<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 1st 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>posters by<strong> Shimadzu </strong>and <strong>Waters Corporation </strong>and<strong> </strong>other document by<strong> Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies: PFAS Analysis in Human Plasma Using the Agilent Ultivo Triple Quadrupole LC/MS&nbsp;</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_ultivo_tq_lcms_5994_8487en_agilent_2968eb7f88.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Perfluoroalkyl and polyfluoroalkyl substances (PFAS) are a group of synthetic compounds that have been widely used in various industrial and consumer applications, including cosmetics and personal care products. Due to their widespread use, persistence in the environment, and known bioaccumulation with adverse effects, PFAS are a significant concern for human health. For example, PFAS have been linked to several adverse health effects, including cardiometabolic diseases,<sup>1</sup> reproductive effects,<sup>2</sup> and increased risk of certain cancers.<sup>3</sup> PFAS exposure has been shown to lead to alterations in lipid and energy metabolism, contributing to metabolic dysfunction.<sup>4,5</sup> It is also known that PFAS accumulate in liver and other tissues, contributing to age‑related morbidities.<sup>6</sup> To increase the understanding the molecular basis of these effects, analysis of PFAS in blood plasma has been combined with lipidomics to identify the lipid biomarkers associated with metabolic risks.<sup>7</sup> Further, the PFAS concentrations in serum have also been shown to differ by gender<sup>7,8 </sup>and ethnicity.<sup>9</sup> Considering these and other findings, monitoring PFAS levels in plasma is important to understand their health impacts and develop strategies for their mitigation. This application note validates an LC/MS/MS method for targeted quantification of fourteen PFAS in plasma using the Agilent Ultivo Triple Quadrupole (TQ) LC/MS. For the method presented, the Ultivo LC/TQ offers performances on par with mid- to high-end TQ systems in a much smaller footprint. The protein-precipitation-based sample preparation method is fast and effective for plasma samples. Method performance in terms of sensitivity, linearity, carryover, accuracy, and precision are described. Stability of targeted PFAS in quality control (QC) samples and analysis of real human plasma samples are also discussed.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation and LC/MS/MS method&nbsp;</strong></h5><p>Chromatographic conditions were optimized for analyte separation and retention time for each of the PFAS as determined by analyzing the labeled and non-labeled standards. PFAS were separated by reversed-phase LC on an Agilent InfinityLab Poroshell 120 EC‑C18, 2.1 × 50&nbsp;mm, 2.7 μm (part number 699775-902) and detected in negative electrospray ionization (ESI) mode using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity%C2%A0II+LC"><strong>Agilent 1290 Infinity&nbsp;II LC</strong></a> system coupled with the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Ultivo+LC%2FTQ"><strong>Ultivo LC/TQ</strong></a>. The liquid chromatograph was equipped with a binary pump (part number G7120A), column compartment (part number G7116B), and Agilent 1290 Infinity II Multisampler (part&nbsp;number G7167B). For each experiment, 5 μL of extract was injected. The LC parameters are listed in Table 2. The Ultivo LC/TQ was operated in dynamic multiple reaction monitoring (dMRM) mode. The dMRM parameters and retention times were optimized by analyzing each unlabeled PFAS standard. The MS parameters are listed in Table&nbsp;3. The Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Acquisition+software"><strong>MassHunter Acquisition software</strong></a> dMRM parameters per PFAS are in Table 4. Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Quantitative+Analysis+software"><strong>MassHunter Quantitative Analysis software </strong></a>was used for data processing.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>The quantitative method for the analysis of 14 PFAS in human plasma samples that is presented here is simple and robust, uses relatively small plasma volumes, and relies on fast and effective protein precipitation, facilitating its large-scale application. The method's sensitivity, linearity, carryover, recovery, and precision make it scalable to population-based studies and biomonitoring. The compact, stackable Ultivo LC/TQ and MassHunter software, in combination with columns and consumables from Agilent Technologies, offer a fit-for-purpose, end-to-end solution to enable widespread adoption in both routine monitoring and research. The method has already been used in combination with plasma lipidomics to characterize the relationship of circulating PFAS and lipidomic profiles.7 These types of studies promise to reveal the molecular basis of the adverse effect of PFAS exposure on human health&nbsp;outcomes.</p><h3><strong>2. Shimadzu / ASMS: One System, Multiple Solutions: Analysis of PFAS &amp; Cyanotoxins in Water Adhering to EPA 537.1, 544, and 545&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_WP_134_197d4ffd22.pdf"><strong>Full PDF for download</strong></a></li><li>PFAS are persistent synthetic chemicals found in consumer and industrial products, while cyanotoxins are harmful substances produced by cyanobacteria in water bodies.&nbsp;</li><li>EPA Methods 537.1 and 533 are approved by EPA for PFAS analysis in drinking water; Methods 544 and 545 target cyanotoxins like microcystins, nodularin, cylindrospermopsin, and anatoxin-a.&nbsp;</li><li>A single Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-8060RX"><strong>LCMS-8060RX</strong></a> system with automatic method switching enables efficient, accurate analysis of PFAS and cyanotoxins, reducing equipment needs and turnaround time.</li></ul><h4><strong>2. Methods</strong></h4><p>Figure 1 illustrates the LC-MS system’s method-switching capability, enabling seamless transitions between EPA Methods 537.1, 544, and 545 on a single platform. For EPA Method 537.1 (PFAS analysis), the flow path includes the delay column to remove background PFAS. In contrast, for EPA Methods 544 and 545 (cyanotoxin analysis), the delay column is bypassed to prevent unnecessary contaminations, ensuring accurate results. This automation enhances workflow efficiency and analytical flexibility.&nbsp;</p><p>To prevent mobile phase contamination when switching between PFAS and cyanotoxin analysis, a simple five-minute rinse (the flow path indicated by the red lines in Figure 2) with the appropriate mobile phase is shown to be sufficient.</p><h4><strong>4. Conclusion</strong></h4><p>This study shows that PFAS and cyanotoxins can be accurately measured using one triple quadrupole mass spectrometer with automatic method switching. A quick five-minute rinse ensures clean transitions between methods, minimizing downtime and manual work. This streamlined setup reduces equipment costs, boosts efficiency, and supports high-throughput environmental testing, including rapid response to events like harmful algal blooms.&nbsp;</p><h3><strong>3. Thermo Fisher Scientific: Nestlé develops an </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/401"><strong>Orbitrap Exploris 480 mass spectrometer</strong></a><strong> method for wide-scope analysis of pesticides and natural toxins in foods</strong></h3><ul><li>Other document (Case study)</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/cs_003406_lsms_nestle_orbitrap_exploris_480_case_study_cs003406_na_en_790e517c7d.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Nestlé is committed to ensuring the highest standards of food quality and safety through rigorous research and innovation. Located in Lausanne, Switzerland, Nestlé Research plays a pivotal role in developing analytical methods for monitoring chemical contaminants in food products. These robust methodologies are implemented across Nestlé's global laboratory network to screen, identify, and ensure compliance with food safety standards. In response to the challenges posed by climate change, evolving regulations, and shifting consumer preferences, Nestlé Research has developed a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/421"><strong>QuEChERS</strong></a>-based liquid chromatography high-resolution mass spectrometry (LC-HRMS) workflow. This innovative approach allows for the simultaneous analysis of over 1,100 contaminants, including pesticide residues, mycotoxins, and plant toxins, across various food matrices such as cereals, fruits, and vegetables. The method's sensitivity and low quantification limits ensure compliance with regulatory standards while facilitating the exploration of additional compounds to preemptively address future food safety risks.</p><h4><strong>Technology selection&nbsp;</strong></h4><p>Next, Nestlé Research scientists aimed to identify the most suitable technology to address the challenges associated with broad-scope contaminant analysis. The versatility and high selectivity of LC-HRMS for screening a broad range of compounds offered a solution. Theoretically, in full-scan mode, HRMS instruments can monitor an unlimited number of molecules simultaneously, opening up avenues for continuous extension of the method’s scope. The high-quality, high-resolution accuratemass (HRAM) data provided by the Thermo Scientific™ Orbitrap™ mass analyzer can help differentiate between compounds with similar masses and isobaric interferences from coextracted matrix components, reducing the chance of false positives. Highresolution mass spectrometry (HRMS) systems offer the capability to perform nontargeted or retrospective analyses by leveraging existing data and potentially identify novel contaminants.&nbsp;</p><p>Due to its sensitivity and HRAM data quality, the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/401"><strong>Thermo Scientific™ Orbitrap Exploris™ 480 mass spectrometer</strong></a> was evaluated and ultimately selected for workflow development. The developed method uses the full-scan MS/data-dependent MS2 (FS-ddMS2 ) acquisition mode, which combines a full scan with MS2 scans on the targets of interest measured in the full scan.&nbsp;</p><h4><strong>Necessary compromises&nbsp;</strong></h4><p>Though HRMS technology theoretically offers an unlimited scope of analysis, the true scope of analysis remains limited by the sample preparation method, chromatographic conditions, and MS ionization efficiency. According to Bessaire, “We needed to compromise on sample preparation and extraction, the LC method—the column and the gradient—and MS ionization mode because not all organic molecules can be analyzed using a single ionization mode. The scope of compounds that we dreamt about at the beginning was not the same as what we had at the end.”&nbsp;</p><p>With these compromises in mind, a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/421"><strong>QuEChERS-based sample preparation</strong></a> followed by dispersive solid-phase extraction (dSPE) cleanup was chosen due to its effectiveness for a wide range of sample types and analyte chemistries. LC method development was carried out on the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/744"><strong>Thermo Scientific™ Vanquish™ Horizon UPHLC system</strong></a>. A 22 minute LC run using acidic mobile phases on a 15 cm reversed phase (RP) C18 column with a smooth gradient slope was chosen to retain a broad range of chemicals with various polarities, while separating a maximum number of isomers and isobaric compounds within an acceptable run time. The generic sample preparation approach has advantages as Dr. Flavia Nagy (-Badoud), Scientist, Nestlé Research noted, “With the generic multiresidue method, we can reduce the use of solvents and work towards greener chemistry.”</p><h4><strong>In-house HRAM mass spectral library maximizes compound identification&nbsp;</strong></h4><p>To maximize the method’s capability to unequivocally confirm the presence or absence of numerous compounds from a single injection, the group developed an in-house HRAM mass spectral library populated in <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1760"><strong>Thermo Scientific™ mzVault™ software</strong></a>. Creating the library was time-consuming and involved injection and analysis of individual standard solutions for each compound. Dr. Nicolas Christinat, Scientist, Chemical Contaminants, Nestlé Research described the library creation process, “We relied on analytical standards for each molecule. That’s a lot of individual injections and we acquired multiple parameters for each, including different fragments at different collision energies, at different polarities, and for different adducts. All this information was stored in our mzVault spectral library, and we can use that information to build targeted methods that use the most relevant collision energy, most abundant ions, and the best polarity. Bessaire added, “Our internal mass spectral library was key to maximizing the identification capabilities of our method.”</p><h4><strong>Orbitrap Exploris 480 mass spectrometer essential capabilities&nbsp;</strong></h4><p>The Orbitrap Exploris 480 mass spectrometer platform provides capabilities essential to developing methods that provide reliable identification and quantification.&nbsp;</p><h5><strong>Sensitivity&nbsp;</strong></h5><p>First, the platform offers good sensitivity compared to other HRMS instruments. Aurélien Desmarchelier, Scientist, Nestlé Research explained, “We need state-of-the-art instruments when we develop new methods. We evaluated the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/402"><strong>Orbitrap Exploris 240 </strong></a>and Orbitrap Exploris 480 mass spectrometers. The Orbitrap Exploris 480 system’s data pointed to a bit more sensitivity and that’s why we selected and are recommending it to the laboratories that will be implementing the method, so we are aligned.” Dr. Nagy (-Badoud) added, “Contaminant analyses are always at low levels—parts per billion normally—so it is very important that we have a sensitive instrument. That’s mostly why in the past HRMS was not considered and contaminant analysis was done by triple quadrupole instruments with targeted approaches. One of the most important criteria was that we reached the required sensitivity.”</p><h3><strong>4. Waters Corporation / ASMS: Analysis of Amino Acids in Plant-Based Proteins and Pet Foods – Modification of AOAC 2018.06 to Fit for Novel Foods and Ingredients</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008914_e210a444bc.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The AOAC International Official Method 2018.06 specifies an analytical procedure for the analysis of amino acids (AA) in infant formula, adult nutrition and dairy products. This procedure is based on the pre-column derivatization with 6-aminoquinoline succinic carbamate (AQC) and reversed-phase ultra-performance liquid chromatography with UV detection.</p><p>When applied to pet foods, a limitation was observed in the target AA list. Specifically, <strong>hydroxyproline (HyPro)</strong>, common in pet foods, exhibited poor retention on the column, making it unmeasurable. HyPro is a marker for potential food adulteration using hydrolyzed animal products to artificially boost protein levels in plant-based proteins. It is also an indicator for animal-derived ingredients such as gelatin and collagen, which are critical in halal and kosher food testing.</p><p>Therefore, it is necessary to develop an analytical method capable of effectively separating and detecting HyPro alongside other amino acids.</p><h4><strong>Experimental</strong></h4><h5><strong>LC Conditions</strong></h5><ul><li><strong>System</strong>: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY Premier System</strong></a> (BSM) with PDA detector</li><li><strong>Detection</strong>: UV (260 nm)</li><li><strong>Tubing</strong>: 0.004 mm ID, 10.5 in (Waters p/n 430001784) between column and detector</li><li><strong>Software</strong>: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/627"><strong>Empower CDS</strong></a></li><li><strong>Columns</strong>:<ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1952"><strong>ACQUITY UPLC BEH C18</strong></a>, 1.7 μm, 2.1 mm × 150 mm (Waters p/n 186002353)</li><li>AccQ∙Tag Ultra C18, 1.7 μm, 2.1 mm × 150 mm (Waters p/n 186009954)</li></ul></li></ul><h4><strong>Conclusion</strong></h4><ul><li>Excellent separation resolution for all amino acids with high repeatability and intermediate reproducibility in RT</li><li>Amino acids in six pet foods and four common plant-based proteins successfully analyzed</li><li>Modified AOAC Method provides a reliable and practical solution for AA analysis in pet foods and plant-based proteins</li></ul>

News from LabRulezLCMS Library - Week 36, 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 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>

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