This novel gas chromatography (GC)–MS approach enables analysis of the suspected mutagens bis(pinacolato)diboron (BPD) and tetrahydroxydiboron (BBA) found at low-levels in certain intermediates and active pharmaceutical ingredients (APIs), even in the presence of boron from other sources.
In this article, the use of comprehensive two-dimensional liquid chromatography (LC×LC) coupled to mass spectrometry (MS) for characterizing glycosylation of therapeutic enzymes is presented.
Trypsin is one of the most commonly used proteases in peptide mapping protocols because of its high level of specificity. However, trypsin alone is not always sufficient for full sequence coverage. In this article, the authors detail how trypsin was combined with chymotrypsin to overcome this, and the benefits of an automated platform.
A new approach based on post-column in situ hydrogenolysis, and flame ionization was used here to improve characterization of volatile aldehydes. We review and describe that approach here.
Quantification of Tau proteoforms in cerebrospinal fluid (CSF) could be useful to diagnose neurodegenerative diseases. LC–MS/MS results can help explain the underlying molecular mechanisms of disease evolution.
The investigation of airborne PFAS transmission is important in preserving the outdoor urban environment. The authors explain why GC–MS/MS and LC–MS/MS are the best techniques for analyzing airborne PFAS.
The authors describe the results they've achieved by using water heated to 100–240 ºC as a liquid eluent for reversed-phase HPLC instead of an organic modifier. They point out that this alternative avoids many of the problems – toxicity, flammability, and cost – associated with organic modifiers.
Because the Covid-19 pandemic of 2020–2023 disrupted yearly face-to-face events, the Dal Nogare Award Symposium at Pittcon 2023 included both the 2021 and 2022 winners. Read more about the symposium here.
Better sample preparation and miniaturized separations are enhancing these analyses.
In this extended special feature to celebrate the 35th anniversary edition of LCGC Europe, key opinion leaders from the separation science community explore contemporary trends in separation science and identify possible future developments.
We explore the impact of two different stationary phases and ion-pair reagents on the retention behavior of a therapeutic peptide using reversed-phase liquid chromatography. This information is of fundamental importance for the development of reliable, selective, and fast analytical methods able to separate and identify the target peptide.
Accelerated solvent extraction (ASE) is widely viewed as a better alternative to GC–MS when analyzing persistent organic pollutants (POPs). The authors explain why new technological developments offer many benefits and accelerate POP sample preparation processes.
By calculating optimal stationary-phase composition and physical parameters, column developers can construct columns that provide the exact separation requirements desired by analysis or current methods.
This review article discusses scientific rationales and current best practices in the pharmaceutical industry for performing chromatographic peak purity assessments (PPA). These activities are associated with the development and validation of liquid chromatographic (LC) stability-indicating analytical methods applicable to regulatory submissions of small-molecule drug candidates. The discussion includes a comprehensive overview of the PPA-related regulatory and scientific landscape and common industry approaches to obtain PPA results, as well as the strengths and weaknesses of PDA-facilitated ultraviolet (UV) PPA and other PPA techniques.
In the present study, a gradient reversed-phase high-performance liquid chromatography (RP-HPLC) method has been designed and validated to quantify ornidazole (OZ) in the marketed formulation (oral gel) with the application of QbD.
For this year’s career issue, LCGC North America teamed up with the American Chemical Society Subdivision on Chromatography and Separations Chemistry to ask the analytical chemistry community what skills new employees in the field need to succeed. In this report, we analyze the survey results and explore how they can inform the future of analytical chemistry curriculum development.
This application note demonstrates how the Empore EZ-Trace SPE system is used to perform multiple extractions simultaneously while achieving clean and reproducible results using EPA Method 525.3 as an example application.
The benefits of a robustness assessment for the analysis of a NIST mAb using a wide pore C4 LC column are described.
This information is supplementary to the article “Non-aqueous Ion-Exchange Chromatography Using High Acid‑base Concentration: A Strategy for Purifying Non-crystalline Pharmaceutical Intermediates” that was published in the March 2022 issue of LCGC Asia Pacific.
Employing ion mobility at atmospheric pressure without vacuum enables coupling to high-resolution mass analyzers. High performance ion mobility–orbital trap mass spectrometry (HPIM-OT-MS) is a useful alternative for separating isomers, such as isomeric metabolites seen in drug discovery.
What parameters can influence an siRNA separation?
FoodOmicsGR_RI aims to characterize unique Greek products and highlight their value and quality using cutting-edge omics technology.
An unexpected retention order for ketamine analogs was observed when using a biphenyl stationary phase for liquid chromatography-mass spectrometry (LC–MS).
Although well known, the extent of adduct ion formation in LC–ESI-MS/MS, and the implications for quantitative analysis and analyte characterization are not fully appreciated. We explore this problem and explain the implications for reproducibility, quantitative and qualitative analyses, and DDA and DIA.
Pharmaceutical excipients, such as polyethylene glycol-based polymers, must be tested for the presence of ethylene oxide (EtO) and 1,4-dioxane as part of a safety assessment, according to USP Chapter <228>.
This article explores the potential of microchip capillary electrophoresis–mass spectrometry (CE–MS) for the characterization of intact biopharmaceuticals, and how this technique can effectively be employed to monitor essential quality attributes of interest.
Why is SFC becoming increasingly more important as a sustainable analytical technique?
Current sample preparation procedures for LC–MS as applied to samples from biological matrices.