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!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application note by Agilent Technologies, posters by Shimadzu and Waters Corporation and other document by Thermo Fisher Scientific!<h3>1. Agilent Technologies: PFAS Analysis in Human Plasma Using the Agilent Ultivo Triple Quadrupole LC/MS&nbsp;</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">Full PDF for download</a></li></ul>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,1 reproductive effects,2 and increased risk of certain cancers.3 PFAS exposure has been shown to lead to alterations in lipid and energy metabolism, contributing to metabolic dysfunction.4,5 It is also known that PFAS accumulate in liver and other tissues, contributing to age‑related morbidities.6 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.7 Further, the PFAS concentrations in serum have also been shown to differ by gender7,8 and ethnicity.9 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.<h4>Experimental</h4><h5>Instrumentation and LC/MS/MS method&nbsp;</h5>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">Agilent 1290 Infinity&nbsp;II LC</a> system coupled with the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Ultivo+LC%2FTQ">Ultivo LC/TQ</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">MassHunter Acquisition software</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">MassHunter Quantitative Analysis software </a>was used for data processing.<h4>Conclusion&nbsp;</h4>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.<h3>2. Shimadzu / ASMS: One System, Multiple Solutions: Analysis of PFAS &amp; Cyanotoxins in Water Adhering to EPA 537.1, 544, and 545&nbsp;</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">Full PDF for download</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">LCMS-8060RX</a> system with automatic method switching enables efficient, accurate analysis of PFAS and cyanotoxins, reducing equipment needs and turnaround time.</li></ul><h4>2. Methods</h4>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;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.<h4>4. Conclusion</h4>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;<h3>3. Thermo Fisher Scientific: Nestlé develops an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/401">Orbitrap Exploris 480 mass spectrometer</a> method for wide-scope analysis of pesticides and natural toxins in foods</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">Full PDF for download</a></li></ul>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">QuEChERS</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.<h4>Technology selection&nbsp;</h4>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;Due to its sensitivity and HRAM data quality, the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/401">Thermo Scientific™ Orbitrap Exploris™ 480 mass spectrometer</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;<h4>Necessary compromises&nbsp;</h4>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;With these compromises in mind, a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/421">QuEChERS-based sample preparation</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">Thermo Scientific™ Vanquish™ Horizon UPHLC system</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.”<h4>In-house HRAM mass spectral library maximizes compound identification&nbsp;</h4>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">Thermo Scientific™ mzVault™ software</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.”<h4>Orbitrap Exploris 480 mass spectrometer essential capabilities&nbsp;</h4>The Orbitrap Exploris 480 mass spectrometer platform provides capabilities essential to developing methods that provide reliable identification and quantification.&nbsp;<h5>Sensitivity&nbsp;</h5>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">Orbitrap Exploris 240 </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.”<h3>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</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008914_e210a444bc.pdf">Full PDF for download</a></li></ul>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.When applied to pet foods, a limitation was observed in the target AA list. Specifically, hydroxyproline (HyPro), 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.Therefore, it is necessary to develop an analytical method capable of effectively separating and detecting HyPro alongside other amino acids.<h4>Experimental</h4><h5>LC Conditions</h5><ul><li>System: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191">ACQUITY Premier System</a> (BSM) with PDA detector</li><li>Detection: UV (260 nm)</li><li>Tubing: 0.004 mm ID, 10.5 in (Waters p/n 430001784) between column and detector</li><li>Software: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/627">Empower CDS</a></li><li>Columns:<ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1952">ACQUITY UPLC BEH C18</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>Conclusion</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

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 10th November 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies, Shimadzu and Waters Corporation and poster by Thermo Fisher Scientific!<h3>1. Agilent Technologies: Feed Injection at Elevated Pressure Using the Agilent 1290 Infinity III Hybrid Multisampler</h3>Optimization of a multipesticide method for the highest sensitivity through feed injection<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/te_feed_injection_multipesticide_1290_infinityiii_hybrid_5994_8478en_agilent_f070801ff2.pdf">Full PDF for download</a></li></ul>Modern analytical methods for the determination of pesticide residues are based on multipesticide methods capable of determining hundreds of pesticides in a sample in one analytical LC/MS/MS run. For chromatographic separation of these pesticides, modern separation columns are used. Their dimensions are typically 2.1 × 150 mm, filled with 1.9&nbsp;µm particle size material. This requires that the LC can work at high pressures up to 1300 bar. The Agilent 1290 Infinity III Hybrid Multisampler can operate within this pressure range. In addition, the Hybrid Multisampler can work in two different modes, the classic flow through mode and the Agilent Feed Injection mode. Feed Injection mode helps to prevent peak broadening and splitting effects as they can occur with the classic flow through mode for injection of samples in solvents with high elution strength and higher injection volumes.<h4>Experimental</h4><h5>Instrumentation</h5><ul><li>Agilent 1290 Infinity III High-Speed Pump (G7120A)&nbsp;</li><li>Agilent 1290 Infinity III Hybrid Multisampler (G7137B)&nbsp;</li><li>Agilent 1290 Infinity III MCT (G7116B)&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Ultivo+Triple+Quadrupole+LC%2FMS+">Agilent Ultivo Triple Quadrupole LC/MS </a>with Agilent Jet Stream source&nbsp;</li></ul><h5>Software&nbsp;</h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Acquisition+Software">Agilent MassHunter Acquisition Software</a> (v. 12.2)&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Qualitative+Analysis">Agilent MassHunter Qualitative Analysis Software</a> (v. 12.0)&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Quantitative+Analysis">Agilent MassHunter Quantitative Analysis Software</a> (v.&nbsp;12.1)&nbsp;</li></ul><h5>Column&nbsp;</h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=InfinityLab+Poroshell+120+Phenyl-Hexyl">Agilent InfinityLab Poroshell 120 Phenyl-Hexyl</a>, 2.1 × 150 mm, 1.9 µm (part number 699675-912)</li></ul><h4>Results and discussion&nbsp;</h4>Calibration curves for a multipesticide method were acquired to demonstrate the possible improvement of peak shape and the lower limits of quantification (LOQ) using Agilent Feed Injection mode in comparison to classical flow through injection mode. This method comprised approximately 120&nbsp;pesticide compounds measured by dynamic MRM. The separation was performed on a 150 mm length column. With the chosen solvents and flow rate, a pressure range above 1000&nbsp;bar was necessary. The calibration curves were acquired for concentrations down to 0.02 ppb (20 ppt), and each calibration point was measured three-fold. The concentrations of the calibration solutions were prepared by dilution using the strong-eluting solvent acetonitrile and injected directly by both injection modes with different injection volumes. An example chromatogram showing the elution pattern for the MRM transitions is displayed in Figure 1.<h4>Conclusion&nbsp;</h4>This technical overview demonstrates the use of the Agilent Feed Injection mode available with the Agilent 1290 Infinity III Hybrid Multisampler in comparison to the classical flow through injection mode for the analysis of pesticides by a multipesticide method. We demonstrated that the use of Agilent Feed Injection mode improves the obtained peak shape for injection of samples dissolved in high elution strength solvent compared to classical flow through mode. With the improved peak shape obtained by Feed Injection mode, signal to noise ratios were improved, resulting in higher sensitivity. Due to retained peak shape, no manual interaction for peak integration was necessary when using feed injection.<h3>2. Shimadzu: Automatic Optimization of Sample Solvent Composition for Achieving Sharp Peak Shapes</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00938_en_c0f4de1265.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>The automatic pretreatment function integrated into the autosampler enables efficient optimization of sample solvent composition, which can be automatically adjusted during analysis.</li><li>The desired composition of sample solvent can be easily specified via the LabSolutionsTM MD interface.</li></ul>In LC analysis, the composition of the sample solvent is critical for achieving proper peak shape. If the sample solvent is a stronger eluting solvent than the mobile phase, sample band condensation at the column inlet may be insufficient, leading to sample band broadening. For instance, increasing the organic solvent ratio in the sample solvent to dissolve low-polar compounds may deteriorate the peak shapes of early-eluting compounds in reversed-phase chromatography. Therefore, determining the optimal ratio of organic solvent in the sample solvent is essential. However, manually preparing multiple solvent compositions is extremely time-consuming. The automatic pretreatment function of the autosamplers (<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+X3">Nexera series</a>), in combination with the method development support <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LabSolutions+MD">software LabSolutions MD</a>, enables consecutive analyses using different sample solvent compositions without manual intervention. This allows evaluation of the effect of sample solvent composition on peak shape while significantly reducing the labor involved in optimization. In this study, we demonstrate the automated determination of the optimal sample solvent composition using metoclopramide, a small-molecule drug, as a model compound.<h4>Automatic Pretreatment Function</h4>The automatic pretreatment function integrated into the autosampler enables drawing and ejecting specified volumes of reagents and solvents from any vial, as well as mixing them within the needle. As an example, Fig. 1 illustrates the procedure for automatically adjusting the water-to-methanol ratio in the sample solvent using this function. The autosamplers (Nexera series) supports up to three rinsing solvents via the multi-rinse function, and in this procedure, methanol and water were supplied from these rinsing lines. By modifying the "methanol eject volume" (2) and “water eject volume” (3) in Fig. 1, sample solvents with desired methanol-to-water ratios can be automatically prepared. In addition, adjusting the “sample drawing volume” (1) allows for not only changing the sample solvent composition but also diluting the sample solution to a specified concentration.<h4>Analytical Conditions and Target Compounds</h4>A 1000 mg/L solution of metoclopramide, a small-molecule drug, was prepared in 100% methanol as a model sample. The water content in the sample solvent was then varied from 0% to 90% in 10% increments (A 10-fold dilution was applied during automatic sample solvent preparation), and its effect on peak shape was evaluated under the analytical conditions shown in Table 1. By simply specifying the desired water content on the LabSolutions MD interface (red frame in Fig. 2), the autosampler’s automatic pretreatment function adjusts the sample solvent composition during consecutive analyses. This eliminates the need for manual preparation of multiple solvent mixtures, significantly reducing the workload involved in optimizing sample solvent composition for ideal peak shapes.<h4>Conclusion</h4>Optimizing the composition of the sample solvent is essential for achieving appropriate peak shapes. However, manual preparation of multiple solvent compositions is time-consuming. The automatic pretreatment function of the autosampler, in combination with LabSolutions MD, enables consecutive analyses with automatic variation of the sample solvent composition. This significantly reduces the effort required for optimization. Since the optimal sample solvent composition depends on both the physicochemical properties of the analyte and the mobile phase conditions, optimization is necessary for each sample. These tasks, however, can be greatly reduced by utilizing the automatic pretreatment function.<h3>3. Thermo Fisher Scientific: Improving selectivity and sensitivity of lipid mediator analyses by coupling nano-flow chromatography with the Stellar mass spectrometer</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_improving_selectivity_sensitivity_lipid_mediator_analyses_po_en_c38bc37825.pdf">Full PDF for download</a></li></ul>Lipid mediators play crucial roles in regulating inflammation and maintaining tissue homeostasis. However, their quantification in biological samples is difficult due to low concentrations (ppt–ppb range), chemical instability, and structural similarity. Conventional LC-MS/MS methods using high-flow UHPLC and triple quadrupole mass spectrometers require extensive optimization of SRM transitions for each analyte. This study introduces a nano-flow LC-MS workflow combining the Thermo Scientific Vanquish Neo UHPLC system with the Thermo Scientific Stellar mass spectrometer, aiming to improve analytical sensitivity and selectivity while reducing solvent and sample consumption.<h4>Experimental</h4>Lipid mediator standards (from Cayman Chemical) were analyzed using two chromatographic configurations: a nano-flow method (500 nL/min) with the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398">Vanquish Neo UHPLC</a> and a high-flow method (300 µL/min) using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/744">Vanquish Horizon UHPLC</a>. Both setups were coupled either to the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1149">Stellar MS</a> or the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/404">TSQ Altis Plus triple quadrupole MS</a>. The Stellar instrument features a dual-pressure linear ion trap and ion routing multipole, enabling both HCD (higher-energy collisional dissociation) and CID (collision-induced dissociation) fragmentation. Parallel reaction monitoring (PRM) was employed instead of SRM, allowing simultaneous detection of multiple transitions. Data were processed using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/77">Thermo Scientific TraceFinder</a> software with internal standards and calibration curves ranging from 0.0001 ppb to 100 ppb.<h4>Results</h4>The nano-flow Stellar method achieved superior sensitivity and selectivity compared with the high-flow methods on both Stellar and TSQ Altis Plus systems. Limits of quantitation (LOQ) reached the low-ppt range, while maintaining fast analysis times (&lt; 30 min) and requiring less than 20 µL of solvent per sample. Chromatograms of key eicosanoids such as 15(S)-HETE, 12(S)-HETE, and 5(S)-HETE demonstrated higher signal intensity and improved peak shapes under nano-flow conditions. Calibration curve reproducibility and scan density (&gt; 10 scans per peak) confirmed reliable quantitative performance.<h4>Conclusion</h4>Coupling nano-flow chromatography with the Stellar mass spectrometer provides a powerful workflow for targeted lipid mediator analysis, significantly enhancing both selectivity and sensitivity compared with conventional high-flow LC-MS/MS. The system’s PRM capability, dual-fragmentation flexibility, and low-volume solvent use make it a robust and cost-effective solution for biological and clinical lipidomics, capable of quantifying trace-level lipid mediators efficiently and reproducibly.<h3>4. Waters Corporation: Investigating Drug Metabolism of Methapyrilene Within a Rat Model Using a Data Dependent Acquisition Workflow with the Xevo MRT Mass Spectrometer</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009001_en_c11ab3b6b7.pdf">Full PDF for download</a></li></ul><h5>Benefits&nbsp;</h5><ul><li>Demonstration of the Waters™ Xevo™ MRT Mass Spectrometer (MS) workflow for the analysis of urine extracts from a drug dosed study, involving methapyrilene.</li><li>Data dependent acquisition (DDA) has been used for data collection, providing highly informative fragmentation data to confidently identify drug metabolites of interest.</li><li>Combining a DDA approach with high-throughput chromatography is shown to consistently yield high quality spectra, providing highly confident compound identifications.</li><li>A seamless workflow allowing drug metabolites to be confidently identified is demonstrated with the UNIFI™ Application within the waters_connect™ Software Platform</li></ul>The introduction of the Xevo MRT Mass Spectrometer allows for comprehensive drug metabolite identification (Met ID) at high acquisition speed. Using urine samples collected over a time course of six days, the excellent mass accuracy, high mass resolution, and sensitivity are highlighted, which can be achieved for drug metabolism studies. DDA provides highly specific MS/MS information, which assists with structural elucidation. The speed at which DDA data can be acquired with the Xevo MRT Mass Spectrometer can be as fast as 50 and 100 Hz, MS, and MS/MS respectively. Combined with fast chromatographic methods, this fast data acquisition rate allows for highly informative, confident data in a high-throughput fashion<h4>Experimental</h4>LC-MS Data Acquisition LC-MS data were collected using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191">ACQUITY™ Premier UPLC™ System</a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1148">Xevo MRT Mass Spectrometer</a>. The reversed-phase (RP) chromatographic separation consisted of a 5.0 minute method (injection to injection) using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1966">CORTECS™ C18</a>, 1.6 µm, 2.1 x 50 mm analytical Column (p/n: 186007114). The LC solvents were comprised of mobile phase A (0.1% formic acid containing 1 mMol ammonium formate) and mobile phase B (95:5 ACN:Water (v/v), 0.1% formic acid, 1 mMol ammonium formate) being ramped from 50% to 99% over 5 minutes using a flow rate of 0.6 mL/minute. The gradient started from 0.1% to 15% (mobile phase B) over 1.5 minutes, 50% at 3 minutes and 99% at 4 minutes. The solvent composition was held at 99% (mobile phase B) for 0.5 minutes and re-equilibration at initial conditions by 5 minutes, ready for the subsequent injection.&nbsp;The Xevo MRT Mass Spectrometer was configured with the source settings as outlined in Table 1. MS data were collected using DDA mode of operation, which consisted of scan rates of 20 Hz (MS) and 50 Hz (MS/MS). The number of components selected for MS/MS were eight with a dynamic exclude applied of 10 mDa with a 10 second retention time tolerance.<h4>Data Processing&nbsp;</h4>The acquired data were processed using the UNIFI Application within the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1544">waters_connect Software Platform</a>. Data were peak picked and screened against a compound database containing MP metabolites and their associated fragments. A mass tolerance of 1 ppm for both MS and MS/MS were applied.<h4>Conclusion&nbsp;</h4>LC-MS analysis of urine collected over a time course following administration of the drug methapyrilene, has been demonstrated using a DDA approach with the Xevo MRT Mass Spectrometer. MP undergoes complex biotransformation to provide a variety of metabolites. Utilizing a DDA workflow provides detailed, clean fragment ion spectra for confident structural elucidation. The additional benefit of sub ppm mass accuracy provides definitive identification(s). Integrating fast chromatography allows for high-throughput analyses while maintaining high resolution and mass accuracy.

News from LabRulezLCMS Library - Week 46, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 2nd February 2026? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies and Waters Corporation, technical note by Shimadzu and poster by Thermo Fisher Scientific / MSACL!<h3>1. Agilent Technologies: Quantitative Separation of THC Isomers and Metabolites from Whole Blood</h3>Using Agilent Captiva Enhanced Matrix Removal (EMR) cartridges and LC/MS/MS<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_thc_isomers_captiva_emr_lctq_5994_8664en_agilent_5eb50dc6f9.pdf">Full PDF for download</a></li></ul>THC isomers (Δ8- and Δ9-THC, in particular) are psychoactive compounds of increasing interest in forensic toxicology, where accurate identification and quantification of these individual isomers and their respective metabolites are essential for legal and clinical assessments. However, an analytical challenge derives from their structural or empirical similarity and the presence of potential isobaric interferences.&nbsp;Isobaric compounds are molecules that are empirically identical, share the same nominal mass, but differ in structure. In the context of THC analysis, CBD and exo-THC are notable isobaric interferences. These compounds can coelute or produce overlapping mass spectral signals, complicating the interpretation of results. CBD, a nonpsychoactive cannabinoid, shares an identical molecular weight and similar fragmentation pattern with THC isomers, making it difficult to distinguish using conventional mass spectrometry alone. Exo-THC, another structural analog, further adds to the complexity for the same reasons.&nbsp;Without adequate chromatographic separation, these isobaric interferences can lead to false positives or inaccurate quantitation. This is particularly problematic in forensic settings, where precise identification of psychoactive substances is critical. Therefore, a robust analytical method that can resolve these compounds and potential interferents is&nbsp;desirable.&nbsp;This study introduces a workflow that combines enhanced matrix removal (EMR) with LC/MS/MS to achieve baseline separation of THC isomers and their metabolites from the isobaric interferences that were examined within the scope of this application note. The method enables confident separation, identification, and quantification in a single 15-minute analysis.<h4>Experimental</h4><h5>Chromatographic separation and LC/MS/MS detection&nbsp;</h5>This procedure can be accomplished using different instrument configurations. Chromatographic separation was verified using both an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1260+Infinity+II+LC">Agilent 1260 Infinity II LC</a> and an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity+II+LC">Agilent&nbsp;1290 Infinity II LC</a>. Analyte detection and quantitation were performed via both an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6475">Agilent 6475 triple quadrupole LC/MS</a> and an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Ultivo">Agilent&nbsp;Ultivo triple quadrupole LC/MS</a>. Method&nbsp;parameters are detailed in Tables 1 and 2. Detailed MRM transition settings are outlined in Appendix A.<h4>Conclusion&nbsp;</h4>This study presents an effective, integrated workflow for the separation and quantification of THC isomers and metabolites in whole blood. Agilent&nbsp;Captiva EMR–Lipid cartridges removed sufficient matrix interferences to enable clean extraction and high analyte recovery. Chromatographic separation using an Agilent InfinityLab Poroshell 120 PFP column provided reliable resolution of isobaric compounds, including CBD and exo-THC. Coupled with Agilent LC/MS/MS systems featuring Agilent Jet Stream ionization technology, the method delivered consistent sensitivity and selectivity across a complex panel of analytes. Together, this methodology offers the basis of a streamlined workflow for the separation of Δ8-, Δ9-, and Δ10-THC isomers and their respective hydroxy and carboxy metabolites and potential interferents from whole blood.<h3>2. Shimadzu: Optimization of Supercritical Fluid Extraction Parameters for Vitamins D2, D3, and K1 from Pharmaceutical Preparations</h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c190_e333_6198eb84b9.pdf">Full PDF for download</a></li></ul>Vitamins are organic compounds, essential in small amount, crucial for the normal functioning of the human body, facilitating numerous enzymatic and metabolic functions[1]. Since the human organism cannot produce vitamins, the diet represents the main route of ingestion of these compounds. As consumer awareness grows, reliable information about the vitamin content in foods is becoming a critical issue. However, considering that vitamins could be losses during food processing and storage, the readyto-use multi-vitamin pharmaceutical preparations are becoming widely employed among consumers. These facts, together with the introduction of labelling regulations, introduced the need for ensure the quality control of these types of formulation.<h4>2. Experimental</h4><h5>2.3 Instrumentation</h5>The supercritical fluid extraction (SFE) was carried out by using a SFE pretreatment system (<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+UC">Shimadzu Nexera UC</a>) equipped with: a CBM-40 controller, an SFE-30A module, an LC-30ADSF CO2 pump, an LC-40D XR modifier pump, an LC-40D make-up pump, an SFC-30A back pressure regulator, a DGU-40 on-line degasser, an FRC-40 fraction collector. A combination of static and dynamic extraction was employed (Figure 2).<h4>Conclusion&nbsp;</h4>Considering the obtained results, the vitamins extraction revealed as strictly matrix dependent, according to the formulation excipients. Therefore, detailed study needs to be performed to better understand the vitamin formulation.<h3>3. Thermo Fisher Scientific / MSACL: Simultaneous quantitation and discovery (SQUAD) of fecal bile acids and their conjugates in children with autism spectrum disorder (ASD)</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_squad_fecal_bile_acids_children_asd_po_en_af787058d3.pdf">Full PDF for download</a></li></ul>This study presents a Simultaneous Quantitation and Discovery (SQUAD) metabolomics workflow applied to the analysis of fecal bile acids and their microbial conjugates in children with Autism Spectrum Disorder (ASD) undergoing microbiota transfer therapy (MTT). Bile acids play a key role in lipid metabolism and gut–brain signaling, and alterations in gut microbiota composition in ASD have been linked to disrupted bile acid metabolism. The SQUAD approach was designed to address the need for both targeted quantification of known bile acids and untargeted discovery of novel metabolic features within a single LC–MS injection.The workflow integrates reversed-phase liquid chromatography with advanced mass spectrometry using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/748">Thermo Scientific Orbitrap Ascend Tribrid mass spectrometer</a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/744">Thermo Scientific Vanquish Horizon UHPLC system</a>. Quantitative analysis was performed using parallel reaction monitoring (PRM) in the linear ion trap, while high-resolution MS¹ scanning in the Orbitrap enabled confident metabolite annotation. The Tribrid architecture—combining a quadrupole, linear ion trap, and Orbitrap—allowed high selectivity and sensitivity, including MSⁿ capabilities for resolving co-eluting structural isomers such as leucine- and isoleucine-conjugated bile acids.Using calibrated bile acid standards, the method achieved absolute quantitation across six orders of magnitude, with limits of quantitation below 1.8 femtomoles on column. The SQUAD workflow was applied to fecal samples collected before and after MTT, revealing distinct shifts in bile acid and lipid-related metabolite profiles following treatment. Multivariate analysis, including principal component analysis (PCA), demonstrated clear separation between pre- and post-treatment samples in the MTT group, while no comparable changes were observed in placebo controls.Overall, the results demonstrate that SQUAD metabolomics enables high-throughput, highly sensitive, and information-rich analysis by combining quantitative rigor with deep metabolic coverage in a single experiment. This integrated LC–MS workflow provides valuable insight into the biochemical effects of microbiome modulation in ASD and highlights the power of Orbitrap Tribrid–based metabolomics for studying complex host–microbiome interactions in clinical research.<h3>4. Waters Corporation: Analysis of Organic Carbonates in Lithium- Ion Battery Electrolyte by High-Performance Liquid Chromatography (HPLC) with Mass Detection (MS)</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009211_en_46cbebda90.pdf">Full PDF for download</a></li></ul><h5>Benefits&nbsp;</h5><ul><li>Sensitive method for low-level detection and quantification of carbonate solvents (0.05–1 ppm) and carbonate-based aging products (0.00075–0.0025 ppm) in lithium-ion battery electrolyte solutions using the ACQUITY QDa II Mass Detector with SIR acquisition mode.</li><li>Robust chromatographic separation using the XSelect Premier HSS PFP Column under 7 minutes analysis time, operated under reversed-phase conditions.</li></ul>The electrolyte is one of the main components in the lithium-ion battery.1,2 It is a conductive solution that transports lithium ions from the cathode to the anode during the charging process. During discharge, the lithium ions flow from the anode to the cathode. The electrolyte solution is composed of lithium salt dissolved in a mixture of organic solvents.1,2 The organic solvents are typically a mixture of cyclic and linear carbonates, including EC, PC, DMC, EMC, and DEC.2 Lithium hexafluorophosphate (LiPF₆) is commonly used as the conducting lithium salt,2 providing the necessary ionic conductivity for efficient battery operation.&nbsp;The LiPF6 salt in carbonate-based systems can exhibit chemical and thermal instability, which can impact the performance of the lithium-ion batteries.2-4 Electrolyte solutions can also degrade, forming aging products including DMDOHC and DEDOHC.2 Various techniques are employed to investigate quality and properties of the electrolytes. Techniques such as scanning calorimetry (DSC) and thermogravimetric analysis (TGA) offer a comprehensive analysis of an electrolyte’s thermal properties, while rheology measures viscosity of the conductivity solutions.1 Additionally, chromatographic methods are used to measure the quantity of carbonate solvents in electrolyte solutions.2-4 Gas chromatography mass spectrometry (GC/MS) and liquid chromatography mass spectrometry (LC/MS) are common techniques used to investigate carbonate-based electrolytes.3&nbsp;In this application note, an HPLC method with mass detection was developed for the analysis of five common carbonate solvents and two carbonate-based aging products (Table 1). The method employed an ACQUITY QDa II Mass Detector coupled with an Arc Premier System. Method performance characteristics including limit of detection (LOD), limit of quantification (LOQ), linearity and system suitability were demonstrated. Additionally, the developed method was applied for the analysis of LiPF6-based electrolyte solution.<h4>Experimental</h4><h5>Method Conditions&nbsp;</h5><ul><li>System: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/306">Arc Premier System</a>, Column Manager with active pre-heating, PDA and the ACQUITY QDa II Mass Detector&nbsp;</li><li>Column: XSelect Premier HSS PFP Column, 2.5 µm, 4.6 mm x 100 mm (Waters, p/n: 186010051)</li><li>MS system: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1543">ACQUITY QDa II Mass Detector</a></li></ul><h5>Data Management&nbsp;</h5><ul><li>Chromatography data software (CDS): <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/627">Empower™ 3.6.1</a></li></ul><h4>Results and Discussion&nbsp;</h4>Chromatographic columns with a wide range of selectivity were explored during this study to ensure separation between carbonate solvents and carbonate-based aging products. The selected columns (XSelect Premier CSH™ C18, XSelect Premier CSH Phenyl Hexyl, XSelect Premier HSS T3, XSelect Premier HSS PFP) were tested with acetonitrile and methanol solvents. The study showed that XSelect Premier HSS PFP Column with methanol provided the best retentivity and separation for all analytes (Figure 1). The method successfully separated carbonate solutions and carbonate-based aging products in less than a 7-minute gradient time. The MS total ion chromatogram (TIC) data was collected across the mass range of 35–300 Da using electrospray ionization in positive (ESI+) mode (Figure 1A). The mass spectral data facilitated quick and accurate identification of the components. The carbonate solvents formed [M + H]+ molecular ions, while the selected aging products formed sodium adducts, [M + Na]+. These ions were measured using a selected ion recording (SIR) acquisition mode, which determines intensity for a single ion of interest (Figure 1B).<h4>Conclusion&nbsp;</h4>A sensitive and reliable HPLC-MS method using the Arc Premier System coupled with the ACQUITY QDa II Mass Detector was developed for the analysis of carbonate solvents and carbonate-based aging products in lithium-ion battery electrolyte. This reversed-phase LC method successfully separated all five carbonate solvents (EC, PC, DMC, EMC, DEC) and two aging products (DMDOHC/DEDOHC) on an XSelect Premier HSS PFP Column. Low-level quantification limits were achieved using SIR acquisition mode ranging from 0.05 to 1 ppm and 0.00075–0.0025 ppm for carbonate solvents and aging products, respectively. The method was demonstrated to be applicable for the analysis of lithium-ion battery electrolyte.

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News from LabRulezLCMS Library - Week 06, 2026

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