<p><strong>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!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies,</strong> <strong>Shimadzu </strong>and<strong> Waters Corporation</strong> and poster by <strong>Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies: Feed Injection at Elevated Pressure Using the Agilent 1290 Infinity III Hybrid Multisampler</strong></h3><p><strong>Optimization of a multipesticide method for the highest sensitivity through feed injection</strong></p><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"><strong>Full PDF for download</strong></a></li></ul><p>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.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation</strong></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+"><strong>Agilent Ultivo Triple Quadrupole LC/MS </strong></a>with Agilent Jet Stream source&nbsp;</li></ul><h5><strong>Software&nbsp;</strong></h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Acquisition+Software"><strong>Agilent MassHunter Acquisition Software</strong></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"><strong>Agilent MassHunter Qualitative Analysis Software</strong></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"><strong>Agilent MassHunter Quantitative Analysis Software</strong></a> (v.&nbsp;12.1)&nbsp;</li></ul><h5><strong>Column&nbsp;</strong></h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=InfinityLab+Poroshell+120+Phenyl-Hexyl"><strong>Agilent InfinityLab Poroshell 120 Phenyl-Hexyl</strong></a>, 2.1 × 150 mm, 1.9 µm (part number 699675-912)</li></ul><h4><strong>Results and discussion&nbsp;</strong></h4><p>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.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>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.</p><h3><strong>2. Shimadzu: Automatic Optimization of Sample Solvent Composition for Achieving Sharp Peak Shapes</strong></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"><strong>Full PDF for download</strong></a></li></ul><h4><strong>User Benefits</strong></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><p>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"><strong>Nexera series</strong></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"><strong>software LabSolutions MD</strong></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.</p><h4><strong>Automatic Pretreatment Function</strong></h4><p>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.</p><h4><strong>Analytical Conditions and Target Compounds</strong></h4><p>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.</p><h4><strong>Conclusion</strong></h4><p>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.</p><h3><strong>3. Thermo Fisher Scientific: Improving selectivity and sensitivity of lipid mediator analyses by coupling nano-flow chromatography with the Stellar mass spectrometer</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_improving_selectivity_sensitivity_lipid_mediator_analyses_po_en_c38bc37825.pdf"><strong>Full PDF for download</strong></a></li></ul><p>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 <strong>nano-flow LC-MS workflow</strong> combining the <strong>Thermo Scientific Vanquish Neo UHPLC system</strong> with the <strong>Thermo Scientific Stellar mass spectrometer</strong>, aiming to improve analytical sensitivity and selectivity while reducing solvent and sample consumption.</p><h4><strong>Experimental</strong></h4><p>Lipid mediator standards (from Cayman Chemical) were analyzed using two chromatographic configurations: a <strong>nano-flow method</strong> (500 nL/min) with the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Vanquish Neo UHPLC</strong></a> and a <strong>high-flow method</strong> (300 µL/min) using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/744"><strong>Vanquish Horizon UHPLC</strong></a>. Both setups were coupled either to the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1149"><strong>Stellar MS</strong></a> or the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/404"><strong>TSQ Altis Plus triple quadrupole MS</strong></a>. The Stellar instrument features a <strong>dual-pressure linear ion trap</strong> and <strong>ion routing multipole</strong>, enabling both <strong>HCD (higher-energy collisional dissociation)</strong> and <strong>CID (collision-induced dissociation)</strong> 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"><strong>Thermo Scientific TraceFinder</strong></a> software with internal standards and calibration curves ranging from 0.0001 ppb to 100 ppb.</p><h4><strong>Results</strong></h4><p>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 <strong>low-ppt range</strong>, while maintaining fast analysis times (&lt; 30 min) and requiring less than 20 µL of solvent per sample. Chromatograms of key eicosanoids such as <strong>15(S)-HETE</strong>, <strong>12(S)-HETE</strong>, and <strong>5(S)-HETE</strong> 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.</p><h4><strong>Conclusion</strong></h4><p>Coupling <strong>nano-flow chromatography</strong> with the <strong>Stellar mass spectrometer</strong> 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 <strong>PRM capability</strong>, <strong>dual-fragmentation flexibility</strong>, and <strong>low-volume solvent use</strong> make it a robust and cost-effective solution for biological and clinical lipidomics, capable of quantifying trace-level lipid mediators efficiently and reproducibly.</p><h3><strong>4. Waters Corporation: Investigating Drug Metabolism of Methapyrilene Within a Rat Model Using a Data Dependent Acquisition Workflow with the Xevo MRT Mass Spectrometer</strong></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"><strong>Full PDF for download</strong></a></li></ul><h5><strong>Benefits&nbsp;</strong></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><p>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</p><h4><strong>Experimental</strong></h4><p>LC-MS Data Acquisition LC-MS data were collected using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY™ Premier UPLC™ System</strong></a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1148"><strong>Xevo MRT Mass Spectrometer</strong></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"><strong>CORTECS™ C18</strong></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;</p><p>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.</p><h4><strong>Data Processing&nbsp;</strong></h4><p>The acquired data were processed using the UNIFI Application within the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1544"><strong>waters_connect Software Platform</strong></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.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>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.</p>

News from LabRulezLCMS Library - Week 46, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 15th June 2026? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies, Shimadzu </strong>and<strong> Thermo Fisher Scientific, </strong>technical note by<strong> KNAUER </strong>and brochure by <strong>Waters Corporation!</strong></p><h3><strong>1. Agilent Technologies: Large-Volume Dilute-and-Shoot Analysis of PFAS in Drinking Water Using the Altura PFAS Column</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_analysis_pfas_drinking_water_altura_5994_9186en_agilent_a66334e5b0.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Per‑ and polyfluoroalkyl substances (PFAS) are synthetic fluorinated compounds valued for their oil‑ and water‑repellent properties, but their environmental persistence and mobility have driven the development of increasingly stringent regulations for drinking water monitoring. Existing dilute-and-shoot methods, such as EPA 8327 and ASTM D7979, were originally designed for screening PFAS in nonpotable water. These methods typically rely on 10 to 30&nbsp;µL injection volumes, setting practical quantitation limits appropriately 10 ng/L.<sup>1,2&nbsp;</sup></p><p>We present a large‑volume injection workflow that extends the capabilities of these methods toward trace PFAS quantitation in drinking water. Using the Agilent 6495D triple quadrupole LC/MS (LC/TQ) coupled with a 1290 Infinity II LC, we achieved injections of 200 µL of methanol‑diluted water on the Altura PFAS column without requiring SPE concentration. The Altura PFAS column maintained peak symmetry and retention stability under these injection conditions. This configuration enabled a working calibration range of 0.25 to 25 ng/L, extending the low-end sensitivity substantially relative to published dilute-and shoot methods.<sup>1,2&nbsp;</sup></p><p>This performance enhancement simplifies operations by removing labor‑intensive extraction steps, while maintaining sensitivity required for regulatory guidelines thereby supporting high‑throughput PFAS workflows suitable for routine drinking water analysis. The PFAS compounds analyzed were PFBS, HFPO-DA, PFHpA, PFHxA, PFHxS, PFOA, PFOS, PFNA, and PFDA. These compounds were selected due to their relevance to ongoing regulatory actions and proposed maximum contaminant level (MCL) considerations for drinking water.&nbsp;</p><p>Specific highlights of this experiment include:&nbsp;</p><ul><li>Minimized peak tailing and solvent effects with 200 µL injections water/methanol (1:1) injections.</li><li>Increased throughput by elimination of solid phase extraction (SPE).&nbsp;</li><li>Enhanced sensitivity of 6495D LC/TQ at low end (0.25&nbsp;ng/L) for the dilute-and-shoot method in drinking&nbsp;water.</li></ul><h4><strong>Experimental&nbsp;</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=+1290+Infinity+II"><strong>Agilent 1290 Infinity II LC</strong></a> coupled to <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6495D"><strong>Agilent 6495D LC/TQ system</strong></a> was utilized for the LC/MS/MS analysis. An Infinity&nbsp;II multisampler with an extended multidraw capillary tube (G7137-68307) was connected to the needle seat and injection valve with a union for large volume injection (200&nbsp;µL). The data were acquired with MassHunter acquisition software version 12.2. All LC/MS parameters are shown in Table 1 and 2. PFAS multiple reaction monitoring (MRM) transition methods were imported from the PFAS MRM database (G1736AA) while labelled homologues were optimized to obtain correct MRM transitions (Table 3).</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This study demonstrates a practical large‑volume dilute-and-shoot workflow for the determination of PFAS in drinking water using the Agilent 1290 Infinity II LC coupled to the 6495D triple quadrupole LC/MS, and Agilent Altura Poroshell PFAS column. With 200 µL water samples diluted in methanol can be injected directly, eliminating the need for SPE concentration and significantly reducing sample preparation time. This method exhibits good sensitivity, accuracy, and reproducibility. The Altura PFAS column maintained consistent peak performance and retention stability even at low sub‑ppt concentrations, supporting long‑term reliability for trace‑level PFAS monitoring. Overall, the findings highlight the method potential to support routine, high‑sensitivity PFAS monitoring in drinking water laboratories.</p><h3><strong>2. KNAUER: Size matters - How to perform narrow calibration using the ClarityChrom® GPC Extension</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/VTN_0049_knauer_size_matters_how_to_perform_narrow_calibration_using_the_claritychrom_gpc_extension_3cfdc7a45b.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Gel Permeation Chromatography (GPC), also known as Size Exclusion Chromatography (SEC), is a separation technique that separates molecules based on their hydrodynamic size rather than chemical interactions. In a GPC column, separation is based on the ability of molecules to access the pores of the stationary phase. Smaller molecules can penetrate these pores and therefore spend more time inside the column, resulting in a delayed elution. Larger molecules, on the other hand, cannot enter the pores and pass through the column more quickly, leading to earlier elution.&nbsp;</p><p>As a result, molecules are separated by size in solution, providing the basis for the determination of molecular weight and molecular weight distributions. Calibration is therefore a fundamental requirement for ensuring the accuracy and reliability of the results. The ClarityChrom® GPC Extension enables users to efficiently create and apply different calibration models for precise analysis. The workflow presented here focuses on narrow calibration using standards with defined molecular weights and low polydispersity (PD ≈ 1).</p><h4><strong>Material and Methods</strong></h4><ul><li><strong>Software&nbsp;</strong><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=503&amp;search=ClarityChrom"><strong>ClarityChrom</strong></a>® 10.1 - station single instrument license one time base</li><li>ClarityChrom® 10.1 - GPC license for GPC data processing &nbsp;</li></ul></li><li><strong>Pump: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2372"><strong>AZURA P 6.1L isocratic HPLC pump</strong></a> with 10 ml pump head for normal phase applications, stainless steel&nbsp;</li><li><strong>Degasser: </strong>Analytical 2 channel GPC degasser&nbsp;</li><li><strong>Autosampler:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2375"><strong>AZURA® AS 6.1L</strong></a>, analytical HPLC autosampler, 862 bar&nbsp;</li><li><strong>Detector:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2429"><strong>AZURA® RID 2.1L</strong></a>, analytical refractive index detector&nbsp;</li><li><strong>Thermostat: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2376"><strong>AZURA® CT 2.1</strong></a> ATC00 Capillaries Start-Up Kit with flexible, precut capillaries for analytical HPLC systems with 1/16" connections</li></ul><h4><strong>Conclusion</strong></h4><p>This technical note demonstrates how to successfully create and apply a narrow calibration using the ClarityChrom® GPC Extension. By following the outlined workflow, users can ensure reliable calibration and determination of molecular weight and molecular weight distributions. The described approach supports consistent and reproducible results, making it a valuable tool for routine GPC/SEC analysis. For further optimization and advanced applications, additional related technical and application notes can be consulted.</p><h3><strong>3. Shimadzu: UHPLC Method for Sensitive Automatic Analysis of Thirty-Seven D/L-Amino Acids and for Liquor Profiling</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_01169_en_2dab331398.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>Enables high-sensitivity simultaneous fast analysis of thirty-seven D/L-amino acids using simple operations.</li><li>Good reproducibility of analytical results can be achieved by keeping the derivatization reaction time constant.</li><li>Statistical analysis software enables easy multivariate analysis of multiple samples.</li></ul><p>Recent advances in analytical techniques have revealed the presence of D-amino acids in fermented foods and biological samples and clarified their role in the taste, preservation, and aroma of foods , and as potential disease biomarkers. Therefore, the demand for D/L separation of amino acids is increasing. Because D-amino acids are only present in trace amounts in fermented foods and biological systems, unlike L-amino acids, it is necessary to determine the concentration of each D-amino acid by separating them from the high concentrations of Lamino acids.&nbsp;</p><p>A comprehensive method for quantitating the thirty-seven D/Lamino acids was previously reported1), in which two chiral derivatizing reagents were employed to provide different diastereomers for each amino acid, with the instrument automatically switching between two separation methods to analyze each sample twice.&nbsp;</p><p>This article introduces an improved method that employs a single chiral derivatizing reagent to enable simultaneous analysis of D/L-amino acidsin a shorter time.</p><h4><strong>D/L-Amino Acid Analysis by UHPLC&nbsp;</strong></h4><p>In general, LC/MS or multi-dimensional LC is used to analyze D/L-amino acids by HPLC, because it is difficult to separate proteinogenic D/L-amino acids with a single separation mode. However, it is known that LC/MS is susceptible to matrix effects and less quantitative than HPLC. It is also known that the multidimensional LC method requires a long analysis time and very complicated HPLC setup. Therefore, a simple operational method that provides good separation for D/L-amino acids in a short time is needed.&nbsp;</p><p>For food analysis, a small particle column is used to achieve appropriate separation of the small amounts of D-amino acids from the large amounts of L-amino acids and co-existing contaminants. A <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=X3"><strong>UHPLC system (Nexera X3</strong></a>) was employed in this study due to the increased system pressure caused by the use of a small particle column.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A method was developed for simultaneous separation of OPA/NIBC diastereomers for thirty-seven D/L-amino acids using a simple UHPLC system in approximately half the time of the conventional methods. By optimizing the derivatization reaction, all compounds were determined sensitively, accurately, and precisely. Separation of the target compounds from the contaminants was good in the liquor samples when evaluated using real liquor samples. It is expected to be easily applicable to D/L-amino acid profiling in food and beverage samples without using expensive MS detection or complicated multidimensional HPLC configurations as long as samples are prepared properly. Moreover, D/L-amino acid profiling could be used to research and develop foods containing D-amino acids intended to help to maintain and improve the intestinal environment, and could help in the early detection of diseases and determining optimal treatment strategies through biomarker discovery</p><h3><strong>4. Thermo Fisher Scientific: Screening of per- and polyfluoroalkyl substances (PFAS) in cosmetics: Utilizing a new combustion-ion chromatography system for total organic fluorine (TOF) analysis</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ap_004098_ic_systems_combustion_ic_environmental_ap004098_na_en_a3a1d33a24.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This application note describes a method for <strong>screening per- and polyfluoroalkyl substances (PFAS) in textiles</strong> using total organic fluorine (TOF) analysis by combustion-ion chromatography (C-IC). PFAS are widely used in textiles to provide water, oil, and stain resistance, but increasing concerns about their environmental persistence and potential health effects have led to stricter regulations worldwide. California’s AB 1817 legislation, for example, limits TOF concentrations in textiles to 100 ppm beginning in 2025 and 50 ppm by 2027, creating a need for reliable analytical methods capable of assessing PFAS content in textile products.</p><p>The study evaluates a new <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2150"><strong>Thermo Scientific Cindion Combustion Ion Chromatography System</strong></a>, which combines a Dionex Inuvion IC system with a Cindion combustion/absorption module. The system features an optimized Z-fold combustion tube design that improves combustion efficiency, shortens analysis time, reduces instrument footprint, and allows complete control through Chromeleon software. Unlike surface-sensitive techniques such as PIGE, the combustion-IC approach analyzes the entire sample, providing results that are independent of sample thickness. The method measures total fluorine (TF) after combustion and total inorganic fluorine (TIF) by direct IC analysis, with TOF calculated as the difference between TF and TIF.</p><p>To validate the approach, six textile samples representing waterproof and stain-resistant consumer products were analyzed and compared with results previously obtained using a Nittoseiko combustion-IC system. TOF concentrations ranged from approximately 1 ppm in one nylon fabric to nearly 375 ppm in a polyester baby bib. The values generated by the new Cindion system showed excellent agreement with the reference system, achieving between 100% and 105% of the previously reported results. Reproducibility was also strong, with relative standard deviations below 8% for all samples.</p><p>The authors conclude that the new Cindion C-IC platform provides an accurate, reliable, and efficient solution for PFAS screening in textiles. In addition to matching the performance of the established combustion-IC method, the enhanced system offers a flexible “2-in-1” configuration that allows seamless switching between combustion-IC and standalone IC operation. This improves workflow efficiency, reduces manual intervention, and provides manufacturers and testing laboratories with a practical tool for monitoring compliance with evolving PFAS regulations in textile products.</p><h3><strong>5. Waters Corporation: Advanced Acquisition Modes for the </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2433"><strong>Xevo MRT P10 Mass Spectrometer</strong></a></h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009362_9baa39e7de.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><p>The Waters solution sheet introduces the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2433"><strong>Xevo MRT P10 Mass Spectrometer</strong>,</a> a next-generation high-resolution mass spectrometer designed to provide significantly greater analytical depth, sensitivity, and flexibility for modern omics workflows. Compared with the previous Xevo MRT platform, the instrument delivers a reported <strong>20-fold increase in MS/MS sensitivity</strong>, incorporates Wideband Enhanced Duty Cycle (WB EDC) technology, and supports ultrafast acquisition rates of up to <strong>100 Hz for MS data</strong> and <strong>200 Hz for MS/MS data</strong>. These performance improvements are intended to enhance the detection of low-abundance compounds while maintaining high-quality spectral information across complex biological samples.</p><p>A major focus of the document is the introduction of the new <strong>SONAR Pulse Acquisition Mode</strong>, an advanced data-independent acquisition (DIA) approach. SONAR Pulse improves selectivity by rapidly stepping a quadrupole isolation window across a defined precursor mass range, allowing fragment ions to be associated with narrower precursor windows than in conventional DIA experiments. This strategy reduces spectral complexity, improves confidence in compound identification, and increases the likelihood of detecting low-level analytes that might be missed by traditional data-dependent acquisition (DDA) methods. The method supports precursor and product ion scans up to m/z 2000, multiple quadrupole isolation window sizes, acquisition speeds up to 200 Hz, and full compatibility with WB EDC technology.</p><p>The second major innovation described is <strong>Mixed Mode Acquisition</strong>, a hybrid workflow that combines targeted and untargeted analysis within a single injection. In this approach, high-sensitivity <strong>Tof MRM</strong> quantification is performed simultaneously with untargeted DIA (MSE) acquisition. This enables users to obtain quantitative data for predefined targets while also collecting comprehensive full-scan information for discovery and screening purposes. The workflow integrates seamlessly with Waters software tools, allowing targeted quantification through the MS Quan application and untargeted analysis through UNIFI or export to open data formats such as mzML for processing in third-party software packages including MZmine, MS-DIAL, DIA-NN, PEAKS, and Progenesis QI.</p><p>According to Waters, both acquisition strategies are designed to maximize information obtained from each sample injection. SONAR Pulse emphasizes deeper molecular coverage, improved selectivity, and simplified interpretation of complex DIA datasets, while Mixed Mode provides a unified quantitative–qualitative workflow that combines targeted measurement and discovery screening without compromising sensitivity or acquisition speed. Together, these capabilities position the Xevo MRT P10 as a versatile platform for metabolomics, lipidomics, proteomics, and other multiomics applications where both comprehensive characterization and accurate quantification are required.</p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 25, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 10th August 2026? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you posters by <strong>Agilent Technologies / ASMS, Thermo Fisher Scientific / ASMS </strong>and<strong> Waters Corporation / ASMS </strong>and application notes by<strong> Metrohm and Shimadzu!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Impurity Monitoring of GLP-1 Therapeutic Peptide RetatrutideUsing a 2D-LC/TOF System</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/glp_1_impurity_monitoring_2d_lc_tof_asms_2026_mp_388_agilent_eadce3f244.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Retatrutide is a next-generation triple agonist (GLP1/GIP/glucagon) and an emerging candidate among multivalent GLP1–based therapeutics. Its structural complexity and diverse impurity profile challenge conventional one-dimensional LC methods, which often lack sufficient resolving power to separate closely related impurities, sequence variants, and synthetic byproducts.&nbsp;</p><p>In this study, we demonstrate an Agilent multiple heart-cutting 2D-LC platform that enables rapid online solvent exchange and enhanced chromatographic selectivity, allowing targeted isolation of impurity peaks from a TFA-based first-dimension separation. When coupled with the Agilent 6230C Accurate Mass TOF LC/MS system, the workflow delivers fast, sensitive, and accurate mass profiling under MS-friendly second-dimension conditions, providing a robust solution for comprehensive impurity characterization of GLP-1 peptides such as Retatrutide.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?instrumentationItems=39&amp;mainauthorItems=10&amp;search=1290+infinity+III+2D-LC"><strong>Agilent 1290 Infinity III 2D-LC system</strong></a><strong> comprised the following modules:&nbsp;</strong><ul><li>1290 Infinity III Bio Multisampler with Thermostat (G7137A)&nbsp;</li><li>1290 Infinity III Multicolumn Thermostat (G7116B)&nbsp;</li><li>1290 Infinity III Diode Array Detector (G7117B) with Max-Light cartridge cell (G7117-60020)&nbsp;</li><li>1260 Infinity III Bio Flexible Pump (G7131C)&nbsp;</li><li>1290 Infinity III Bio High-speed Pump (G7132A)&nbsp;</li><li>1290 Infinity Valve Drive (G1170A) with 2D-LC ASM Valve (G5643B)&nbsp;</li><li>Two 1290 Infinity III Valve Drives (G1170A) with multiple heart-cutting valves (G5642-64000) equipped with 40 µL Bio loops&nbsp;</li></ul></li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6230C"><strong>Agilent 6230C Accurate Mass TOF LC/MS System</strong></a></li></ul><h4><strong>Conclusions</strong></h4><p>Agilent 2D-LC with multiple heart-cutting effectively bridges TFA-driven chromatographic performance with FA-compatible MS detection, overcoming ion suppression limitations.&nbsp;</p><p>The integrated 2D-LC/Accurate Mass TOF workflow delivers confident impurity identification and robust characterization, supporting peptide analysis in both QA/QC and development environments.</p><h3><strong>2. Metrohm: Vinylene carbonate water determination via coulometric Karl Fischer titration</strong></h3><p><strong>Water determination in vinylene carbonate by Karl Fischer coulometric titration made simple with alcohol-free reagents</strong></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_k_076_download_8658665940.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Vinylene carbonate (vc) is commonly used as a battery electrolyte additive in lithium-ion batteries. Its popularity is due to the positive impact it has on anode cyclability and reduction of irreversible capacity. Small amounts of moisture in Li-ion batteries can significantly decrease performance and lifetime. Therefore, moisture levels in electrolyte solutions and their additives are controlled for use in manufacturing. Until recent years, accurate moisture quantification in vinylene carbonate samples was difficult due to side reactions. With the commercial development of alcohol-free coulometric Karl Fischer reagents, accurate determination is now much more accessible to end-users.</p><h4><strong>EXPERIMENTAL</strong></h4><p>This analysis was performed using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=852+titrando"><strong>852 Titrando</strong></a> (2.852.0060) instrument, equipped with the electrodes listed in Table 1.</p><h4><strong>CONCLUSION&nbsp;</strong></h4><p>During battery manufacturing, control of all moisture present is important to guarantee adequate performance in the finished product. More easily quantifying the moisture contribution from additives such as vinylene carbonate makes this a much simpler task. The introduction of alcohol-free Karl Fischer reagents accomplishes this effectively, allowing the generation of accurate and repeatable moisture data—even for a difficult sample matrix.</p><h3><strong>3. Shimadzu: Non-Targeted Analysis of Metabolites in Alcoholic Beverages Using LabSolutions Insight Profiler</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_01241_en_57b43edb57.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>Using an LC-QTOFMS system with LabSolutions Insight Profiler non-targeted analysis software enables comprehensive comparative analysis of metabolites in food samples.&nbsp;</li><li>Principal component analysis and volcano plots can be used to detect characteristic features in each sample.&nbsp;</li><li>A variety of functions, including MS/MS spectral library searching, enable easy qualitative analysis of components.</li></ul><p>Metabolomics, a technique that analyzes metabolites in living organisms, is increasingly being applied in the food industry for product development and quality control. A particularly powerful approach is non-targeted metabolomics, which aims to analyze not only known metabolites but also unknown compounds without prior assumptions to reveal unexpected chemical differences between samples. Quadrupole time-of-flight mass spectrometry (QTOFMS), with its accurate-mass capability, is well suited for this purpose. However, the large volume of generated data creates challenges for feature identification and data comparison.&nbsp;</p><p>This article presents a case study in which LabSolutions Insight Profiler, a software platform for non-targeted analysis, was used to characterize compounds in beer and beer-like beverages. Peak detection, retention-time alignment, and library searching were performed across multiple datasets. Multivariate analysisrevealed compound profiles that likely reflect the differences in raw materials and manufacturing processes, demonstrating the utility of the approach for beverage characterization.</p><h4><strong>LabSolutions Insight Profiler&nbsp;</strong></h4><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LabSolutions+Insight+Profiler"><strong>LabSolutions Insight Profiler </strong></a>is software for batch processing of LC-QTOFMS data that enables non-targeted analysis through an intuitive workflow. It readily supports easy spectral feature detection, alignment, statistical processing, filtering, list screening, MS/MS spectra-based library searching, principal component analysis (PCA), displaying volcano or box plots, and more. Fig. 1 shows the data analysis workflow.</p><h4><strong>Analysis Conditions&nbsp;</strong></h4><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=nexera+X3"><strong>Nexera X3 UHPLC</strong></a> and<strong> </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=9030"><strong>LCMS-9030 systems</strong></a> were used as the analytical instruments. The LC method included in the LC/MS/MS Method Package for Primary Metabolites was used as the method. The data-dependent acquisition (DDA) mode was used to simultaneously acquire precursor m/z and MS/MS data. Table 2 shows the analysis conditions.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>In this study, compounds in various beer and beer-like beverages were analyzed by non-targeted analysis using an LCMS-9030 quadrupole time-of-flight mass spectrometer system. Analyzing compounds characteristic of each sample with LabSolutions Insight Profiler software confirmed that the resulting profiles reflected differences in raw materials and manufacturing methods.&nbsp;</p><p>LabSolutions Insight Profiler enables efficient non-targeted analysis by processing LC-QTOFMS data with an intuitive workflow. This workflow allows for objective evaluation of the taste, quality, and nutritional value of food products. Furthermore, this method is applicable not only to the analysis of compounds in beverages but also to non-targeted analysis of other types of samples.</p><h3><strong>4. Thermo Fisher Scientific / ASMS: High throughput targeted proteomic workflows with Adaptive Retention Time on the </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom MS</strong></a></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_004699_lsms_art_astral_zoom_proteomics_po004699_asms2026_na_en_78767efdc9.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Advances in MS instrumentation have accelerated the identification of biomarkers, but validating and translating these discoveries into assays for clinical use remains challenging and typically requires robust and accurate targeted approaches. While these often rely on predetermined reference target retention time (RT) windows, analytical column degradation or replacement, aging solvents, sample matrix effects, etc. can cause peptide RT shifts between injections and across longer-term analyses. To accommodate this, targeted MS experiments generally schedule wide target RT windows (&gt;1 min) or rely on heavy labeled peptides to trigger acquisition of endogenous peptides. Both greatly limit the number of quantifiable targets per assay. To overcome this, we utilize adaptive RT (aRT) alignment for live correction of RTs together with the speed and sensitivity of the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom MS</strong></a>. This allows reproducible tracking of &gt;2000 targets with narrow RT windows, high throughputs, such as 300 samples per day (SPD), and hybrid workflows combining targeting, of up to 1000 targets, and discovery.</p><h4><strong>Materials and methods&nbsp;</strong></h4><h5><strong>LC-MS Experiments&nbsp;</strong></h5><p>Experiments were performed using Thermo Scientific Pierce HeLa protein digest resuspended in 0.1% TFA, or individual or pooled human plasma samples. Peptides were separated using a 15 cm Thermo Scientific PepMap analytical columns (150 µm inner diameter) and the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Thermo Scientific Vanquish Neo UHPLC system</strong></a> at throughputs of 60 or 300 SPD. The liquid chromatography (LC) system was interfaced with the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom MS.</strong></a> Reference runs using MS1 and/or data-independent-acquisition (DIA) scans were acquired to obtain reference aRT spectra, and to determine target RTs. For aRT alignment, methods consisting of aRT MS1 and/or DIA scans, as well as targeted MS2 scans with RT correction were optimized. For hybrid DIA workflows, we used aRT MS1 scans for reference acquisition and alignment, combined with narrow window DIA and a targeted MS2 experiment. Observed RT shifts were caused by natural column degradation, sample matrix effects or when indicated induced by variation in gradient flow rate and buffer composition.&nbsp;</p><h5><strong>Data analysis&nbsp;</strong></h5><p>Reference DIA data was analyzed using Spectronaut. Targets lists were then generated from the search output by selecting varying number of targets evenly distributed across the RT dimension. Target RTs for smaller scale assays were manually validated and exported from Skyline, while target RTs for large scale assays were exported from Spectronaut. For alignment runs, DIA and PRM data were analyzed using Spectronaut and Skyline respectively.</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>Adaptive RT alignment on Orbitrap Astral Zoom MS shows robustness against various sources of RT shifts and has high target recovery even for thousands of targets&nbsp;</li><li>aRT enables the use of target acquisition windows &lt;15 s for robust targeting at high throughput&nbsp;</li><li>aRT Hybrid DIA allows targeting of up to 1000 targets with minimal cost to DIA depth</li></ul><h3><strong>5. Waters Corporation / ASMS: BOOSTING SENSITIVITY IN TOP-DOWN PROTEIN STUDIES USING CYCLIC IMS-ENABLED WIDEBAND ENHANCEMENT</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009471_51f2e8b546.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><p>The poster evaluates <strong>Wideband Enhancement (WBE)</strong> as a way to improve sensitivity in top-down protein mass spectrometry. In top-down workflows, intact proteins are fragmented directly, but the signal is distributed across multiple charge states, isotope envelopes, and numerous product ions, which can limit MS/MS sensitivity. WBE addresses this problem by synchronizing ion packets leaving the ion mobility region with the time-of-flight pusher, thereby increasing the number of ions that reach the detector within a selected <i>m/z</i> range.</p><p>Experiments were performed using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2434"><strong>Waters Cyclic IMS P20 Mass Spectrometer</strong></a> equipped with an <strong>electron capture dissociation cell</strong>. Samples were introduced by direct infusion in positive electrospray ionization mode. Two proteins were studied under denaturing conditions: bovine ubiquitin, approximately 8.5 kDa, and bovine carbonic anhydrase II, approximately 29 kDa. Single-pass and bypass ion mobility measurements were carried out with and without WBE, using both <strong>collision-induced dissociation (CID)</strong> and <strong>electron capture dissociation (ECD)</strong>. Data were acquired in <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/635"><strong>MassLynx</strong></a><strong> v4.2</strong> and processed using <strong>DriftScope</strong> and the <strong>waters_connect UNIFI peptide-mapping workflow</strong>.</p><p>For ubiquitin, WBE substantially increased the intensity of CID- and ECD-derived fragment ions. Improvements of up to tenfold were observed across the c- and z-ion series, while bypass ion mobility mode produced the largest overall sensitivity gain. The results indicate that WBE can enhance fragment detection while retaining the benefits of cyclic ion mobility separation and without sacrificing mass-spectral resolution.</p><p>The larger carbonic anhydrase II protein also showed marked improvements. CID fragment signals increased by up to tenfold for lower-<i>m/z</i> ions and about eightfold for higher-<i>m/z</i> fragments. Because ECD is generally less efficient than CID, the benefit of WBE was especially evident in ECD experiments: sequence coverage increased from <strong>54% without WBE to 70% with WBE</strong> in bypass mode. The authors conclude that combining WBE with complementary CID and ECD fragmentation on the Cyclic IMS P20 enables more sensitive and comprehensive top-down protein characterization.</p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 33, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 17th August 2026? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you posters by <strong>Agilent Technologies / ASMS, Thermo Fisher Scientific / ASMS </strong>and<strong> Shimadzu / ASMS </strong>and application note by<strong> Waters Corporation!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Quantitation of N-Nitroso Duloxetine N-Nitrosamine Drug Substance Related Impurities (NDSRI) in API and Formulation by 6475 LC/TQ</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_drug_impurities_lc_tq_tp_402_asms_2026_en_agilent_b933b9bddf.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Nitrosamine impurities are nitroso derivatives where the nitroso group is attached to an amine. The active pharmaceutical ingredient (API) derived from a class of nitrosamines are known as N-nitrosamine drugsubstance-related impurities (NDSRI). Nitrosamine impurities in APIs and drug products pose safety concerns, even in small quantities, and thus are a major concern for drug makers [1].&nbsp;</p><p>Analytical methods must be sufficiently sensitive to quantify the nitrosamine of interest at levels as low as 10% of the specification limit and, where feasible, down to ≤5% of the specification limit, for the determination of the limit of detection. LC/MS/MS is an inherently selective and highly sensitive analytical technique that is well suited for the identification and quantification of trace-level impurities at extremely low concentrations. Consequently, LC/MS/MS has been widely adopted within the pharmaceutical industry, particularly for nitrosamine analysis [2-3].&nbsp;</p><p>Therefore, manufacturers must develop and qualify a dedicated analytical method that is appropriate for the specific sample matrix and targeted NDSRIs. An LC/MS/MS method based on multiple reaction monitoring (MRM) was developed for the detection and quantification of the N-nitroso duloxetine NDSRI impurity over a concentration range of 0.5 to 40 ppb (absolute standard concentration), using an atmospheric pressure chemical ionization (APCI) source on an Agilent 6475A LC/TQ instrument.</p><h4><strong>Experimental</strong></h4><ul><li><strong>MS:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6475"><strong>6475 Triple Quadrupole LC/MS System</strong></a></li><li><strong>Column:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Poroshell+HPH+C18"><strong>Poroshell HPH C18</strong></a> (4.6*150mm, 2.7µm)</li></ul><h4><strong>Conclusions</strong></h4><ul><li>A highly sensitive and robust MRM LC/MS/MS method was developed for the quantitation of N-nitroso duloxetine in duloxetine hydrochloride API and finished formulation using the Agilent 6475A LC/TQ.&nbsp;</li><li>The optimized chromatographic conditions provided effective separation of the analyte from the API, placebo, and formulation matrices, ensuring reliable quantitation.&nbsp;</li><li>The calibration curve was linear over the concentration range of 0.5-40 ng/mL, with 1/x weighting. R and R2 values were observed for both to be greater than 0.99.&nbsp;</li><li>Recovery studies demonstrated efficient sample extraction, with recoveries ranging from 92-99% in API samples and 109-116% in pellet formulations at the LOQ, specification, and 200% specification levels.&nbsp;</li><li>The method also showed excellent reproducibility across all evaluated concentration levels, confirming its suitability for routine analysis.</li></ul><h3><strong>2. Shimadzu / ASMS: Non-Targeted Analysis of Per- and Polyfluoroalkyl Substances in Environmental Extracts by Microflow LC-QToF Coupled with Multi-spray ESI</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/TP_562_Non_Targeted_Analysis_of_Per_and_Polyfluoroalkyl_Substances_in_Environmental_Extracts_by_Microflow_LC_Q_To_F_Coupled_with_Multi_spray_ESI_c2a7e1d5bf.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Targeted screening methods are well established for monitoring Perand polyfluoroalkyl substances (PFAS) in environmental samples. However, PFAS comprise a large and evolving class of compounds, creating a need to screen existing, emerging, and transformation products across diverse matrices. Non-targeted Analysis (NTA) allows for the confirmation of suspected PFAS in the environment, but the sample characterization is often limited by analytical sensitivity. Microflow (0.5 – 40 µL/min) coupled with a multi-nozzle emitter enhances sensitivity by improving desolvation. When this is coupled to a high mass accuracy and resolution Quadrupole Time-ofFlight Mass Spectrometer (QToF), capable of data-dependent and independent MS/MS, PFAS characterization of unknown analytes is possible. In this study, various environmental extracts were processed and screened using NTA for PFAS compounds.</p><h4><strong>Methods</strong></h4><p>A <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+Mikros"><strong>Shimadzu Nexera Mikros LC</strong> </a>was used to introduce the sample to a Newomics DuoESI source with an M3 emitter on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=9050"><strong>LCMS-9050 QToF MS</strong></a> (Fig. 1). A direct injection on an octadecyl column without delay column was performed. Direct injection was chosen over trapand-elute configuration to minimize selectivity bias caused by the trap column.&nbsp;</p><h4><strong>Conclusion</strong></h4><p>With the increased sensitivity of microflow LC-QToF coupled with multi-spray ESI with DIA acquisition, Insight Explore aided in NTA PFAS analysis. When paired with Insight Discovery and Profiler, a streamlined batch data processing workflow with statistical analysis was shown to effectively handle complex environmental matrices and their analyses.</p><h3><strong>3. Thermo Fisher Scientific / ASMS: Robust and sensitive quantitation of 18 steroids in human serum using Thermo Scientific TSQ Certis Triple Quadrupole mass spectrometer</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_004707_lsms_18_steroids_tsq_certis_clinical_po004707_asms2026_na_en_244c52437b.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Accurate quantification of endogenous steroids in human serum is essential for biomonitoring physiological functions such as hormone regulation, reproduction, and immune response in clinical research laboratories. Liquid chromatography–tandem mass spectrometry (LC–MS/MS) is the gold standard for steroid analysis due to its superior sensitivity, selectivity, and multiplexing capability compared to immunoassays. However, steroid measurements remain challenging because of low endogenous concentrations and complex serum matrices. Here, we describe a robust and sensitive LC–MS/MS method for the simultaneous quantification of 18 steroids in human serum using the Thermo Scientific TSQ Certis triple quadrupole mass spectrometer (Figure 1). The method leverages advanced ion source design and fast acquisition to deliver enhanced sensitivity, stability and throughput suitable for high-volume laboratory workflows.</p><h4><strong>Materials and methods</strong></h4><h5><strong>Liquid chromatograph – mass spectrometry&nbsp;</strong></h5><p>Samples were analyzed on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/744"><strong>Thermo Scientific Vanquish Horizon UHPLC system</strong></a> coupled to the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2207"><strong>TSQ Certis MS</strong></a><strong> </strong>operated in selected reaction monitoring (SRM) mode. The mobile phase composition, analytical column details, LC gradient, and overlaid extracted ion chromatograms (EICs) are shown in Figure 3.&nbsp;</p><h5><strong>Data analysis&nbsp;</strong></h5><p>Data were acquired and processed using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/77"><strong>Thermo Scientific TraceFinder software</strong></a> (v 5.2).</p><h4><strong>Conclusions&nbsp;</strong></h4><p>A sensitive and robust LC–MS/MS method was developed for simultaneous quantification of 18 steroids in human serum using the Vanquish Horizon UHPLC and TSQ Certis MS with OptaMax Plus ion source. The method demonstrated excellent linearity, accuracy, and reproducibility across a wide dynamic range. Optimization of MS conditions, particularly vaporizer temperature, significantly improved sensitivity. Overall, the workflow delivers high sensitivity, selectivity, and long-term stability, providing a reliable solution for high-throughput steroid analysis in clinical and research settings.</p><h3><strong>4. Waters Corporation: Alkaline-hydrolysis Method for PFAS in Textiles and Textiles Products by Xevo™ TQ-S micro with ACQUITY™ UPLC™ H-Class Plus System</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009443_en_0ab4914d72.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><h5><strong>Benefits&nbsp;</strong></h5><ul><li>Alkaline hydrolysis method (EN 17681-1:2025) used for preparing textiles, coated textiles and textile products for PFAS analysis allowed the inclusion of side-chain fluorinated polymers&nbsp;</li><li>Extraction method provided significant advantages in handling complex textile matrices by creating clear extracts free from dispersions, settleable solids and particulates&nbsp;</li><li>Protected the high-value LC-MS/MS components from potential damage&nbsp;</li><li>The method improved analytical sensitivity, reproducibility and accuracy, enabled cost-effective and timeefficient PFAS analysis maintained high analytical quality even for challenging high-matrix samples</li></ul><p>Many PFAS are linked to health concerns because of their ability to interfere with the body’s hormone systems, acting as endocrine disruptors also, linked to other toxic effects. Since textiles come into direct and prolonged contact with the skin, there is an increased risk of human exposure—especially for babies and children.4 In addition, PFAS pose significant environmental concerns. These “forever chemicals” do not readily break down and can be released during manufacturing, washing and disposal, allowing them to enter water pathways and persist in the environment. As a result, testing for PFAS has become increasingly important in the textile industry to demonstrate supply chain transparency, build consumer trust and protect brand reputation.</p><p>Synthetic fluorinated chemicals are categorized into two main groups - non-polymeric PFAS and polymeric PFAS, known for their use as water and grease repellent, heat resistant finishes in textiles, upholstery, leather, apparel, carpet and other industrial applications such as packaging, firefighting foams, non-stick cookware, etc. (Figure 1). PFAS are fluorinated substances contain at least one fully fluorinated methyl or methylene carbon atom (without any H/Cl/Br/I atom attached to it), i.e. with a few noted exceptions, any chemical with at least a perfluorinated methyl group or a perfluorinated methylene group.2 PFAS are classified as long chain and short chain based on their perfluorinated carbon chain length. Short chain fluorinated polymers encompasses a diverse range of chemistries, categorized according to their generic chemical and repeating units structures. Few examples are: derivatives of fluorotelomers, perfluoropolyethers with varying carbon chain lengths and acrylates, epoxylates, urethane, silicones of repeated units based structures.3 Polyfluoroalkyl substances such as fluorotelomer alcohols (FTOHs) contain C–H bonds, rendering them more susceptible to degradation. The ethoxylates in fluorotelomers-methacrylate break down to FTOH whereas polymeric fluorinated urethanes, acrylates break down to PFCAs (non-polymeric and polymeric side chain fluorinated polymers). In contrast, perfluoroalkyl substances such as PFOS and PFOA are extremely persistent due to their fully fluorinated carbon chains.&nbsp;</p><p>In alkaline hydrolysis methods, methanolic aqueous sodium hydroxide is used to break down precursor PFAS such as FTOHs, branched side chain PFAS. This process releases terminal perfluorinated carboxylic acids (PFCAs), which can then be measured. However, the efficiency of hydrolysis varies among different PFAS compounds and the presence of interfering substances such as organic matter or other chemicals in the sample matrix can inhibit the cleavage and detection of these analytes.</p><h4><strong>Experimental</strong></h4><ul><li><strong>LC system:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/198"><strong>ACQUITY UPLC H-Class Plus System</strong></a> and SMFTN fitted with PFAS kit</li><li><strong>Column(s):</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1823"><strong>XBridge™ BEH™ C18 5 µm Column</strong></a>, 4.6 x 100 mm&nbsp;</li><li><strong>MS system: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/209"><strong>Xevo TQ-S micro Mass Spectrometer</strong></a></li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>By strictly following the critical steps of the alkaline hydrolysis method using methanolic aqueous sodium hydroxide (NaOH) both freely extractable PFAS and those previously bound within side-chain fluorinated polymers such as esters linked to fluorotelomer alcohols (n:2 FTOHs, where n = 4, 6, 8, 10, 12), can be effectively extracted. This approach also safeguards the LC-MS/MS instrumentation from blockages, damage, or contamination by preventing polymer accumulation and matrix interferences.&nbsp;</p><p>The analytical method using the ACQUITY UPLC H-Class Plus System and Xevo TQ-S micro LC-MS/MS System was found to be sensitive, reproducible and accurate, enabling cost-effective and time-efficient PFAS analysis in chemically processed textiles, coated textiles and textile products whilst maintaining high analytical quality even for challenging high-matrix samples.</p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 34, 2026

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European Symposium on Analytical Spectrometry (ESAS) 2026

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ICP-MS for Hybrid Photoelectrode Characterization

Modern Methods for Faster Microbial Analysis

Addressing LC Method Optimization - Scaling For Efficiency, Throughput And Reproducibility