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Automated PFAS Extraction with Resolvex® PrepThis note demonstrates efficient PFAS extraction from contaminated surface water using automated mixed-mode µSPEed® cartridges and Tecan's Resolvex® Prep.
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Affinity Selection-Mass Spectrometry: Defining the Bioactive Compounds in Complex Mixtures of Natural Products and Combinatorial LibrariesDrug discovery using high-throughput screening of discreet compounds, and the discovery of natural products with pharmacological mechanisms of action, rely on bioassay-guided fractionation analysis. Recent applications of affinity selection–mass spectrometry (AS-MS) are useful for exploring the discovery of ligands to membrane-bound proteins and RNA targets.
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Top-Down Mass Spectrometry of Intact Proteins and Complexes: From Rare to RoutineIn recent years, top-down mass spectrometry has quickly advanced from academic rarity to (near-) routine. How did we get here? And what can we expect in the near future?
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Development of a “Freeze-Pour” Sample Preparation Method for the GC Analysis of Semivolatile Flavouring Chemicals Present in E-cigarette Refill LiquidsHS-GC analysis is presented as an excellent method for the analysis of high volatile components in e-liquids. For the analysis of semivolatile ingredients, an additional sample preparation step is proposed based on a LLE followed by a freeze-out of the matrix components.
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Development of a Standardized Protocol for the Classification of Column Sets in Comprehensive Two-Dimensional Gas ChromatographyThe article discusses the classification and characterization of GC×GC column sets based on polarity and orthogonality, introducing a standardized approach using a reference mixture called the Century Mix to evaluate the selectivity and performance of these column sets.
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Methods for the Passivation of HPLC Instruments and ColumnsNonspecific adsorption leads to poor peak shapes and poor performance from HPLC systems, but coating-enabling technologies can serve as a potential solution. We explain how.
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In-Loop Analyte Degradation in Two-Dimensional Liquid Chromatography: Example and SolutionsIn this installment of “LC Troubleshooting,” we describe an artifact that can arise because of compound degradation during the transfer of fractions of the first dimension (1D) column effluent to the 2D separation.
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The Effects of Inner Surface Roughness of Microbore Column Blanks on Column PerformanceThe efficiencies of microbore-2 columns, which are prepared from blanks that have a wide variety of inner surface roughness, drop sharply when the size of individual surface roughness features approaches the particle size of the packing material. The results suggest that two categories of packed column structure relate to the surface features and yield high and low efficiency columns. This installment of "Column Watch" discusses this conclusion in terms of the stability of an agglomerated layer of packing particles on the blank wall when subjected to shear forces during column packing.
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Acid-Catalyzed Isomerization of Carbonyls-2,4- dinitrophenylhydrazone in Mainstream Smoke of Heat-Not-Burn Tobacco Product for HPLC AnalysisErrors arising from the DNPH approach commonly used to analyze carbonyl compounds in smoke from heat-not-burn (HNB) tobacco can be avoided by using the approach described in this study.
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Optimal Separation of Polar Anionic Pesticides from Fruits and Vegetables with HPLC Column SelectivityThis article presents a new column technology that uses reversed phase separation and offers excellent peak shape, resolution, and robustness for a wide variety of food matrices.
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Online Solid-Phase Extraction–Gas Chromatography–Flame Ionization Detection System for Monitoring Contaminants at Parts-Per-Trillion Concentrations in Process WatersOnline monitoring of odour and taste components that occur at parts-per-trillion (ppt) levels in industrial process waters requires specialized analytical hardware that is generally not compatible with the harsh environmental conditions in these typical industrial settings. An alternative instrumental method is proposed that uses dynamic extraction in combination with gas chromatography (GC) equipped with a simple flame ionization detector (FID) to achieve these extremely low detection limits.
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A Suitable Therapeutic Drug Monitoring Method for Amoxicillin in Plasma by High Performance Liquid Chromatography–UV (HPLC–UV) in NeonatesThis simple, rapid, and accurate HPLC-UV method can facilitate routine therapeutic drug monitoring in neonates.
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Cannabis Metabolomic Data Processing: Challenges to be AddressedThe challenges that arise during cannabis metabolomics analysis using ultrahigh-performance reversed-phase liquid chromatography coupled with high-resolution tandem mass spectrometry (UHPLC–reversed-phase–HRMS/MS) are presented.
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Identification of Microplastics in Environmental Monitoring Using Pyrolysis–GC–MS AnalysisPyrolysis–gas chromatography–mass spectrometry has advantages for the analysis of environmental microplastic samples compared to other leading analytical methods, including spectroscopic techniques.
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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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Determination of Polychlorinated Biphenyls in Water Samples Using a Needle Trap Device Combined with Gas ChromatographyThe method presented here, which uses a novel needle trap device (NTD) with sol-gel PEG-coated fibers in conjunction with GC, is a simple, inexpensive, and accurate tool for the analysis of trace levels of PCBs in water samples.
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Electromembrane Extraction with Vials of Conducting PolymerIn electromembrane extraction (EME), the target analyte is extracted from an aqueous sample across a supported liquid membrane (SLM) and analyzed using LC. Through the study presented here, we demonstrate the principles of the technique and test its performance.
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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 Utilizing 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.
