News from LabRulezLCMS Library - Week 32, 2026
LabRulez / AI: News from LabRulezLCMS Library - Week 32, 2026
Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 3rd 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, Shimadzu / ASMS, Thermo Fisher Scientific / HPLC Symposium and Waters Corporation / ASMS and application note by Metrohm!
1. Agilent Technologies / ASMS: Ultra-Trace Quantification of N-Nitroso-desmethyl-sumatriptan with Interference Resolution Using LC–TQ
- Poster
- Full PDF for download
Sumatriptan succinate, an antimigraine drug contains nitrosylating functional groups and is susceptible to forming its own nitrosamine drug substance-related impurity (NDSRI), specifically N-nitroso-desmethylsumatriptan. As a Category 1 genotoxic impurity, its specification limit is established at 0.0428 ppm with respect to the API. In this study, samples and standards were prepared in methanol:water (1:1, v/v). The LC/TQ method was developed with a target limit of detection (LOD) at least 20-fold lower than the specification limit to ensure adequate sensitivity. Analytical data were collected in replicate for a 10 mg/mL API sample, as well as LOQ- and specification-level spiked samples, to evaluate recovery, relative standard deviation (RSD), linearity, and repeatability.
Experimental
- LC System: 1290 Infinity III UHPLC
- MS: 6495D LC/TQ
- Column: Poroshell 120 EC C18, 3x150mmx2.7µm, 40 Deg C
Conclusions
- A sensitive and robust method has been developed for N-nitroso-desmethyl Sumatriptan in Sumatriptan.
- Method LOQ is 10% lower than specification level, RSD of <5%, and linearity across 0.00214 to 0.1 ppm.
- The recovery of NDSRI in Sumatriptan at LOQ level and specification level are 95%.
2. Metrohm: Moisture analysis of rebaudioside M by Karl Fischer titration
Simplified rebaudioside M moisture determination via volumetric Karl Fischer titration paired with an oven system
- Application note
- Full PDF for download
Natural sweeteners like stevia and its derivatives are an increasingly important part of the global sweetener market as more consumers substitute sugar with healthier alternatives. Stevia’s derivatives are significantly sweeter than table sugar. These compounds are estimated to be 50 to 300 times sweeter in comparison. This sweet taste coupled with the fact that the human body cannot metabolize steviol glycosides (i.e., they contribute zero calories to one’s diet), makes them a very attractive sugar replacement.
The moisture content of stevia materials is a crucial factor when discussing their shelf life and stability. Measuring the moisture content of a stevia derivative, rebaudioside M, using an oven system coupled with volumetric Karl Fischer (KF) titration provided a repeatable approach for quantifying the moisture content of this material.
Experimental
The analysis was carried out with a Double Pt ring electrode for volumetry (6.00346.100). Testing was executed on the 874 Oven Sample Processor (2.874.0120) coupled with an 852 Titrando (2.852.0060). Approximately 0.2 g of sample was weighed into an 874 Oven Sample Processor 6 mL vial and placed onto the rack. The oven was set to a temperature of 100 °C, and the evaporated moisture was carried to the volumetric titration vessel by nitrogen gas flow at 70 mL/min. The moisture from the sample was titrated with Hydranal Comp 5 reagent.
Conclusion
Natural low-calorie sweeteners like stevia derivatives are growing in popularity as people choose healthier alternatives to sugar. Working to develop standardized, specific methodology can help support sweetener industry development, effective quality assessment, and the evaluation of rebaudioside M and other steviol glycosides’ stability.
This Application Note provides a foundation for the analysis of stevia powder by Karl Fischer titration. An oven system paired with volumetric Karl Fischer analysis provides an accurate, repeatable method to evaluate stevia powder and its derivatives. This method’s compatibility with the 874 Oven Sample Processor allows increased sample throughput through automation, providing operators even more time to complete other important tasks in parallel.
3. Shimadzu / ASMS: Quantitative analysis of 6 beta blockers on an LCMS-8045RX
- Poster
- Full PDF for download
Beta-adrenergic blocking agents, commonly known as beta blockers, competitively inhibit the binding of catecholamines such as epinephrine and norepinephrine to β-adrenergic receptors, thereby reducing heart rate and blood pressure. These drugs are widely prescribed for the treatment of hypertension, angina and heart failure1 . However, beta blockers may also be misused by athletes resulting in their inclusion on the World Anti-Doping Agency (WADA) prohibited list2 . Owing to both their therapeutic importance and potential misuse, sensitive and selective analytical methods are required for reliable detection and quantification. Liquid chromatography tandem mass spectrometry (LC-MS/MS) offers high sensitivity and specificity for such analyses.
Method
Nadolol, metoprolol, propranolol, atenolol & carvedilol were purchased from Sigma Aldrich and Thermo Fisher Scientific. Standards were prepared in 1 mg/mL in LCMS grade methanol. Nexera 40-series HPLC system connected to a LCMS-8045RX was used for data acquisition. The mixture of standards was further diluted in LCMS grade methanol (Sigma Aldrich) and Sigmatrix urine diluent to create the standards for the calibration curves. A Shim-pack Velox Biphenyl column was used for the chromatographic separation. All analytes were ionized with electrospray ionization (ESI) in positive ion mode.
Conclusion
- Superior sensitivity in complex matrices: Limit of Detection (at accuracy ±20% and S/N > 3) of 0.010 ng/mL for all the analytes evaluated in this study.
- Excellent linearity and accuracy: Linear responses (with R2 > 0.99) observed across the evaluated concentration range, and consistent accuracy within ±20% for all 17 calibrants included in this study.
- Optimized throughput: Automated interface and MRM optimization via LabSolutions Connect MRM ensured maximum signal-to-noise determination for this study, while the high-organic flush at the end of each run, maintained column integrity
4. Thermo Fisher Scientific / HPLC Symposium: A switchable 2D-LC platform in PAT: routine UV monitoring or MS-based characterization of mAb PQAs directly from the bioreactor
- Poster
- Full PDF for download
Monitoring quality attributes throughout the upstream processing of mAbs is critical due to potential effects of biological variability on product safety and efficacy. Thus, there is a growing need for streamlined analytical workflows that provide timely and reliable insights to enable fast and informed process decisions.
Materials and methods
- Thermo Scientific Vanquish Flex Simple Switch 2D-LC system for loop heart-cutting consisting of Quaternary Pump F (VF-P20-A), Binary Pump F (VF-P10-A-01), Dual Split Sampler FT (VF-A40-A-02), 2x Column Compartment H (VH-C10-A-03), and Diode Array Detector FG (VF-D11-A-01)
- Thermo Scientific Orbitrap Exploris MX Mass Detector (BRE725536) with BioPharma option (BRE725539)
- Thermo Scientific MAbPac Protein A column, 12 µm, 4 x 35 mm (PN 082539)
- Thermo Scientific ProPac 3R SCX, 2 x 50 mm, 3 µm (PN 43103-052068)
- Thermo Scientific MAbPac SEC-1, 5 µm, 4 x 300 mm (PN 074696)
Data analysis
Thermo Scientific Chromeleon 7.3.2 Chromatography Data System (CDS) and Thermo Scientific BioPharma Finder 5.2 software
Conclusions
- Switchable 2D-LC-UV/MS offers a streamlined approach for at-line monitoring of mAb titer, charge and size variants directly from the bioreactor in <1h.
- UV monitoring provides quick and simple trendlines, while HRAM-MS allows deep characterization at intact level.
- Near real-time information supports in-time process decisions to protect yield and product quality.
5. Waters Corporation / ASMS: SOFTWARE TOOLS FOR AUTOMATED LC/MS ANALYSIS OF CRITICAL QUALITY ATTRIBUTES OF mRNA MOLECULES
- Poster
- Full PDF for download
This poster presents an automated LC-MS workflow for evaluating three critical quality attributes (CQAs) of mRNA therapeutics: 5′-capping efficiency, Poly(A) tail length and heterogeneity, and mRNA sequence integrity. A custom firefly luciferase (Fluc) mRNA construct containing a Cap-1 structure, 1,919 nucleotides, and a Poly(A) tail was used as the model sample. Importantly, all three CQAs were assessed using a single LC-MS assay, supported by specialized waters_connect software tools designed to streamline nucleic acid characterization from sequence entry through final data processing.
The analytical platform consisted of a Waters ACQUITY Premier Binary UPLC System with TUV detector coupled to a Xevo MRT Q-Tof Mass Spectrometer, which uses multi-reflectron time-of-flight technology. Separations were performed on an ACQUITY Premier OST 1.7 µm, 300 Å, 2.1 × 150 mm column, while data-independent acquisition was carried out in MSE mode. Data processing used the waters_connect Informatics Platform together with SYNTHETIC Library 2.0, MAP Sequence 2.0, and INTACT Mass 1.9 applications. For sequence mapping, the mRNA was independently digested using four endonucleases—RNase T1, RapiZyme MC1, RapiZyme Cusativin, and human RNase4—providing complementary cleavage patterns.
The workflow produced detailed information on both capping and Poly(A) tail characteristics. The Fluc mRNA showed 100% capping efficiency, with 62.7% carrying an m7GpppAm Cap-1 structure and 37.3% an m7GpppGm Cap-1 structure; no uncapped digestion product or Cap-related impurities were detected. Poly(A) tail analysis identified ten major species ranging from 98-mer to 107-mer, resulting in an average Poly(A) tail length of 102.3 nucleotides. The Xevo MRT Q-Tof provided high-resolution measurements—approximately 100,000 resolution in the examples shown—and very good mass accuracy for the detected Poly(A) species.
For sequence integrity, combining the four complementary enzymatic digestions achieved 93.7% unambiguous mRNA sequence coverage, demonstrating the value of a multi-enzyme approach for comprehensive sequence confirmation. MAP Sequence 2.0 also automatically distinguished structural isomers using elevated-energy fragment-ion information, helping resolve isobaric and isomeric digestion products with less manual interpretation. Overall, the poster demonstrates that high-resolution MSE acquisition on the Xevo MRT Q-Tof combined with automated waters_connect informatics can provide an integrated and efficient approach for comprehensive characterization of key mRNA quality attributes.
