states.&nbsp;</p><ul><li><strong>General Data Protection Regulation (GDPR): </strong>GDPR is the cornerstone of data protection in the European Union (EU). It sets strict rules on handling personal data, including requirements for data breach notifications, data minimization, and individual rights over personal data. Noncompliance can result in severe fines.</li><li><strong>Network and Information Security Directive (NIS&nbsp;Directive): </strong>Adopted in 2016, the NIS Directive focuses on the cybersecurity of essential services (such as energy, transportation, and finance) and digital service providers. It requires member states to strengthen their national cybersecurity capabilities and cooperation.&nbsp;</li><li><strong>European Union Agency for Cybersecurity (ENISA):</strong> ENISA is the EU's dedicated cybersecurity agency, helping to develop and promote cybersecurity standards across Europe, including guidelines for incident reporting and cybersecurity&nbsp;certifications.</li><li><strong>ISO/IEC 27001: </strong>While ISO/IEC 27001 is a global standard for information security management systems, it is heavily adopted in Europe. This standard outlines processes for systematically managing sensitive company information, ensuring its security.&nbsp;</li><li><strong>Cybersecurity Act (EU): </strong>The Cybersecurity Act establishes a framework for cybersecurity certification for products, services, and processes, ensuring they meet recognized EU-wide standards.</li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>With the initial release of the InfinityLab Assist Control Software, the InfinityLab Assist Hub offers plenty of cybersecurity features that can be leveraged for a secure lab network environment founded on a customer-specific OT/IT security strategy.</p><h3><strong>2. Shimadzu / ASMS: Single Quadrupole Mass Spectrometry Quick Workflows Specified to Oligonucleotides Screening&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_25_TP_605_fa8deb906e.pdf"><strong>Full PDF for download</strong></a></li></ul><p>A workflow has been developed to deliver molecular mass information on the full-length product and related impurities for chemically synthesized oligonucleotides by applying a deconvolution algorithm to all detected components within a targeted data stream (UV/PDA, TIC or BPC). It has been designed to simplify the data processing experience without the need for a sequence input delivering results quickly by automating mass assignment of all detected components in a data stream.</p><h4><strong>2. Materials and Methods&nbsp;</strong></h4><h5><strong>2.1 LC-MS/MS method&nbsp;</strong></h5><p><strong>20-mer sample.</strong> A phosphorothioate-modified oligonucleotide purified was used as a model sample (20-mer anti-sense oligo; C229 H316 N69 O121 P19 S19; average mass 7168.05, Te-smCe-sTe-sTe-sGe-sGd-sTd-sTd-sAd-sCd-sAd-sTd-sGd-sAd-sAd-sAe-sTe-smCe-smCesmCe) spiked with 10% impurities (N-1(5’) and N-3(5’) shortmers) to the full-length product.&nbsp;</p><p><strong>80-mer antisense DNA sample</strong>. 80-mer PolyT oligonucleotide sample (C800 H1041 N160 O558 P79; average mass 24273.62) was also analyzed was analyzed by ion-pair reversedphase chromatography mode using HFIP (hexafluoroisopropanol) and 10 mM TEA (triethylamine).</p><p><strong>LC Separation</strong>. Components were separated using the Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=Nexera+XS"><strong>Nexera XS</strong></a> inert LC and Shim-pack Scepter Claris column using HFIP (hexafluoroisopropanol) and 10 mM TEA (triethylamine) as ion pair additives.&nbsp;</p><p><strong>Mass Spectrometry Detection. </strong>Shimadzu Single Quadrupole<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=+LCMS-2050"><strong> LCMS-2050</strong></a>. Data acquired in profile mode. MS mass scan m/z 600-2000; 1 secs; negative ion mode.</p><h4><strong>3.Results&nbsp;</strong></h4><h5><strong>3.1 Workflows and Methods&nbsp;</strong></h5><p>Insight Biologics software application supports two workflows to help accelerate oligonucleotide characterization. The default data processing behavior was driven by a defined FLP sequence to confirm sequence composition, identify product related impurities and assess impurity profiles. Data processing has been further augmented by enabling automated deconvolution routines to be applied without a defined FLP sequence input to help workflows that need to quickly check on molecular mass information in a synthesis (Figure 2).</p><h4><strong>4. Conclusions&nbsp;</strong></h4><ul><li>LabSolutions Insight Biologics offers flexibility by supporting both user-defined and automated deconvolution workflows for comprehensive oligonucleotide analysis.&nbsp;</li><li>A Quick Picking algorithm has been developed and applied to the analysis of 20-mer and 80-mer antisense DNA. In the case of a 20-mer sample, the FLP and associated impurities were also automatically detected and molecular weight information reported. The analysis showed high correspondence with data processing results using a defined FLP sequence input.&nbsp;</li><li>The Quick Picking algorithm enables a molecular weight confirmation of any detected peak and can be a powerful tool for synthesis confirmation in cases where the product is not as intended.&nbsp;</li><li>This LC-MS analysis platform provides a rapid and cost-effective solution for purity analysis and molecular weight confirmation, making it ideal for quality control environments.</li></ul><h3><strong>3. Thermo Fisher Scientific / ASMS: Comprehensive data acquisition workflow on a modified Orbitrap Astral MS to achieve deep lipidome coverage with high confidence annotations</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PO_003964_ms_ASMS_25_Astral_Zoom_Lipidomics_po003964_na_en_0ccd4bd053.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Lipid identification is often considered the most challenging and bottleneck of the lipidomics workflow. This is due to the vast diversity of lipid structures, isomers and varying concentrations. Fragmentation of lipids generate characteristic fragments that help in lipid annotation, structural elucidation, isomer differentiation, and improved confidence in lipid identification. Having fragmentation for most of the lipids detected in a sample hence is highly desirable. This requires fast and sensitive instrumentation. Here we evaluated the new Orbitrap Astral Zoom mass spectrometer (Figure 1) for deeper lipidome coverage and confident lipid identification from 73 mice plasma extracts.</p><h4><strong>Materials and methods&nbsp;</strong></h4><h5><strong>Sample Preparation&nbsp;</strong></h5><p>Lipids were extracted from plasma samples obtained from 73 mice fed with a high fat diet and a normal diet. Lipid standards and bovine liver lipid extracts were purchased from Avanti Polar Lipids.&nbsp;</p><h5><strong>LCMS Method&nbsp;</strong></h5><p>Plasma lipid extract was separated using Thermo Scientific nanoLC PepMap (C18, 75µmx150mm, 2µm) column connected to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Vanquish Neo UHPLC system</strong></a>. Data acquisition was carried out on the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom mass spectrometer</strong></a> using full-scan Orbitrap MS1 in parallel with data-dependent Astral MS2.</p><h5><strong>Data Analysis&nbsp;</strong></h5><p>Data processing was performed using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1759"><strong>Thermo Scientific Compound Discoverer 3.4 software</strong></a>. Compound Discoverer 3.4 software includes new features such as Thermo Scientific LipidSearch software node for simplified lipid identification, QC for small molecule experiments using internal standards, automatically detects and groups MS1 fragments and other performance improvements.</p><h4><strong>Results&nbsp;</strong></h4><h5><strong>Orbitrap Astral Zoom mass spectrometer DDA MS2 scan rate&nbsp;</strong></h5><p>The Orbitrap Astral Zoom mass spectrometer offers an enhanced MS2 scan rate compared to the already high-speed Orbitrap Astral MS system, enabling DDA with Top 30, Top 40, or even Top 50 MS2 scans (Figure 2) without compromising data quality. This advancement delivers unprecedented speed, achieving faster DDA MS2 scan rates than ever before.</p><h5><strong>Unprecedented speed and depth: dual analyzer power of Orbitrap Astral Zoom MS</strong></h5><p>The parallel data acquisition on Orbitrap Astral Zoom MS using both the Thermo Scientific Orbitrap analyzer and Thermo Scientific Astral analyzer, enables a higher number of Orbitrap HRAM MS1 full scans with sub-ppm mass accuracy. Simultaneously, the fast Astral analyzer delivers a significantly greater number of highquality MS2 scans at 80k resolution (77% more) compared to Orbitrap-Orbitrap configurations, which is essential for deep coverage and confident lipid identification (Figure 3).</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>The novel Orbitrap Astral Zoom mass spectrometer provides deeper lipidome coverage and confident identification, utilizing the parallel operation of Orbitrap and Astral analyzers.&nbsp;</li><li>The enhanced MS2 speed in Orbitrap Astral Zoom mode, coupled with Stepped NCE, enables efficient data acquisition and comprehensive lipidome coverage with a 15% increase with grade A and B lipid annotation.&nbsp;</li><li>The use of nano-flow increased the sensitivity and the number of detected lipids while achieving a significant reduction in the use of sample and solvent.&nbsp;</li><li>A significant difference was observed between control and high fat diet mice samples with potential biomarker upregulated neutral lipids (triglycerides and cholesterol esters) in the high fat diet.</li></ul><h3><strong>4. Waters Corporation / ASMS: Routine EPA 1633 PFAS Analysis with a Novel Slotted Bandpass Ion Guide to Improve Signal Response Robustness</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008888_65b495feb8.pdf"><strong>Full PDF for download</strong></a></li></ul><p>With increasing regulatory pressure around PFAS monitoring, this study evaluates a robust and long-term solution for EPA 1633A-compliant PFAS analysis. It focuses on how the StepWave XR ion guide, integrated into the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=5&amp;search=Xevo+TQ+Absolute+XR"><strong>Waters Xevo TQ Absolute XR tandem quadrupole mass spectrometer,</strong></a> improves signal robustness and method stability across demanding environmental matrices such as river water, biosolids, and landfill leachate.</p><h4><strong>Materials and Methods</strong></h4><p>Samples included NIST-certified biosolids, landfill leachate, and spiked river water. Solid-phase extraction (SPE) was followed by LC-MS/MS analysis on an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY Premier System</strong></a> with BEH C18 columns and detection via the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=5&amp;search=Xevo+TQ+Absolute+XR"><strong>Xevo TQ Absolute XR</strong></a> using negative electrospray ionization and MRM. The robustness of the method was assessed over 12 weeks with over 9,000 injections and weekly calibrations, using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1544"><strong>waters_connect for Quantitation Software</strong></a> for data processing and review.</p><h4><strong>Results</strong></h4><p>Throughout the 12-week study, all sample types showed high consistency and low variability. For example, L-PFHxS in biosolids averaged 8.78 µg/kg (%RSD 7.2%) compared to the certified 9.39 µg/kg, while PFOA in landfill leachate showed a mean of 2.52 ng/mL (%RSD 2.7%). QC plots confirmed that all monitored PFAS met trueness and ion ratio targets across thousands of injections with no unscheduled downtime, highlighting the system’s long-term reliability.</p><h4><strong>Conclusion</strong></h4><p>The StepWave XR ion guide enabled reliable, high-throughput PFAS analysis with minimal maintenance and excellent reproducibility. The Xevo TQ Absolute XR maintained calibration stability, accurate quantitation, and strong matrix resilience across diverse sample types. Combined with streamlined software workflows, this setup is well-suited for routine EPA 1633A PFAS analysis in environmental labs.</p>

News from LabRulezLCMS Library - Week 27, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 21st 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 posters by <strong>Agilent Technologies / ASMS, Shimadzu / ASMS, Thermo Fisher Scientific / ASMS, Waters Corporation / ASMS</strong> and application note by<strong> Metrohm!</strong></p><h3><strong>1. Agilent Technologies / ASMS: De Novo PFAS Annotation and Classification Using Highly Accurate Formula Prediction and Kaufmann Algorithms Embedded in FluoroMatchSuite</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_fluoromatch_de_novo_pfas_annotation_asms_2025_wp_113_en_agilent_4190191ba4.pdf"><strong>Full PDF for download</strong></a></li></ul><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=FluoroMatch+Suite"><strong>FluoroMatch Suite </strong></a><strong>MS1 Only Algorithms: </strong>FluoroMatch Suite covers the entire non-targeted PFAS workflow (Figure 1) using MS/MS algorithms and the largest fragmentation database to date providing a &lt;5% false positive rate. However, MS/MS coverage is often incomplete, and DIA methods often provide lower quality spectra after deconvolution. Therefore, we developed MS1 only algorithms for providing highly accurate formula predictions (Figure 2) and for classifying features as PFAS or not PFAS using Kaufmann analysis (Figure 3)&nbsp;</p><p><strong>Validation: </strong>Algorithms were validated on NIST A and NIST C samples from the NIST PFAS interlaboratory study. NIST A consisted of known PFAS chemical standards, and NIST C consisted of an aqueous fire fighting foam (AFFF) contaminated soil sample. Formula prediction with homologous series voting (taking the most common repeating formula) was extremely accurate for both samples with a 0% false positive rate, and without homologous series voting the false positive rate was between 17-26% (Table 1). Kaufmann Analysis was highly specific for classifying PFAS with only 4% of non-PFAS being classified as PFAS with our Kaufmann based model, and only 6% of PFAS not be classified as PFAS according to our model for NIST C (Table 2).</p><h3><strong>2. Metrohm: Detection of heavy metals with differential pulse voltammetry</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_sens_002_download_aa3cc76472.pdf"><strong>Full PDF for download</strong></a></li></ul><p>DPV, alongside square wave voltammetry (SWV), already discussed in <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_sens_001_download_6ed955a5ff.pdf"><strong>AN-SENS-001</strong></a>, is another example of a pulsed voltammetric technique. DPV was actually developed first and is often linked to the field of polarography. This pulsed voltammetric technique is typically used with a dropping mercury electrode, although the general principle can be applied to static electrodes as well. In the case of DPV, a short pulse with constant height is superimposed at the end of every step of a staircase linear sweep voltammetry (LSV) determination (Figure 1). During the experiment, the current is sampled at two points: before (i1 ) and after (i2 ) the pulse. The difference (i1 -i2 ) vs. the potential is the signal which is plotted in DPV. Sometimes i1 is referred to as the base current and i2 as the pulse current. Figure 1. Typical DPV waveform for the forward direction (e.g., from 0 to 1 V).&nbsp;</p><p>Like SWV, this approach allows the separation of faradaic and capacitive current, boosting the sensitivity of the technique compared to normal staircase voltammetry. In <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=INTELLO"><strong>INTELLO</strong></a>, the i1 and i2 signals can optionally be sampled in the signals tab of the DPV command. In NOVA, custom plots of either signal can be produced in the same tab. The waveform is characterized by the height of the pulse (ΔE) and the step height (ΔEs ). The scan rate is determined only by step height and step duration of the underlying LSV. The pulse duration should not be set longer than the step duration in order to avoid artifacts, with typical values for the step being around 100–500 ms, and around 50 ms for the pulse. In comparison to SWV, DPV is considered less applicable to a wider range of systems due to the interference of oxygen and the slower scan rates required for DPV. In some cases it can produce better separation of closely positioned peaks and sharper peaks in general. The following is an example of a typical DPV measurement made with a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=PGSTAT302N"><strong>PGSTAT302N</strong></a> and the Metrohm 663 VA stand, with the same measurement also possible with the next-generation <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=VIONIC"><strong>VIONIC </strong></a>powered by INTELLO.</p><h4><strong>SAMPLE AND EXPERIMENTAL DETAILS&nbsp;</strong></h4><p>A PGSTAT302N equipped with a Metrohm 663 VA stand (2.663.0020) was used for this study. The working electrode (WE) was a Multi-Mode Electrode pro (6.1246.120) in the hanging dropping mercury electrode (HDME) configuration. The reference electrode (RE) was a double junction Ag/AgCl reference electrode (6.0728.120). All potential values mentioned in this Application Note are referred to the potential of this electrode. The electrolyte was composed of 10 mL H2 O + 0.5 mL of acetate buffer, made of 1 mol/L ammonium acetate + 1 mol/L acetic acid.&nbsp;</p><p>The concentration of heavy metal ions was quantified by making two standard additions. For the first addition, the solution was composed as follows: 10 mL H2 O, 500 μL acetate buffer, 100 μL Pb standard solution (1 mg/L), and 100 μL Cd standard solution (1 mg/L). For the second addition, the solution was composed as follows: 10 mL H2 O, 500 μL acetate buffer, 200 μL Pb standard solution (1 mg/L), and 200 μL Cd standard solution (1 mg/L).&nbsp;</p><p>Each measurement consisted of a step to precondition the Hg electrode, where nitrogen was purged in the stirring solution and a new Hg drop was formed. Then, a reduction potential of -0.9 V was applied at the Hg drop in order to reduce the Pb and Cd cations at the Hg drop surface under stirring conditions and accumulate them at the Hg drop. The stirrer was then switched off and the DPV measurement was performed by oxidizing the previously accumulated Pb and Cd in a positive potential sweep from -0.9 to -0.2 V. The DPV measurement was repeated twice.&nbsp;</p><p>The peak heights were determined from the current vs. potential plot of the three experimental iterations (i.e., sample, sample with first standard addition, and sample with second standard addition). Peak height vs. analyte concentration plots were created for both Pb and Cd. The analyte concentration in the sample can be calculated from the intersection of the regression line with the x-axis.</p><h3><strong>3. Shimadzu / ASMS: EPA 533 and 537.1 with the Novel LCMS-8050RX: Demonstration of Instrument and Method Performance to meet PFAS regulatory levels&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_25_TP_270_ebf0e2c9b0.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The harmful impacts of per- and polyfluorinated alkyl substances (PFAS) continue to afflict the environment. Water utilities require sensitive and robust analytical methods to assess the current and ongoing burden of PFAS from source waters to meet regulatory demands in treated water and to protect public health. Improvements in sensitivity and/or runtime without sacrificing robustness can aid laboratories by increasing sample throughput to better meet the significant demand for PFAS sample analysis. The novel RX probe was developed to yield better heat distribution and more consistent nebulization to improve sensitivity and reproducibility. Chromatographic improvements compared to existing EPA methods were also performed to decrease runtime while maintaining the integrity of sample analysis.</p><h4><strong>Methods</strong></h4><p>PFAS were separated by a Nexera LC and quantified by a Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-8050RX"><strong>LCMS-8050RX</strong></a> for EPA methods 533 and 537.1 (EPAM533 and EPAM537.1). Neat standards were analyzed in the required composition (i.e., 80% methanol for EPAM533 and 96% methanol for EPAM537.1). Standards were analyzed twenty times to determine the instrument detection limits.</p><h4><strong>Results and Conclusion</strong></h4><ul><li>All PFAS were sufficiently analyzed by the respective methods and passed regulatory criteria at a reduced runtime (19 minutes shorter).</li><li>Superb precision and reproducibility were demonstrated with the RX probe, which resulted in an analytical blueprint that greatly exceeds the Final PFAS National Primary Drinking Water Regulation promulgated in 2024.</li></ul><h3><strong>4. Thermo Fisher Scientific / ASMS: Comprehensive and high-throughput plasma proteome profiling for biomarker discovery using the Orbitrap Astral Zoom Mass Spectrometer and the Seer Proteograph ONE workflow</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_381_plasma_proteome_profiling_biomarker_discovery_po381_asms2025_en_074e0d2a50.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Plasma proteomics, the study of proteins in blood plasma, is crucial for biomarker discovery and understanding global signaling and immune responses1, aiding disease diagnosis, monitoring, and personalized medicine. However, the plasma proteome's complexity and dynamic range—spanning up to 12 orders of magnitude²—pose challenges, especially for detecting low-abundance proteins. Additionally, preanalytical, analytical, and biological variables complicate reliable biomarker identification, necessitating optimized techniques³. Liquid chromatography-mass spectrometry (LC-MS) excels in plasma proteomics due to its high analytical dynamic range and capability to measure peptides and characterize posttranslational modifications (PTMs). Advances in sample preparation, separation, MS, and data analysis are improving method sensitivity and robustness. We demonstrate the Thermo ScientificTM OrbitrapTM AstralTM Zoom Mass Spectrometer's high sensitivity and reproducibility in detecting a comprehensive plasma proteome across neat, depleted, and plasma processed with the Seer® Proteograph® ONE workflow, facilitating potential biomarker discovery¹.</p><h4><strong>Experimental Procedure</strong></h4><h5><strong>Liquid chromatography-mass spectrometry &amp; data analysis</strong></h5><p>All LC-MS runs for neat, depleted, and Proteograph ONE processed peptides were separated and analyzed using a Thermo Scientific <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Vanquish Neo UHPLC</strong></a> System in trap and elute configuration, paired with an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom Mass Spectrometer</strong></a>. Peptides were separated on the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Vanquish Neo UHPLC</strong></a> System using Thermo Scientific EASY-Spray PepMap analytical columns (ES906, 2µm C18, 150µm × 15 cm for 100 and 60 SPD and ES75500PN 2µm C18, 75µm × 50 cm for 24SPD) and 12.6-, 22.35-, and 54-minute chromatographic gradients, respectively, were formed using 0.1% formic acid in water for mobile phase A and 0.1% formic acid in 80% acetonitrile for mobile phase B. Samples were injected with 2 loading mass amounts (200/500 ng for 100/60 SPD; 500/1250 ng for 24 SPD) in triplicate. Liquid chromatography parameters are shown below in Table 1A. Mass spectrometer scan parameters can be found below in Table 1B. All data was processed using the Proteograph® Analysis Suite (PAS) (Seer). Output files were imported to Rstudio (2023.09.0 Build 463) with R (v4.3.1) for downstream data analysis and visualization.</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>With the Orbitrap Astral Zoom Mass Spectrometer, neat plasma proteome coverage exceeds 1,000 protein groups in a single pooled sample, providing exceptional quantitative precision without additional sample handling steps.&nbsp;</li><li>High Select Top 14 abundant protein depletion enhances plasma proteome depth by ~2x across 100, 60, and 24 SPD throughputs with comparable or superior analytical measurement precision.&nbsp;</li><li>Seer Proteograph ONE enhances plasma proteome depth by 7.9x (100SPD), 6.9x (60SPD), and 6.2x (24SPD) with comparable or superior analytical measurement precision and no compromise on sample preparation throughput.&nbsp;</li><li>The combination of the Orbitrap Astral Zoom Mass Spectrometer and the Proteograph ONE Workflow allows for over 7,000 protein groups to be identified from a single injection.&nbsp;</li><li>The speed, sensitivity, and robustness of the Orbitrap Astral Zoom Mass Spectrometer enables in-depth biological discovery, paving the way for novel findings and advancements in clinical cohort and population-scale translational research.</li></ul><h3><strong>5. Waters Corporation / ASMS: PFASt and Furious: A Targeted and Non-Targeted LC-MS/MS Study on the Environmental Impact of Using Fluorinated Ski Waxes&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008880_8590308c24.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This study by Waters Corporation explores the environmental impact of fluorinated ski waxes—specifically per- and polyfluoroalkyl substances (PFAS)—on soil and water quality at competitive ski sites in New England. Using both targeted LC-MS/MS and non-targeted high-resolution mass spectrometry, the research team analyzed samples from slalom and cross-country racing courses to determine the extent of PFAS contamination.</p><p>PFAS were found in all collected samples, with soil showing significantly higher concentrations than water. Long-chain perfluorocarboxylic acids, commonly used in ski waxes, dominated the contaminant profile. At slalom courses, the highest concentrations were found at the wax application zones near the start line, decreasing progressively downhill. At cross-country sites, similar patterns emerged near waxing and testing areas, with alarming migration of PFAS into adjacent ponds and even a vegetable garden.</p><p>The study employed automated sample preparation systems (CEM EDGE and Promochrom SPE-03) to ensure efficiency and reproducibility. Advanced LC-MS/MS analysis with Waters’ <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY Premier </strong></a>and <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/554"><strong>Xevo TQ Absolute</strong></a> platforms enabled the detection of common PFAS, while cyclic ion mobility HRMS revealed additional, untargeted long-chain species (e.g., C15/C16 carboxylic acids) not typically included in regulatory workflows.</p><p>The findings highlight the long-term environmental risks posed by legacy ski wax formulations and underscore the need for continued monitoring. Notably, unexpected PFOS levels in garden soil suggest multiple PFAS sources may be contributing to contamination, warranting further investigation.</p>

News from LabRulezLCMS Library - Week 30, 2025

News from LabRulezLCMS Library - Week 32, 2025

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

News from LabRulezLCMS Library - Week 40, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 6th October 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 other document by <strong>Agilent Technologies </strong>and posters by<strong> Shimadzu / AOAC, Thermo Fisher Scientific / ASMS </strong>and <strong>Waters Corporation / AOAC!</strong></p><h3><strong>1. Agilent Technologies: PFAS Food Legislation Overview</strong></h3><ul><li>Other document</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ebook_pfas_food_legislation_5994_8575en_agilent_dfe5a6222c.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This <strong>Agilent Technologies eBook</strong> provides an overview of <strong>global PFAS (per- and polyfluoroalkyl substances) regulations and analytical methods</strong> for monitoring these compounds in food, beverages, and food-contact materials. PFAS are synthetic chemicals valued for their water- and grease-resistant properties but are highly persistent and bioaccumulative. Their potential health risks—including immune suppression, elevated cholesterol, liver enzyme changes, and developmental effects—have prompted worldwide regulatory action to limit exposure through food and packaging.</p><p>In the <strong>European Union</strong>, <strong>Regulation (EU) 2023/915</strong> establishes maximum allowable levels of PFAS in various food products (e.g., meat, fish, eggs), ranging from 0.2 to 8 µg/kg depending on the matrix. <strong>Recommendation (EU) 2022/1431</strong> encourages member states to collect PFAS occurrence data and harmonize testing methods, while the upcoming <strong>Packaging and Packaging Waste Regulation (PPWR 2025/40)</strong> will, from August 2026, limit PFAS in food packaging to <strong>25 ppb per compound</strong> and <strong>250 ppb total</strong>. Analytical testing across Europe relies primarily on <strong>liquid chromatography coupled with tandem mass spectrometry (</strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?instrumentationItems=32&amp;mainauthorItems=10"><strong>LC/MS/MS</strong></a><strong>)</strong>, which provides the ppb-to-ppt sensitivity needed for regulatory compliance.</p><p>In the <strong>United States</strong>, the framework combines federal, state, and industry standards. The <strong>USDA CLG-PFAS 2.04</strong> method employs <strong>UHPLC/MS/MS</strong> to detect 16 PFAS in animal tissues, while the <strong>FDA C-010.03</strong> method quantifies 30 PFAS in food and feed using <strong>solid-phase extraction (SPE)</strong> followed by <strong>LC/MS/MS</strong>. The <strong>AOAC SMPR 2023.003</strong> standard defines performance criteria for PFAS testing across multiple food categories, ensuring validated and reproducible results. Several U.S. states—including Maine, California, and Washington—have also enacted specific limits for PFAS in meat, milk, and food-contact packaging.</p><p>In <strong>China</strong>, national standard <strong>GB 5009.253-2016</strong> specifies the determination of PFOS and PFOA in animal-derived foods via <strong>isotope-dilution LC/MS/MS</strong>. A new draft revision expands testing to 30 PFAS compounds (including isomers) across broader food matrices such as fish, vegetables, and milk. Chinese authorities have also introduced bans and restrictions on PFOS, PFOA, and PFHxS production and use, along with environmental management and disposal requirements.</p><p>Agilent offers <strong>comprehensive PFAS testing solutions</strong> for food laboratories, including robust <strong>HPLC and LC/MS instrumentation</strong>, validated methodologies aligned with EPA, EU, and ASTM standards, and a curated <strong>PFAS MRM database</strong>. The portfolio also features <strong>Captiva EMR PFAS Food cartridges</strong> pre-tested for background contamination, certified PFAS standards, and data-handling tools such as <strong>Agilent MassHunter</strong> and <strong>SLIMS</strong>. Together, these workflows enable reliable PFAS quantification, reduced contamination risk, and full compliance with international food-safety legislation.</p><h3><strong>2. Shimadzu / AOAC: Reliable and direct quantitative analysis of multi-mycotoxins in animal feed by using Shimadzu LCMS-8050RX</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/aoac_2025_m040_3bceabefcd.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Mycotoxins are toxic compounds produced by moulds that contaminate crops such as cereals, nuts, spices, dried fruits, apples, and coffee especially under warm, humid conditions. These chemically stable toxins can persist through food processing and pose serious health risks to humans and animals, ranging from acute poisoning to cancer and immunosuppressive. Among the many identified toxic compounds, Aflatoxins, Ochratoxin A, Fumonisins, T-2, Zearalenone, and Deoxynivalenol (DON) (Figure 1) are of particular concern. These are the most studied and regulated due to their significant impact on human and animal health, making their testing critically important. While conventional testing methods (HPLC-UV/FLD) are still common, regulatory focus is shifting toward LC-MS/MS testing due to its sensitivity and specificity.</p><p>The European Committee for Standardization (CEN), under the M/520 mandate, is developing standardized methods for this purpose. Mycotoxins are generally extracted via liquid–liquid (for milk, wine, juices) or solid–liquid extraction (for cereals, dried fruits, spices, feed), typically using acidic buffers. In this study, we developed a fast, highthroughput LC-MS/MS method for multi-mycotoxin detection in animal feed using the Shimadzu LCMS8050RX (Figure 2). MRM based quantitative method was developed using Shim-pack GIST C18-AQ HPLC column with an aim to achieve improved peak separation and required sensitivities for the compounds under study. A matrix-matched calibration curve (0.5–50.0 ppb) showed accuracy between 80–120 %, and recoveries (at 2.5 and 5.0 ppb) were 70–120 %, complying with SANTE guidelines[1] .</p><h4><strong>Materials and method</strong></h4><h5><strong>LC-MS/MS analysis</strong></h5><ul><li><strong>UHPLC:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+X3"><strong>Nexera X3</strong></a></li><li><strong>MS:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-8050RX"><strong>LCMS-8050RX</strong></a></li></ul><h4><strong>Conclusion&nbsp;</strong></h4><ul><li>Average recovery values for multi-mycotoxins in animal feed sample were found to be within the acceptance criteria as per the SANTE/12682/2019 guidelines.&nbsp;</li><li>The results obtained at 2.5 ppb and 5.0 ppb concentration level were accurate, repeatable and reproducible with RSD less than 20 %.</li><li>A simple liquid-liquid extraction method has been successfully developed and validated for the simultaneous quantification of nine mycotoxins in a single run.</li></ul><h3><strong>3. Thermo Fisher Scientific / ASMS: High-throughput proteomics using narrow window DIA on the Orbitrap Astral Zoom MS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_407_narrow_window_dia_proteomics_po407_asms2025_en_eea95fbc58.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The recently introduced Orbitrap Astral mass spectrometer has significantly expanded the scale and scope of proteomics experiments, advancing discovery and translational research. Building on this innovation, we demonstrate the performance of the next evolution of the platform, the Orbitrap Astral Zoom mass spectrometer, at throughputs ranging from 30 to 300 samples-per-day (SPD) analysing a HeLa digest using narrow window data-independent (nDIA) acquisition. The novel instrument features a higher acquisition rate (270 Hz vs. 200 Hz) achieved through improved ion optics settling times and faster ion transfers, increased sensitivity via pre-accumulation, and deeper coverage through enhanced spectral processing, among other improvements. Comparative analysis with the Orbitrap Astral MS reveals further improvements in peptide and protein group identifications enabling even deeper coverage at high throughput whilst maintaining precise quantitation.</p><h4><strong>Methods</strong></h4><p>HeLa digest standard measured on <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom MS</strong></a> and Thermo Scientific <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/836"><strong>Orbitrap Astral MS</strong></a> coupled to Thermo Scientific <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Vanquish Neo UHPLC</strong></a> utilizing 30-300 samples-per-day (SPD) LC-MS methods</p><h4><strong>Conclusions&nbsp;</strong></h4><p>The novel Orbitrap Astral Zoom mass spectrometer is, among its broad and comprehensive range of applications, an excellent instrument for high-throughput proteomics.&nbsp;</p><ul><li>High-throughput nDIA on the Orbitrap Astral Zoom MS generates deep coverage of proteomes</li><li><span>&nbsp;</span>The novel Orbitrap Astral Zoom MS further pushes the boundaries in terms of quantity and quality of identifications&nbsp;</li><li>The Orbitrap Astral Zoom MS enables precise quantitation with full flexibility to focus on MS2-based quantitation</li></ul><h3><strong>4. Waters Corporation / AOAC: Integration of Ultra-short Chain PFAS Into Routine Analysis Methods: Addressing Retention and Confirmatory Ions</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009019_f2e0c3e56f.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The poster presents a novel LC-MS/MS workflow enabling simultaneous quantification and confirmation of ultra-short through long-chain PFAS in a single analysis. The work was conducted using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>Waters ACQUITY Premier LC system</strong></a> equipped with a <strong>PFAS kit</strong>, <strong>Atlantis Premier BEH C18 AX mixed-mode column</strong>, and a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/554"><strong>Xevo TQ Absolute tandem mass spectrometer</strong></a> with <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1544"><strong>waters_connect software</strong></a> for quantitation.</p><p>The study addresses two analytical challenges: (1) the poor chromatographic retention of ultra-short chain PFAS (e.g., TFA, PFPrA) on conventional reverse-phase columns and (2) the absence of confirmatory ions for some short-chain PFAS, which typically produce limited fragment ions. Using the <strong>Atlantis Premier BEH C18 AX column</strong>, which combines reversed-phase and anion-exchange mechanisms, the authors achieved stable retention of C2–C4 PFAS. Optimized pH control using ammonium hydroxide and acetic acid further stabilized retention times of highly polar compounds.</p><p>For mass spectrometric confirmation, the team demonstrated the use of the <strong>m/z 19 fragment transition</strong> as a new confirmatory ion for PFAS that previously lacked one. On the <strong>Xevo TQ Absolute system</strong>, low-mass transmission enhancement significantly increased sensitivity for this ion, allowing confirmatory detection of PFBA and PFPeA even at low (ppt-level) concentrations. Ion ratio stability across calibration curves met common method validation criteria (±30%), demonstrating robustness for routine use.</p><p>The combined method enables the <strong>simultaneous analysis of ultra-short to long-chain PFAS</strong> in a single injection without requiring additional columns or HRMS verification. Results from landfill leachate and surface water samples confirmed the method’s capability to resolve co-eluting interferences and to reliably identify PFAS at environmentally relevant levels. This workflow offers an efficient and practical solution for laboratories transitioning to include ultra-short chain PFAS within standard monitoring methods.</p>

News from LabRulezLCMS Library - Week 41, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 20th October 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 posters by <strong>Agilent Technologies / AOAC,</strong> <strong>Shimadzu / AOAC </strong>and<strong> Thermo Fisher Scientific / HPLC Symposium </strong>and application note by <strong>Waters Corporation!</strong></p><h3><strong>1. Agilent Technologies / AOAC: Evaluating System Robustness of a High-Sensitivity Triple Quadrupole LC/MS for PFAS Analysis in Food Matrix Over an Extended Period&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_pfas_salmon_6495d_robustness_aoac_2025_t004_en_agilent_9b7b469a22.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Due to the rapidly evolving regulatory environment of per- and polyfluoroalkyl substances (PFAS), many analytical laboratories are opting to use highsensitivity triple quadrupole mass spectrometers for the targeted analysis of such compounds to ensure meeting present and potential future requirements for sensitivity and PFAS coverage. These assays are regularly conducted in a high-throughput manner involving complex matrices such as food, soil, wastewater or biological samples. Therefore, system robustness and instrument uptime are crucial for such applications to maintain productivity and profitability. In this work, we present results from an expedited robustness testing of a high-sensitivity triple quadrupole LC/MS system using select PFASs in one of the most challenging food matrices.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation</strong></h5><p>Data was collected using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Agilent+1290+Infinity+II+LC"><strong>Agilent 1290 Infinity II LC</strong></a> system coupled to an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6495D+LC%2FTQ"><strong>Agilent 6495D LC/TQ mass spectrometer.</strong></a> Instrument parameters are summarized in Tables 1 and 2.</p><h4><strong>Conclusions</strong></h4><p>The robustness of a 6495D LC/TQ was tested using undiluted salmon extract, a complex and challenging food matrix. During the experiment, the system was exposed to more than 130 mL of the matrix over a period of ~3 weeks of continuous operation, without any maintenance. System performance was monitored by injections of a mixture of native and isotopically labelled PFAS samples. The monitored signals exhibited low variations (RSD&lt;6%) throughout the entire experiment. No obvious performance degradation or significant contamination of the inner ion optics elements were observed after the conclusion of the test.&nbsp;</p><p>Although no loss of instrument performance was observed during this expedited robustness test, a routine maintenance of ion source and optics is recommended to ensure prolonged instrument operation.</p><h3><strong>2. Shimadzu / AOAC: Analysis of Chlordane by DUIS (Dual Electrospray/Atmospheric Pressure Chemical Ionization) Liquid Chromatography Mass Spectrometry&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/aoac_2025_w050_036db56f51.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The legalization of cannabis has led to many laboratories developing methods to meet local cannabis testing regulatory requirements. One of the challenging residual pesticides to quantitate is chlordane, an organochlorine compound used as a pesticide on crops until 1983 and for termite treatment in homes until 1988. Chlordane is highly persistent in the environment and has been linked to cancers. Gas chromatography mass spectrometry and atmospheric pressure chemical ionization (APCI) – liquid chromatography mass spectrometry (LCMS) methods were published for analysis of chlordane. However, for laboratories without APCI functionality or who prefer not to switch between two different ionization sources, chlordane remains a challenging target for LCMS analysis. This study demonstrates the successful quantitation of chlordane using additive-free DUIS electrospray ionization – LCMS at concentrations below the New York State testing limits.</p><h4><strong>Methods&nbsp;</strong></h4><p>Technical chlordane (CAS 57-74-9) was obtained from Restek, diluted in water, and analyzed on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-8060"><strong>Shimadzu LCMS-8060</strong></a> triple quadrupole mass spectrometer equipped with a DUIS ionization source. The DUIS source was utilized in APCI mode. Technical chlordane is a mixture of transchlordane, cis-chlordane, and related chemicals. The LC parameters shown in Table 1 allowed separation of the cis- and trans-chlordane isomers.</p><h4><strong>Results&nbsp;</strong></h4><p>Initial MS data was collected in Q1 and Q3 Scan mode. Due to the 8 chlorine atoms per chlordane molecule, a distribution of isomers is expected in the mass spectrum. LabSolutions Insight Explore was used to predict isotopic distributions for chlordane with and without adducts. The predicted spectra for the [M-H]- and [M+CH3OH]- are shown in Figure 1A and 1B, respectively. The experimentally observed isotopic distributions for the [M-H]- and [M+CH3OH]- ions are shown in Figure 1C and 1D, respectively. Figure 1E shows the relative intensity of the [M+CH3OH]- versus the [M-H]- isotope clusters. As the [M+CH3OH]- showed the greatest intensity, it was selected for optimization.</p><p>Voltage optimization was performed for the 441.80 to 441.80 MRM with the CID gas turned off. Even after voltage optimization, the signal-to-noise from the primary species in the technical chlordane (in this case, trans-chlordane) was insufficient. Automated source optimization using LabSolutions MRM Connect was used to improve signal by optimizing Interface Temperature, Heating Gas Flow, Nebulizing Gas Flow, Drying Gas Flow, DL Temperature, Heat Block Temperature, and Interface Voltage. As a representative example, Figure 3 shows the impact of Interface Temperature on the MRM intensity for the 441.80 m/z.</p><h3><strong>3. Thermo Fisher Scientific / HPLC Symposium: HPLC transfer and optimization of deoxycholic acid analysis using HPLC – Charged Aerosol Detector</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_hplc_transfer_optimization_deoxycholic_acid_analysis_po_en_55bc47dc90.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The United States Pharmacopeial Convention monograph outlines a high-performance liquid chromatography with charged aerosol detection (HPLC-CAD) method [1] for the accurate measurement of deoxycholic acid (also known as desoxycholic acid) and its primary impurity, cholic acid. Key detector settings that influence detection performance metrics such as detection limit, resolution, and linearity include:&nbsp;</p><ul><li>The evaporation temperature (EvapT) for setting the temperature of the evaporation tube and influencing sensitivity related to volatility factors.&nbsp;</li><li>The filter constant for balancing noise and adjusting the detector's response time to changes in analyte concentration.&nbsp;</li><li>The PV for optimizing the linear range within the detector's dynamic range for a given application.&nbsp;</li></ul><p>These parameters are crucial for successful method transfer and optimization. Consequently, this work offers guidelines for method transfer and optimization from the Vanquish CAD to the Vanquish CAD HP</p><p><strong>Methods:</strong> A <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/743"><strong>Thermo Scientific Vanquish Flex UHPLC system</strong></a> equipped with both the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2176"><strong>Vanquish Charged Aerosol Detector </strong></a>and HP was used to perform method transfer and optimization for deoxycholic acid analysis. Chromatographic separation was achieved using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2005"><strong>Thermo Scientific Acclaim 120 C18 column</strong></a> under gradient elution with formic acid-modified aqueous and organic phases</p><h5><strong>Chromatography Data System&nbsp;</strong></h5><p>The <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/76"><strong>Thermo Scientific Chromeleon 7.3.2 Chromatography Data System (CDS) software</strong></a> was used for data acquisition and analysis.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>This study highlights the successful optimization and method transfer of the USP-NF deoxycholic acid assay using Vanquish CAD detectors. Through careful evaluation of chromatographic performance, detector settings, and calibration parameters, the Vanquish CAD HP was shown to deliver enhanced performance across multiple criteria:&nbsp;</p><h5><strong>Key Takeaways:&nbsp;</strong></h5><ul><li><strong>Excellent Sensitivity and Response:</strong> Vanquish CAD HP demonstrated significantly lower LOD/LOQ values and higher peak responses compared to Vanquish CAD, making it the detector of choice for low-level analyte quantification.&nbsp;</li><li><strong>Enhanced method optimization Flexibility: </strong>Vanquish CAD HP allows simultaneous data collection for multiple PVs, ensuring faster method development and optimization.&nbsp;</li><li><strong>Seamless Method Transfer:</strong> Transitioning from Vanquish CAD to CAD HP was achieved by optimizing power value (PV), EvapT, and signal filter settings, ensuring improved performance.&nbsp;</li></ul><p>Together, these findings demonstrate that the Vanquish CAD HP not only supports efficient method transfer but also elevates performance, sensitivity, and usability—making it an ideal solution for modern HPLC applications.</p><h3><strong>4. Waters Corporation: Multi-Residue Analysis of Pharmaceuticals, Personal Care Products (PPCPs) and Pesticides in Water by Direct Injection Using LC-MS/MS</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008819_en_4c0e9bc91e.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>Benefits&nbsp;</strong></h5><ul><li>Sensitivity of Xevo TQ Absolute allows for the trace level detection of PPCPs and pesticides in drinking and surface waters without the need for lengthy clean-up or concentration steps</li><li>The direct injection approach increases productivity and provides faster turn-around time for reporting of results while being well aligned with green analytical chemistry principles</li><li>More than 150 analytes reach limits of quantification of 10 ng/L, making this method suitable for screening for multi-class analytes in water matrices&nbsp;</li></ul><p>In recent years, there has been increasing concern about the presence of pesticides, pharmaceuticals and personal care products (PPCPs) in water bodies throughout the world.1 The effect of these emerging contaminants on human health and their potential impact on the environment is not yet fully understood. The updated Drinking Water Directive entered into force in January 2021 and is the EU's main law for drinking water. The Directive applies to all water, either in its original state or after treatment, intended for drinking, cooking, food preparation or other domestic purposes, regardless of its origin and whether it is supplied from a distribution network, supplied from a tanker or put into bottles or containers.2 It further protects human health thanks to updated water quality standards, in accordance with World Health Organisation (WHO) recommendations, addressing emerging pollutants, such as endocrine disruptors, and promoting a preventive, risk-based approach to reduce pollution at its source.</p><p>Water bodies such as rivers, lakes and groundwaters have their status defined in the EU Water Framework Directive.3 An amendment to Directive 2013/39/EU sets environmental quality standards for hazardous substances that require monitoring in these waters. A Commission Implementing Decision4 document, 2022/1307, includes Watch List analytes with Maximum Acceptable Method Detection Limits for compounds of concern across multiple chemical classes. Numerous studies have demonstrated that PPCPs are present at parts-per-trillion (PPT) levels in rivers and streams highlighting the need for methods that are able to detect compounds at these trace levels.5-10 In addition to the low-level detection of these compounds, a major analytical challenge lies in the wide chemical diversity of chemicals of concern. Furthermore, to establish a more complete understanding of water pollution it is necessary to monitor a wide variety of types of water. This application note demonstrates the direct injection, separation and detection of PPCPs and pesticides including acidic, basic, and neutral compounds from multiple regulated analyte lists in a variety of water types.</p><h4><strong>Experimental</strong></h4><ul><li><strong>LC system:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY Premier</strong></a> FTN</li><li><strong>MS system: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/554"><strong>Xevo TQ Absolute</strong></a></li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>The updated EU Drinking Water and Water Framework Directives provide the regulatory framework for effective monitoring and management of water quality and include provisions for emerging contaminants. Ensuring compliance with these regulations and comprehensive coverage for an ever increasing analyte lists requires versatile, robust analytical methods and high performance LC/MS/MS systems. The direct-injection method investigated in this work is effective at detection of a wide range of PPCPs and pesticides at trace levels suitable for monitoring multiple water types for the presence of compound classes known or suspected to pose risks to human and environmental health. It further provides more rapid turn around time and greener operation than methods that rely upon high volumes of solvent and extensive sample preparation. Method performance was assessed using criteria described in ISO 21253–2:2019. The calibration characteristics, linearity, and residuals were excellent over the concentration range studied. Accuracy and precision were evaluated at three matrix QC levels with six replicate spikes and found to provide excellent performance for 154 analytes in tap and bottled water and 74 analytes in surface water matrix.</p>

News from LabRulezLCMS Library - Week 43, 2025

News from LabRulezLCMS Library - Week 48, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 8th December 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 notes by <strong>Agilent Technologies </strong>and<strong> Waters Corporation, </strong>technical note by <strong>Shimadzu </strong>and poster by <strong>Thermo Fisher Scientific / ASMS!</strong></p><h3><strong>1. Agilent Technologies: Robust and Reproducible Monitoring of PFAS in Treated Wastewater by Direct Injection on 6495D LC/MS</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_pfas_wastewater_lctq_5994_8346en_agilent_c2412e7d84.pdf"><strong>Full PDF for download</strong></a></li></ul><p>PFAS is a class of synthetic chemicals that are resistant to heat, water, grease, and oil. Exposure to this class of chemicals is widespread and their ability to move and persist in the environment makes them difficult to clean up. Found in everyday household and workplace products such as drinking water, food packaging, fish caught from compromised environments, and personal care products is an indication of how widespread the use of PFAS and its contamination in the&nbsp;environment.&nbsp;</p><p>Traditional techniques of analysis to enhance sensitivity incorporate the use of solid phase extraction, which allows enrichment of the sample before injection. Increased awareness of emerging contaminants has necessitated the need for higher throughput methods, some bypassing the sample preparation step, to decrease sample analysis time. Direct injection analysis can save time by removing the need to prepare samples but still providing robustness and reproducibility to justify its capabilities and improved&nbsp;efficiency.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><p><strong>Liquid chromatography system:&nbsp;</strong></p><ul><li>Agilent 1290 Infinity II Bio-LC High‑Speed Pump (G7132A)&nbsp;</li><li>Agilent 1290 Infinity II Bio-LC Multisampler (G7137B)&nbsp;</li><li>Agilent 1290 Infinity II Multicolumn Thermostat (G7116B)&nbsp;</li></ul><p><strong>Mass spectrometry system:&nbsp;</strong></p><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6495D"><strong>Agilent 6495D Triple Quadrupole LC/MS (G6495D)&nbsp;</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Jet+Stream"><strong>Agilent Jet Stream (AJS) Source</strong></a> A PFC free kit, together with a delay column, was also used.</li></ul><h4><strong>Results and discussion&nbsp;</strong></h4><p>The sensitivity of the method was calculated with ten spikes of water at 1&nbsp;ng/L resulting in the method detection limit. The calculated concentration was prior to dilution of methanol and demonstrates that all but three analytes were equal or less than 1 ng/L detection limits, the analytes with greater than 1&nbsp;ng/L MDL were 3:3 FTCA and 8:2 FTSA (Table 6).</p><h4><strong>Conclusion&nbsp;</strong></h4><p>The increased awareness of PFAS globally has meant that regulations are constantly being adopted and larger amounts of samples at lower limits are required. By incorporating the direct injection technique on the Agilent 6495D LC/MS we get a combination of high sample throughput while providing excellent analytical sensitivity. Also, increasing throughput and reducing consumables cost creates increased value in the instrument. The method displays a clean baseline and sensitivity with the observation of 1 ng/L detection in spiked wastewater. Reproducibility and robustness were measured between the concentrations of 0.5 to 100 ng/L on the 6495D LC/MS. The system was able to detect 38 PFAS between 0.25 to 3.4 ng/L with RSD &lt; 20% over 150&nbsp;direct injections, providing confidence in the data for a complex matrix like&nbsp;wastewater.</p><h3><strong>2. Shimadzu: A sustainable analytical approach for detecting extra virgin olive oil adulteration using Nexera™ UC</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c190_e341_c488032e81.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Knowledge of the composition of triacylglycerols (TAGs) in vegetable oils is important for dietary and nutritional reasons, due to the influence of the different properties of each fatty acid on the human organism. Specifically, extravirgin olive oil (EVOO) is a popular food ingredient worldwide, and for this reason, detecting economically motivated adulteration is important to protect consumers’ interest and health[1]. According to the latest report from the EU Food Fraud Network (European Union, 2021), olive oil (OO) tops the list of reported adulterated food products. The official methods to assess OO purity and detect the presence of extraneous vegetable oils include the analysis of fatty acids (FAs), triacylglycerols (TAGs) and sterols (Regulation (EU) No 2568/91 and its amendments) [2].&nbsp;</p><p>A variety of chromatographic techniques has been employed for TAGs analysis and separation. High-performance liquid chromatography (HPLC) methods, which use reversed-phase (RP) and silver-ion (Ag) columns for TAGs separation, have been employed either independently or in combination[3]. However, both these approaches have the drawback of relying on toxic organic solvents. The alternative separation technique employed in TAGs analysis is supercritical fluid chromatography (SFC) coupled with a UV detector at very low wavelengths, due to the weak UV absorption of the mobile phase. In this study, a fast, simple and green methodology was optimized to detect intentionally adulterated olive oil with cheaper seed oils at different levels by means of SFC with UV detection, followed by statistical analysis.</p><h4><strong>2. Experimental</strong></h4><h5><strong>2.2 SFC-PDA Nexera™ UC system&nbsp;</strong></h5><p>All experiments were performed on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera%E2%84%A2+UC"><strong>Nexera™ UC system</strong></a> (Shimadzu Europa, Germany). The system was equipped with a CBM-20A communication bus module, a DGU-20A5R degasser, an LC-30ADSF CO2 pump, one LC-20ADXR dual plunger parallelflow pump, a Sil-30AC autosampler, a CTO-20AC column oven, a SPD-M20A photodiode array (PDA) detector, and a SFC-30A backpressure regulator (BPR). Chromatograms were recorded using Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LabSolutions"><strong>LabSolution</strong></a> ver. 5.80 software. Four Ascentis Express C18 columns, provided by KGaA (Darmstadt, Germany), were connected in series for TAGs separation. The analytical conditions used are summarized in Table 1.</p><h4><strong>3. Results and discussion&nbsp;</strong></h4><p>Using four C18 columns packed with superficially porous particles, a highly efficient separation of TAGs with an isocratic elution mode was provided, allowed for complete sample TAG elution within 30 min with the conditions used in this method (Figure 1). Peak identification was carried out according to partition number (PN), the published composition of these common vegetable oils and the relative amount of major and minor peaks, and finally taking into account TAGs retention times. For compounds with identical PN, separation was achieved based on the number of unsaturations. The elution order of TAGs was primarily governed by the hydrophobicity of the solutes. As the PN increases, the non-polar character of TAGs becomes more dominant.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>The Nexera™ UC system provided excellent results for assessing TAGs composition in ten different vegetable oils examined in this study employing an SFC-PDA analytical method using isocratic mode and UV detection at 205 nm. This approach does not require any sample preparation and enables analyses to be completed with less waste and less cost compared to traditional methods, making it feasible for routine analyses, while providing reliable quantitative values.&nbsp;</p><p>Quantification of adulterated EVOO was performed by establishing curves based on peak areas of LLL marker versus seed oils concentrations. Statistical analysis using PCA and one-way ANOVA also visually distinguished adulterated EVOO from pure EVOO, and the result was in accordance with the present quantitative method. This fast and environmental method exhibits a huge potential for quality control and authenticity evaluation of EVOO.</p><h3><strong>3. Thermo Fisher Scientific / ASMS: Uncovering biological differences at scale: high-throughput and in-depth plasma proteomics with the Seer Proteograph ONE workflow and Orbitrap Astral Zoom Mass Spectrometer</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_393_uncovering_biological_astral_zoom_seer_po393_asms2025_na_en_f697aef9c0.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Plasma proteomics enables minimally invasive biomarker discovery by capturing disease-related molecular signatures. However, its effectiveness is limited by the wide dynamic range of protein concentrations. To address this, we combined the Seer Proteograph ONE workflow with the Orbitrap Astral Zoom mass spectrometer to enable a high-throughput, high-precision platform that delivers deep plasma profiling and actionable insights for large-scale clinical and translational research (Figure 1).</p><h4><strong>Methods:&nbsp;</strong></h4><p>The Seer Proteograph ONE workflow was used to prepare plasma samples from a small disease cohort with matched healthy controls to evaluate its performance and feasibility in detecting biologically meaningful differences. Samples were then separated and analyzed using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Thermo Scientific Vanquish Neo UHPLC system </strong></a>coupled to the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom mass spectrometer</strong></a>, enabling deep and reproducible proteome coverage. Two analytical approaches—a high-throughput method and a Max-ID workflow—were tested to demonstrate the versatility and throughput for comprehensive biomarker discovery in clinical cohort studies.</p><h4><strong>Results:&nbsp;</strong></h4><p>The Seer Proteograph ONE workflow with Orbitrap Astral Zoom mass spectrometer demonstrated that both high-throughput and Max-ID workflow were able to detect differences in biology in diseased states from healthy controls. The high-throughput workflow enabled rapid, reproducible analysis, while the Max-ID approach delivered deeper proteome coverage. The synergy between the Seer Proteograph workflow and Orbitrap Astral Zoom mass spectrometer supports scalable, high-resolution biomarker discovery, making it suitable for large clinical studies and precision medicine applications.</p><h4><strong>Conclusions&nbsp;</strong><span><strong>&nbsp;</strong></span></h4><ul><li>The Seer Proteograph ONE workflow combined with Orbitrap Astral Zoom mass spectrometer identified &gt;10,800 protein groups using ultradeep profiling, compared to &gt;8,200 with the high-throughput method—demonstrating scalable, reproducible plasma proteomics with clear detection of biological differences for biomarker discovery.&nbsp;</li><li>The Protoeograph ONE workflow combined with the Orbitrap Astral Zoom Mass Spectrometer captures exceptional dynamic range of 7-8 orders of magnitude in plasma proteome&nbsp;</li><li>&gt;1,000 differentially abundant proteins detected with biologically relevant dysregulated pathways such as immune signaling or tissue remodeling underscores the complex biology of lung cancer&nbsp;</li><li>Identification of FDA markers as differentially expressed showcases the workflow’s strength for capturing biologically relevant plasma proteins</li></ul><h3><strong>4. Waters Corporation: Improving Throughput and Analytical Greenness in Pharmaceutical Discovery Using Ultrashort (2.1 x 10 mm) HPLC Columns</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009074_en_406ea811f9.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>Benefits&nbsp;</strong></h5><ul><li>Up to 60% decrease in analysis time using the ultrashort (2.1 x 10 mm) column</li><li>Lower AMGS metric values indicating improvements in analytical method greenness</li></ul><p>Drug discovery is a fast-paced, high-throughput environment where chemists screen large numbers of samples to determine if a suitable compound has been created. Supporting these efforts from an analytical standpoint using liquid chromatography (LC) or liquid chromatography-mass spectrometry (LC-MS) can present challenges. For many discovery workflows, hundreds if not thousands of samples are analyzed for the determination of drug concentrations in biological matrices, for structural confirmation or for an assessment of purity. Analytically speaking, this means that the number of samples that may be analyzed per unit time, or throughput, is valued more highly than is achieving baseline separation of all components. To maximize throughput, rapid (“ballistic”) gradients can be employed along with short analytical columns.1 Ballistic gradients are designed to run at the highest flow rate possible while using the steepest gradient slope, in terms of percent solvent per column volume (%/VC).2 This allows for the fastest elution off the column possible. Shorter columns are used not only to limit the pressure generated by the column, thereby allowing faster flow rates, but also to reduce the analysis time.&nbsp;</p><p>In this application note, the use of a 2.1 x 10 mm 2.5 µm XSelect™ HSS T3 Column is examined compared to 2.1 x 30 mm and 2.1 x 50 mm columns packed with the same stationary phase. These three columns were used to analyze a full 96-well QuanRecovery™ Plate to simulate the output of a drug discovery environment where multiple samples need to be run as fast as possible. Prior to sample analysis, instrument methods were created to increase throughput by limiting the inter-injection delay. The inter-injection delay time was calculated and recorded. The total analysis time for each column configuration was determined and compared, along with the AMGS. While the loss of efficiency in using a 10 mm column was expected, the shorter column configuration achieved adequate results for a single component sample. Coupling this column with mass spectrometry for peak identification would be sufficient for high-throughput discovery screening where separation quality is not the most important attribute of the analysis, but rather speed is of the highest value.3</p><h4><strong>Experimental</strong></h4><h5><strong>Reversed Phase LC Conditions&nbsp;</strong></h5><ul><li><strong>LC system: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY™ Premier</strong></a> Binary Solvent Manager with Column Manager, TUV Detector, and<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/554"><strong> Xevo™ TQ Absolute Mass Spectrometer</strong></a></li><li><strong>Columns:&nbsp;</strong><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1864"><strong>XSelect HSS T3</strong></a>, 2.1 x 50 mm, 2.5 µm (p/n: 186006149)&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1864"><strong>XSelect HSS T3</strong></a>, 2.1 x 30 mm, 2.5 µm (p/n: 186006148)&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1864"><strong>XSelect HSS T3</strong></a>, 2.1 x 10 mm, 2.5 µm (p/n: 186011466)</li></ul></li><li><strong>Chromatography software:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/635"><strong>MassLynx™ V4.1 Software</strong></a></li></ul><h4><strong>Results and Discussion&nbsp;</strong></h4><h5><strong>Instrument Considerations&nbsp;</strong></h5><p>Prior to sample analysis, the system being used was considered. For Waters™ LC systems, there are a few parameters in the inlet method that can be adjusted to speed up the time between injections, or inter-injection delay. This delay comes from the sequence of steps that the system takes to draw the sample and inject it into the flow path of the LC. The parameters that need adjustment are all located in the sample manager panel of the instrument method or inlet method. Figure 1 shows screenshots of the sample manager panel and where the mentioned parameters are located.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>The use of high-throughput LC separations in pharmaceutical discovery allows new lead compounds to be selected quickly and efficiently. This may be achieved using short columns with ballistic gradients. To support these activities 2.1 x 10 mm columns were developed and used to analyze a full 96-well plate of samples. Comparing the results obtained on the 10 mm column to those produced using 30 and 50 mm columns showed a 57–146% higher throughput. Additionally, the use of the 10 mm column was determined to be substantially “greener” as measured by the analytical method greenness scores, with decreases of 40 and 68% relative to 30 and 50 mm length columns.</p>

News from LabRulezLCMS Library - Week 50, 2025

News from LabRulezLCMS Library - Week 20, 2026

News from LabRulezLCMS Library - Week 21, 2026

Article

Product

Events

Webinars

Application

Academy

Video

Poster

Scientists

Plastics

Environment

Food

Water

Health

Presentation

Scientific article

Interview

Toxicology

Popularization

Science and research

Software

Covid-19

Career

Laboratories

Various

Zaměření

Type of News

Focus

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

News from LabRulezLCMS Library - Week 21, 2026

News from LabRulezLCMS Library - Week 20, 2026

News from LabRulezLCMS Library - Week 50, 2025

News from LabRulezLCMS Library - Week 48, 2025

News from LabRulezLCMS Library - Week 43, 2025

News from LabRulezLCMS Library - Week 41, 2025

News from LabRulezLCMS Library - Week 40, 2025

News from LabRulezLCMS Library - Week 32, 2025

News from LabRulezLCMS Library - Week 30, 2025

News from LabRulezLCMS Library - Week 27, 2025

Upcoming events

Waters ASMS Users Meeting 2026

SciY at ASMS 2026

KNAUER at ASMS 2026

Webinars

Data handling and DMPK analysis with confidence

Reliable quantitation of GLP‑1 analogues in bioanalysis and IP 2026 updates

Enhancing Next-Gen Drug Discovery with High-Performance Inert LC Solutions