News from LabRulezLCMS Library - Week 34, 2026
LabRulez / AI: News from LabRulezLCMS Library - Week 34, 2026
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!
👉 SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES
👉 Need info about different analytical techniques? Peek into LabRulezGCMS or LabRulezICPMS libraries.
This week we bring you posters by Agilent Technologies / ASMS, Thermo Fisher Scientific / ASMS and Shimadzu / ASMS and application note by Waters Corporation!
1. Agilent Technologies / ASMS: Quantitation of N-Nitroso Duloxetine N-Nitrosamine Drug Substance Related Impurities (NDSRI) in API and Formulation by 6475 LC/TQ
- Poster
- Full PDF for download
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].
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].
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.
Experimental
- MS: 6475 Triple Quadrupole LC/MS System
- Column: Poroshell HPH C18 (4.6*150mm, 2.7µm)
Conclusions
- 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.
- The optimized chromatographic conditions provided effective separation of the analyte from the API, placebo, and formulation matrices, ensuring reliable quantitation.
- 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.
- 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.
- The method also showed excellent reproducibility across all evaluated concentration levels, confirming its suitability for routine analysis.
2. Shimadzu / ASMS: Non-Targeted Analysis of Per- and Polyfluoroalkyl Substances in Environmental Extracts by Microflow LC-QToF Coupled with Multi-spray ESI
- Poster
- Full PDF for download
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.
Methods
A Shimadzu Nexera Mikros LC was used to introduce the sample to a Newomics DuoESI source with an M3 emitter on a LCMS-9050 QToF MS (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.
Conclusion
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.
3. Thermo Fisher Scientific / ASMS: Robust and sensitive quantitation of 18 steroids in human serum using Thermo Scientific TSQ Certis Triple Quadrupole mass spectrometer
- Poster
- Full PDF for download
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.
Materials and methods
Liquid chromatograph – mass spectrometry
Samples were analyzed on a Thermo Scientific Vanquish Horizon UHPLC system coupled to the TSQ Certis MS 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.
Data analysis
Data were acquired and processed using Thermo Scientific TraceFinder software (v 5.2).
Conclusions
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.
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
- Application note
- Full PDF for download
Benefits
- 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
- Extraction method provided significant advantages in handling complex textile matrices by creating clear extracts free from dispersions, settleable solids and particulates
- Protected the high-value LC-MS/MS components from potential damage
- 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
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.
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.
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.
Experimental
- LC system: ACQUITY UPLC H-Class Plus System and SMFTN fitted with PFAS kit
- Column(s): XBridge™ BEH™ C18 5 µm Column, 4.6 x 100 mm
- MS system: Xevo TQ-S micro Mass Spectrometer
Conclusion
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.
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.
