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Supplementary Info: Non-aqueous Ion-Exchange Chromatography Using High Acid‑base Concentration: A Strategy for Purifying Non-crystalline Pharmaceutical IntermediatesThis 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.
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Guidance on Dissolution Testing for Optimized Lab FiltrationGuidance to help pharma laboratories select the right dissolution filter and conduct robust analyses that fulfill current regulatory requirements.
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Modifying the Metal Surfaces in HPLC Systems and Columns to Prevent Analyte Adsorption and Other Deleterious EffectsA novel surface modification technology has been developed to reduce interactions between analytes and metal surfaces in HPLC instruments and columns. We demonstrate the impact of this technology on peak symmetry, peak area, and injection-to-injection and column-to-column reproducibility for several metal-sensitive analytes.
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Analysis of Boronic Compounds as Potential Mutagenic Impurities in Drug Substances By GC–MSThis 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.
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Detailed Glycosylation Analysis of Therapeutic Enzymes Using Comprehensive 2D-LC–MSIn 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.
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Enhancing Peptide Mapping Sequence Coverage Through an Automated Dual Protease DigestTrypsin 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.
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In situ Hydrogenolysis with 3D-Printed Jet and Flame Ionization Detection for Carbon Oxides and Volatile Aldehydes AnalysisA 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.
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LC–MS/MS for the Quantification of Tau and Phosphorylated Tau in Alzheimer’s Disease Patients’ CSFQuantification 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.
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A Multiphase Sampling and Analytical Approach for Investigating Airborne PFAS TransmissionThe 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.
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Superheated Water: A New Look at Chromatographic Eluents for Reversed-Phase HPLCThe 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.
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Dal Nogare Session Highlights Approaches for Difficult Separations, Improved Efficiency, Better Sustainability, and Career SuccessBecause 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.
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Development of Highly Sensitive LC–MS and CE–MS Methods for In-Depth Proteomic and Glycomic Profiling of Limited Biological SamplesBetter sample preparation and miniaturized separations are enhancing these analyses.
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Separation Science: The State of the Art: Nontargeted Screening in Environmental Analysis: An Example Showing Migration of Chemicals from Reusable Sports Plastic Bottles into Drinking WaterIn 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.
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The Role of Adsorption and pH of the Mobile Phase on the Chromatographic Behavior of a Therapeutic PeptideWe 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.
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New Technologies That Accelerate Persistent Organic Pollutant (POP) Sample PreparationAccelerated 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.
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Achieving Optimum GC Separation – Designing New Capillary Column Stationary Phases Using Computer ModelingBy 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.
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Liquid Chromatographic Peak Purity Assessments in Forced Degradation Studies: An Industry PerspectiveThis 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.
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Validation of HPLC-DAD Based Stability Indicating Assay Method for Ornidazole in Periodontal Polymeric Hydrogel: Robustness Study using Quality by Design (QbD) ApproachIn 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.
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LCGC and ACS Subdivision on Chromatography and Separations Chemistry Survey 2023: What Skills Do New Analytical Chemistry Employees Need?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.
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Using the Empore EZ-Trace SPE Workstation to Perform Efficient and Reproducible Extractions of SVOCsThis 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.
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Method Robustness and Reproducibility for Monoclonal Antibody Purity AnalysisThe benefits of a robustness assessment for the analysis of a NIST mAb using a wide pore C4 LC column are described.
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Supplementary Info: Non-aqueous Ion-Exchange Chromatography Using High Acid‑base Concentration: A Strategy for Purifying Non-crystalline Pharmaceutical IntermediatesThis 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.
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Separation of Isomeric Metabolites and Gangliosides with High Performance (Drift Tube) Ion Mobility–Mass SpectrometryEmploying 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.
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A Study on Optimum Method Conditions for Denaturated and Non-Denaturated siRNA by Ion Pair Reversed-Phase Liquid ChromatographyWhat parameters can influence an siRNA separation?
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Innovation in Nutrition and Food Analysis: The FoodOmicsGR_Research InfrastructureFoodOmicsGR_RI aims to characterize unique Greek products and highlight their value and quality using cutting-edge omics technology.
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On the Surprising Retention Order of Ketamine Analogs Using a Biphenyl Stationary PhaseAn unexpected retention order for ketamine analogs was observed when using a biphenyl stationary phase for liquid chromatography-mass spectrometry (LC–MS).
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The Origin and Implications of Artifact Ions in Bioanalytical LC–MSAlthough 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.
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Rapid Quantitative Analysis of Ethylene Oxide and 1,4-Dioxane in Polymeric Excipients Using SIFT-Mass SpectrometryPharmaceutical 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>.
