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

News from LabRulezLCMS Library - Week 41, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 19th January 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, Shimadzu, Waters Corporation and poster by Thermo Fisher Scientific!<h3>1. Agilent Technologies: Automated Bioprocess Monitoring with Agilent 1290 Infinity III Bio Online LC Solutions</h3>Process analytics of L-alanine production using genetically modified Vibrio natriegens<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_automated_bioprocess_monitoring_1290_infinity_bioonline_solutions_5994_8865en_agilent_9f33de6ddf.pdf">Full PDF for download</a></li></ul>Bioprocess engineering is a challenging field because of the constantly changing nature of bioprocess models which make them difficult to validate.1 Consequently, process control needs to be developed at various levels using strategies tailored to these specific requirements.1 The performance and effectiveness of the bioreactor are determined by key performance indicators such as product yield, titer, production rate, and quality of the product.1 These factors can be quickly influenced by changes in process variables and the raw materials used.1,2 The ability to react quickly to problems is therefore crucial for preserving ongoing production, a factor that can be particularly significant in bioprocesses due to the substantial cost and time investmented.1,2 Such challenges can be tackled by constantly monitoring the bioprocess, which requires the ability to analyze and collect data quickly. Therefore, monitoring is of the utmost importance.&nbsp;This application note describes the advantages of using an Agilent 1290 Infinity III Bio Online LC solution with Agilent Online LC Monitoring software. A bioreactor was interfaced with a Flownamics Seg-Flow S3 sampling system for aseptic withdrawal and an Agilent 1290 Infinity III Bio Online LC to make an hourly analysis.&nbsp;This is a fully automated approach for taking sterile samples from a bioreactor and preparing or diluting them. In addition, the 1290 Infinity III Bio Online LC solution displays data in near real time, which is a crucial element for effective bioprocess&nbsp;monitoring.<h4>Experimental&nbsp;</h4><h5>Equipment&nbsp;</h5>The <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity+III+Bio">1290 Infinity III Bio </a>Online LC comprised the following&nbsp;modules:&nbsp;<ul><li>Agilent 1290 Infinity III Bio Flexible Pump (G7131A) with an InfinityLab Quick Change Bio inline filter assembly (part&nbsp;number 5067-1607), 2.1 mm id, 0.2 µm pore size&nbsp;</li><li>Agilent 1290 Infinity III Bio Online Sample Manager (G3167B) with Sample Thermostat (option #101) clustered with Agilent 1290 Infinity Valve Drive (G1170A), featuring a reactor valve pod (part number 5067-6680) and Online LC Monitoring Software&nbsp;</li><li>Agilent 1290 Infinity III Multicolumn Thermostat (G7116B) equipped with an Agilent Quick Connect Bio Heat Exchanger Std. (G7116-60071)&nbsp;</li><li>Agilent 1290 Infinity III Diode Array Detector (DAD) (G7117B), equipped with a Bio Max-Light Cartridge Cell (G4212-6008), 10 mm, 1 µL&nbsp;</li><li>Agilent 1260 Infinity High-Performance Degasser (G4225A) is connected between S1 (transport solvent) solvent line and Agilent 1290 Infinity III Bio Online Sample Manager (G3167B)&nbsp;</li></ul><h5>Software&nbsp;</h5><ul><li>Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=OpenLab+CDS">OpenLab CDS</a> version 2.8 or later versions&nbsp;</li><li>Agilent Online LC Monitoring Software version 1.3 or later&nbsp;versions&nbsp;</li><li>Flownamics FlowWeb control&nbsp;software</li></ul><h5>Instrumental configuration&nbsp;</h5>The 1290 Infinity III Bio Online LC solution was used with a Seg-Flow interface for automatic sampling and online analysis (see Figure 1). The Seg-Flow interface was used to withdraw samples from a bioreactor through a Flownamics F-Series 310 FISP probe with a ceramic membrane filter (0.2&nbsp;µm pore size) from a 5 L bioreactor. The drawn samples were sent through the built-in sample collection cup on the Seg‑Flow to the LC and the samples were retained into vials. The collected samples were then automatically derivatized by using an injector program and subsequently analyzed. A more detailed description of the instrumental configuration has been published.3<h4>Conclusion&nbsp;</h4>For online bioprocess monitoring, a fully automated setup consisting of a bioreactor, a Flownamics sampling system, and an Agilent 1290 Infinity III Bio Online LC solution was successfully established. This setup is capable of taking aseptic samples from a bioreactor, preparing, analyzing, and processing samples without the need for manual interaction. In addition, the added value of the Agilent Online LC Monitoring software was evident in the display method and the ability to track it quickly.<h3>2. Shimadzu: Analysis of Oligonucleotide Impurities Using Single Quadrupole Mass Spectrometer</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00974_en_c50bb67c7a.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>Combination use of LCMS-2050 single quadrupole mass spectrometer and LabSolutions Insight Biologics provides comprehensive characterization of oligonucleotides and related impurities.</li><li>Purity calculations for target components can be performed even on poorly separated peaks by utilizing MS spectra simultaneously acquired with UV chromatogram.</li></ul>In recent years, oligonucleotide therapeutics have been paid attention as a novel drug discovery modality because of their rapid progress of development. During the synthesis of oligonucleotide therapeutics, impurities that have differing base chain lengths are generated along with the target oligonucleotide. To ensure the safety and efficacy of the drug, comprehensive detection and identification of these impurities are required.&nbsp;Reversed phase ion-pair chromatography is often employed as a method to separate the target compound from co-existing impurities. However, it is often difficult to establish analytical conditions that provide compete separation of all impurities that are formed in synthesis process due to their similar structures and properties to the principal compound of active ingredient. Against this drawback, liquid chromatography-mass spectrometry (LC-MS) is commonly used for impurity detection and identification. For analysis of oligonucleotide impurities, quadrupole time-of-flight mass spectrometers are mainly used because of their high mass resolution and ability to perform sequence and structure estimations via MS/MS analysis. However, in quality control process, the use of a single quadrupole mass spectrometer is expected to be advantageous because of providing mass information with easy operation when impurity information is already known.&nbsp;This article presents a simulated impurity analysis of synthetic oligonucleotide using the LCMS-2050 high-performance liquid chromatography-mass spectrometer and LabSolutions Insight Biologics.<h4>Analytical conditions</h4>The employed instrument setup was <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+XS">Nexera XS inert</a> and <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-2050">LCMS-2050</a>. HPLC conditions are shown in Table 2, and MS conditions are shown in Table 3. The conditions were set where n-1(5') co-eluted with FLP, while n-3(5') was separated (Fig. 1) to demonstrate impurity analysis performance.<h4>Conclusion</h4>The simulated sample consisting of mainly FLP and small amounts of n-1(5')/n-3(5') was analyzed using the LCMS-2050 and LabSolutions Insight Biologics software and obtained data were processed appropriately. Detection, identification, and quantitation at low concentrations were accomplished not only for n-3(5') well-separated from FLP but also for n-1(5') co-eluted with FLP. In case that establishing analytical conditions is difficult, Using this instrument setup and software will provide efficient quality confirmation of oligonucleotide therapeutics.<h3>3. Thermo Fisher Scientific: Simultaneous Quantitation and Untargeted Discovery (SQUAD) workflow using multiple fragmentation techniques for quantitation and characterization of trace level nitrosamine in biological matrices</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_squad_workflow_multiple_fragmentation_techniques_po_en_94a5b27b12.pdf">Full PDF for download</a></li></ul>N-Nitrosamines are a class of carcinogenic chemical compounds that pose threat to humans exogenously through matrices like drinking water, food, cosmetics, and endogenously by nitrosation in gastrointestinal tract, nitrate to nitrite conversion, etc. An accurate, reliable analytical method is critical for detection and quantification of these trace-level, polar and low molecular weight compounds to understand the association between their exposure and related diseases.&nbsp;An optimized SQUAD workflow is presented that discovers unknown compounds in the matrix by using high resolution orbitrap and a sensitive linear ion trap detector that quantifies the low intensity nitrosamines in a single run. The workflow uses multiple fragmentation types – HCD, CID and UVPD and MSn to help characterize isomeric structures.<h4>Methods</h4>Serial dilution of Nitrosamine standards were subjected to Simultaneous Quantitation and Discovery (SQUAD) analysis using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/744">Thermo Scientific™ Vanquish™ Horizon UHPLC system</a> and the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/561">Thermo Scientific™ Orbitrap IQ-X™ Tribrid™ mass spectrometer</a> . Nitrosamine spiked matrices of human pooled urine and human Serum were subjected to SQUAD analysis.<h4>Data Analysis&nbsp;</h4>Spectra were evaluated for nitrosamines using Thermo Scientific™ FreeStyle™ software and annotated using Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1757">Mass Frontier™ 8.0 software</a>. Untargeted data analysis was performed using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1759">Compound Discoverer 3.4 software</a>. Calibration curves were generated using Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/77">TraceFinder™ 5.2 software</a>.<h4>Conclusions&nbsp;</h4><ul><li>Detection limits as low ppb levels ( 0.2 ppb –0.5 ppb) and quantitation limits (0.2 ppb- 5 ppb ) in presence of the matrix were achieved for all seven nitrosamines by applying parallel ion trap analysis&nbsp;</li><li>SQUAD analysis was run on Orbitrap IQ-X Tribrid MS and achieved low ppb level quantitation in ion trap and identified unknown compounds through discovery analysis in Orbitrap.&nbsp;</li><li>Employing nano LC helped achieve lower limit of quantitation (5 ppt)</li></ul><h3>4. Waters Corporation: Validated LC-MS/MS Method for Vitamin E Acetate in Cannabis Plants and Derived Products</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009082_en_c7a6fc6190.pdf">Full PDF for download</a></li></ul><h5>Benefits&nbsp;</h5><ul><li>The validated LC-MS/MS method provides high sensitivity and specificity for VEA quantification in complex cannabis matrices, including flower and concentrates.&nbsp;</li><li>Minimal sample preparation reduces handling time and improves laboratory throughput, supporting efficient routine analysis.&nbsp;</li><li>The method demonstrates robust performance across multiple matrices, ensuring reliable detection even in lipid-rich, chemically diverse samples.</li><li>Use of Waters ACQUITY UPLC H-Class System and Xevo TQ-S micro Mass Spectrometer enables accurate quantitation well below regulatory requirements.&nbsp;</li><li>The validated method complies with Missouri DCR and DHSS regulatory limits, enabling laboratories to confidently monitor VEA in cannabis products.</li></ul>VEA is used as a diluent and viscosity modifier in certain cannabis-derived products, including vaping formulations. Following increased public health awareness during 2019, VEA became a marker of interest for quality control and regulatory surveillance across cannabis supply chains due to its potential impact on lung health. In addition to concentrates and vape liquids, trace residues may be present in infused products and processing intermediates. Therefore, reliable quantification of VEA in these chemically diverse, lipid-rich matrices requires an analytical method that is sensitive, selective, and robust against matrix effects. In February 2024, Missouri’s DCR revised the tolerance limit for VEA in cannabis products from 0.2 ppm to 5 ppm.1&nbsp;Liquid chromatography coupled with tandem quadrupole mass spectrometry (LC-MS/MS) provides the sensitivity and specificity required to distinguish VEA from endogenous cannabinoids, terpenes, and other lipophilic excipients, while also offering the sensitivity to support low-ppm and sub-ppm action limits. Unlike UVbased methods, where co-eluting chromophores may interfere, LC-MS/MS enables targeted multiple reaction monitoring (MRM) for confident identification and accurate quantitation in complex cannabis matrices.&nbsp;This application note describes the validation of an LC-MS/MS method for the quantitation of VEA in two inhalable products, cannabis flower and cannabis concentrates. The method was developed and validated using the Waters ACQUITY UPLC H-Class System coupled with a Xevo TQ-S micro Triple Quadrupole Mass Spectrometer. Chromatographic separation was achieved with a reversed-phase ACQUITY UPLC BEH C18 Column. A streamlined sample preparation approach was applied for cannabis flowers and concentrates, which minimizes handling time and increases sample throughput.&nbsp;The validation study was conducted at GPA. Method performance was evaluated for calibration range, linearity, LOD, LOQ, accuracy, precision, recovery, repeatability, and robustness. The results of these are evaluated against acceptance criteria set by State of Missouri DHSS and presented in this application note.<h4>Experimental&nbsp;</h4><ul><li>LC system: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/198">ACQUITY UPLC H-Class Plus System&nbsp;</a></li><li>MS detection: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/209">Xevo TQ-S micro Mass Spectrometer&nbsp;</a></li><li>Column: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1952">ACQUITY UPLC BEH C18 Column</a>, 2.1 x 50 mm, 1.7 µm (p/n: 186002350)</li><li>Software: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/635">MassLynx™ 4.1 Software&nbsp;</a></li><li>Data processing: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=5&amp;search=TargetLynx">TargetLynx™</a> Application</li></ul><h4>Conclusion&nbsp;</h4>The LC-MS/MS method developed and validated for VEA quantification in cannabis flower and concentrates demonstrates excellent linearity, accuracy, precision, and robustness, and meets the regulatory requirements. Calibration curves achieved R² values greater than 0.999, with LOD and LOQ well below the Missouri action limit of 5 ppm. Matrix-spiked recoveries across flower and concentrate samples were within the 70–130% acceptance range, and QC samples met all performance criteria, confirming method reliability. Robustness testing across analysts and matrices further validated the method’s reproducibility. Overall, this approach provides a streamlined, sensitive, and regulatory-compliant workflow for laboratories, enabling accurate monitoring of VEA to support quality control, consumer safety, and regulatory compliance in cannabis-derived products

News from LabRulezLCMS Library - Week 04, 2026

Pilot study of screening method for pancreatic cancer using lipidomic profiling of plasma or serum

News from LabRulezLCMS Library - Week 18, 2026

News from LabRulezLCMS Library - Week 22, 2026

News from LabRulezLCMS Library - Week 23, 2026

This study presents a rapid and sensitive LC-MS/MS method for determining flibanserin in products marketed as female sexual desire enhancers. The method was fully validated according to ICH guidelines, achieving a low quantification limit and a short 5-minute analysis time. Confirmation was performed using LC-MS-IT-TOF.Analysis of commercial products revealed either the absence or only trace amounts of flibanserin, raising concerns about product authenticity, efficacy, and consumer safety. In addition, sustainability assessment demonstrated that the analytical approach is suitable for routine quality control applications.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c13004">Determination of Flibanserin in Female Sexual Desire Enhancer Products by LC–MS/MS and Its Confirmation by LCMS-IT-TOF</a></h4>Abeer Elriş, Mazlum Akif Altun, Saniye Özcan, Serkan Levent, and Nafiz Öncü Can*ACS Omega 2026, 11, 6, 10828–10836<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsomega.5c13004">https://doi.org/10.1021/acsomega.5c13004</a><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6></blockquote>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.<div>In the world, many people experience sexual problems at some point in their lives. Women are disproportionately affected due to the lack of appropriate treatments in modern medicine, leading to most of them not receiving treatment or finding an appropriate solution. The research showed that one in every 10 women in the United States has some form of sexual dysfunction. <a href="javascript:void(0);">(1)</a> Flibanserin (FLB), an active substance that can be used especially in hypoactive sexual desire disorder (HSDD), has become a source of hope for many women with this problem.FLB was initially developed as an antidepressant; however, due to FLB’s inability to demonstrate an antidepressant effect in the experiments, participants indicated heightened sexual desire as a side effect, suggesting the potential application of this substance in the treatment of HSDD. So the Food and Drug Administration (FDA) approved FLB again in 2015, but this time for the treatment of HSDD instead of depression. <a href="javascript:void(0);">(2)</a> According to the data obtained from the begonia, daisy and violet studies, 12.8% of those taking FLB experienced side effects such as drowsiness, 10.6% dizziness, 9.9% nausea and 7.1% fatigue. <a href="javascript:void(0);">(3)</a> Due to these side effects, it is recommended that FLB be taken before going to bed. Also, taking FLB with alcohol was avoided due to the risk of fainting and hypotension.Although flibanserin (FLB) is one of the few active substances approved for the treatment of hypoactive sexual desire disorder, the number of available studies remains limited, as its approval by the FDA is relatively recent. The majority of published studies have focused on pharmaceutical quality control or bioanalytical applications, predominantly employing LC–MS/MS <a href="javascript:void(0);">(4−10)</a> and HPLC <a href="javascript:void(0);">(4,11)</a> techniques. These studies have investigated a wide range of sample matrices, including natural products such as beer, grape wine, and herbal tea, as well as biological samples (e.g., plasma and brain tissue) and pharmaceutical formulations such as Veroxeserin. In contrast, a study conducted in Poland reported the presence of FLB in certain herbal products, raising concerns regarding the unauthorized use of this compound. <a href="javascript:void(0);">(7)</a> This finding prompted questions about the potential presence of FLB in products marketed as female sexual desire enhancers in the Turkish market. Therefore, the present study aimed to determine FLB in various commercially available products obtained in Türkiye to assess the presence of FLB and to characterize their contents. Notably, it was observed that some products lacked manufacturer address information, despite regulatory requirements, and that the recommended usage instructions were concerning, particularly in light of the known side effects of FLB.This study aimed to develop and validate a sensitive and reliable LC–MS/MS method for the determination of flibanserin (FLB) in commercial products collected from the Turkish market that are marketed as female sexual desire enhancers. The samples were additionally analyzed using an LC-MS-IT-TOF instrument to support the qualitative characterization of their contents. A further objective of this work was to investigate whether FLB is being inappropriately incorporated into over-the-counter products in a manner analogous to the illicit use of sildenafil in food products or dietary supplements. By screening products predominantly obtained through online sales channels, this study sought to assess the potential unauthorized presence of FLB and to highlight possible risks to women’s health associated with such unregulated practices. As a complementary aspect, the environmental and practical performance of the proposed analytical approach was evaluated using greenness, whiteness, and blueness assessment tools, including ComplexMoGAPI, AGREE, WAC, and BAGI.<h4>2. Experimental Section</h4><h5>2.2. Instrumentation</h5>The mass spectrometric studies were succeeded in an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=8040">8040 model MS/MS</a> instrument connected to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+XR">Nexera XR Series LC</a> (from Shimadzu); the whole system was composed with DGU-20A3R degasser, LC-20AD gradient pump, SIL-20AC autosampler, CBM-20A communications bus module, CTO-10ASVP column oven.The LCMS-IT-TOF series liquid chromatography–high-resolution mass spectrometry instrument (Shimadzu) was used for structural characterization; the instrument consisted of the following modules: DGU-20A3 degasser, 2× LC-20AD gradient pump, SIL-20A autosampler, CTO-10ASVP column oven, CBM-20A communication module, and ion-trap and time-of-flight (IT-TOF) mass spectrometer. LCMS Solutions 3.80 software was used for setting instrumental parameters and spectrum integration.<h4>3. Result and Discussion</h4><h5>3.1. Ionization Characteristics of Flibanserin</h5>Although the LC–MS/MS system has some financial disadvantages, its ability to detect even very low concentrations makes it a suitable system for this study. Analyses were performed to determine the ionization type, and it was determined that FLB causes positive ionization. The daughter ions and collision energy observed under multiple reaction conditions using the electrospray ionization method are given in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c13004#tbl2">Table 2</a>. The waiting time was determined to be 100 ms. Three daughter ions were detected, 161.05, 119.05, and 133.05 m/z. Their fragmentation paths are given in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c13004#fig1">Figure 1</a>. It is suggested that the daughter ion with the m/z value of 161.05 is fragmented by heterolytic fragmentation, the daughter ion with the m/z value of 133.05 is fragmented by heterolytic fragmentation and carbonyl release, and the ion with the m/z value of 119.05 is fragmented by McLafferty rearrangement and hydroxyl release. The product ions at m/z 161 and m/z 119 have been reported in previous studies, while the ion at m/z 133 is considered a transitional step and is formed in lower abundance than the other two. <a href="javascript:void(0);">(4,6)</a><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2026_11_6_10828_10836_Figure_1_Fragmentation_paths_of_FLB_in_positive_electrospray_ionization_mode_79d6842698.jpeg" alt="ACS Omega 2026, 11, 6, 10828–10836: Figure 1. Fragmentation paths of FLB in positive electrospray ionization mode." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2026_11_6_10828_10836_Figure_1_Fragmentation_paths_of_FLB_in_positive_electrospray_ionization_mode_79d6842698.jpeg 245w," sizes="100vw" width="1458" height="807"><h5>3.7. Comparison of the Method with Data in the Literature</h5>The analytical methods developed for FLB analysis in the literature were summarized in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c13004#tbl5">Table 5</a>. The methods could be divided into two parts: quality control and bioanalytical purposes. It was obvious that all the instrumentation systems used for bioanalytical analyses presented so far were LC–MS/MS. The methods developed for quality control analyses were based on analysis with HPLC and LC–MS/MS. Apart from these, there are two other high-throughput methods that were developed for various purposes. However, these two methods have significant disadvantages, such as requiring experience and mastery for routine analyses. <a href="javascript:void(0);">(17,18)</a> Poplawska et al. were created to analyze both FLB and tadalafil at the same time in herbal products using an LC system along with PDA, MS, and a charged aerosol detector, just like the method that was developed. <a href="javascript:void(0);">(7)</a> They also characterized herbal preparations with LCMS-IT-TOF. Compared to their method, our method has advantages such as a working range that was approximately 100 times and LOQ was 0.5 times lower. Also, they characterized 9 compounds in herbal products with high-resolution mass spectrometry studies. Our method used high-resolution mass spectrometry to characterize all samples from 9 different market brands in detail. In addition, starting from sample collection to final analysis, the principles of less environmental harm and efficient and sustainable analytical method development were considered and evaluated with 4 different metric tools, which is another originality of the our article. Moreover, this study encourages other researchers to focus on such synthetic products and assess their impact on public health. In certain societies, these products hold a peculiar appeal: their sale remains hidden, yet their use is widespread. As a result, the table already presents a detailed comparison of all the methods developed so far. <a href="javascript:void(0);">(19)</a><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2026_11_6_10828_10836_Table_5_Comparison_with_Previous_Studies_5e930ca443.webp" alt="ACS Omega 2026, 11, 6, 10828–10836 - Table 5. Comparison with Previous Studies.webp" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2026_11_6_10828_10836_Table_5_Comparison_with_Previous_Studies_5e930ca443.webp 122w," sizes="100vw" width="625" height="797"><h4>4. Conclusion</h4>Due to the lack of the drug treatment for hypoactive sexual desire disorder in women and the feeling of shame or hesitation stemming from cultural reasons. People in many countries do not think about or try to seek medical help for this issue. This situation not only complicates the diagnosis of such diseases but also exposes those affected to potential harm. Many women who cannot get medical help or access treatments like flibanserin and bremelanotide, which are available in only a few countries, often seek other options. In this case, products marketed as sexual desire enhancers for women are based on taking advantage of people’s helplessness. When marketing such products, the following is stated: “If you want to make a sweet surprise for your partner without him knowing, it will be enough to drop 7–8 drops into her drink and wait for half an hour.” Beyond the fact that such statements could lead women to take these products against their will, marketing them in this way encouraging people to use them and making it seem normal is also wrong.FLB was licensed by the United States Food and Drug Administration as the only medication for the treatment of female sexual interest/arousal disorder of any degree. <a href="javascript:void(0);">(11)</a> The current LC–MS/MS method is a novel, simple, and time-saving analytical method for the determination of FLB with a low quantification limit. The method was fully validated and used to determine FLB in samples that were bought as a solution to the treatment of female sexual desire enhancement. It has been shown that some of the products did not include content information. In addition, it has also been determined that the manufacturer’s address was present in some products while not others. As a result of the analysis, in some products had low concentration of FLB, which was not enough to make an effect. When the same samples were given to LCMS-IT-TOF to characterization, it was shown that the contents of the product did not match with that given in the lists on their boxes, and they included substances like caffeine, lactose, and citric acid, which have no effect on the disease., Finally, analyzing products like this in detail and identifying any substances that may threaten human health is an important point in terms of public health, especially considering that patients using such products do not have any other solution in Türkiye or in the other countries.In the present study, a comprehensive screening of 15 finished products was conducted, making it one of the most extensive surveys of commercially available formulations reported in the literature to date. Owing to the nanogram-per-milliliter-level LOQ achieved with the developed LC–MS/MS method, the method offers not only a highly sensitive approach for the analysis of finished products but also a potential alternative for plasma and urine analyses in future bioanalytical applications. Furthermore, the method is distinguished by its strong ecological profile, demonstrated through multiple green analytical chemistry assessment tools, underscoring its suitability as an environmentally conscious analytical approach. Although the proposed method demonstrated favorable greenness, whiteness, and blueness characteristics, further enhancements in environmental performance may be achieved in future studies through the implementation of miniaturized or low-flow LC systems and the integration of automated sample preparation, which could reduce energy consumption and improve overall sustainability.Overall, the analytical strategy presented herein provides a robust and versatile platform that can be effectively utilized across pharmaceutical quality control laboratories, food and dietary supplement testing facilities, and a wide range of academic research settings. This study therefore represents a valuable contribution to the field by combining comprehensive product surveillance with a highly sensitive, validated, and sustainability-oriented analytical methodology.</div>

Determination of Flibanserin in Female Sexual Desire Enhancer Products by LC–MS/MS and Its Confirmation by LCMS-IT-TOF

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