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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-MSPharmaceutical 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>.
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Exploring Capillary Electrophoresis–Mass Spectrometry for the In-Depth Intact Native Analysis of Cysteine-Conjugated Antibody-Drug ConjugatesThis 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.
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Book Review: Practical Application of Supercritical Fluid Chromatography for Pharmaceutical Research and DevelopmentWhy is SFC becoming increasingly more important as a sustainable analytical technique?
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New Sample Preparation Approaches to Biological Matrices for LC–MSCurrent sample preparation procedures for LC–MS as applied to samples from biological matrices.
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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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Analyzing the Light of the FutureA novel analytical method for the analysis of OLED materials using SFC is presented.
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Chromatographic Isolation of Sensitive Compounds: Challenges and SolutionsIn this installment of “LC Troubleshooting,” we discuss strategies that can be used to minimize the likelihood of compound degradation in the isolation process.
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A Simple LC–MS Multi-Analyte Method to Determine Food Additives and Caffeine in BeveragesA simple LC–MS method has been developed and validated for the simultaneous determination of 18 synthetic food additives and caffeine in soft and energy drinks, and in various alcoholic beverages. Nine food colours (tartrazine, sunset yellow FCF, azorubine, ponceau 4R, allura red AC, patent blue V, brilliant blue FCF, green S, brilliant black BN), two preservatives (sorbic and benzoic acid) and seven sweeteners (acesulfame K, aspartame, cyclamic acid, saccharin, sucralose, neohesperidin DC, neotame) were targeted food additives. The method employs reversed-phase ultra-high performance liquid chromatography (UHPLC) for analyte separation and a single quadrupole mass spectrometer for their detection. The limits of quantification were low enough to enable a reliable control of maximum limits set for some additives (Regulation [EC] No. 1333/2008). The method was applied for analysis of a wide range of samples collected at a typical supermarket: 14 soft drinks, 19 energy drinks, and 43 alcoholic beverages.
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Combined Chromatographic and Spectrometric Approaches for Cleaning Verification of Small-Molecule Pharmaceutical Compounds in the Manufacturing EnvironmentWe assess recent advances in cleaning verification methods for small-molecule pharmaceuticals, and propose a workflow.
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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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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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Novel Sorptive Sample Preparation Techniques for Separation ScienceA recent intercontinental collaboration between two academic research laboratories—the Aristotle University of Thessaloniki, Greece, and the Florida International University, USA—has yielded a significant number of analytical/bioanalytical methods using fabric phase sorptive extraction (FPSE), magnet integrated fabric phase sorptive extraction (MI-FPSE), and capsule phase microextraction (CPME) for the isolation of various analytes from different complex sample matrices.
