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Determination of Corrosion Inhibitor–Lubricity Improver in Jet Fuels by Liquid Chromatography–Electrospray Ionization Mass SpectrometryMilitary jet fuel (JP-8) is very similar to commercial jet fuel (Jet A) except for the presence of three additives, fuel system icing inhibitor, corrosion inhibitor–lubricity improver (CI-LI), and antistatic additive, which are added to improve characteristics of JP-8.
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Determination of Fipronil and Its Metabolites in Eggs and Environmental Matrices by LC–MS/MSAn improved LC–MS/MS method that can rapidly detect fipronil, an insecticide harmful to human health, is presented here for chicken eggs, feed, and soil.
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Racing Against Time: High-Throughput Analysis of Dermorphin in Equine UrineThis article examines the problem of dermorphin doping in horse racing and presents an effective method for its detection using LC–MS TQ.
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A Proactive Approach to Reference Material Production for New Psychoactive SubstancesThis article discusses the novel legal highs that appear on the market and how forensic laboratories work to keep ahead of the game.
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Practical Tips on Preparing Plasma Samples for Drug Analysis Using SPMEThis month's guest authors review the application of solid-phase microextraction (SPME) to the analysis of drugs in human plasma discussing important factors in the optimization of extraction efficiency. The column concludes with a discussion of method validation issues.
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A Multimodal Liquid and Supercritical Fluid Chromatography Chiral Separation Screening and Column Maintenance Strategy Designed to Support Molecules in Pharmaceutical Development (Part 1)Chiral separation screening has become a widely accepted approach for the rapid identification of an appropriate chiral stationary phase for use in more focused enantioseparation optimization. A set of extended screens encompassing various chromatographic modes using HPLC and SFC is presented.
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LC–MS Identification of Wax Esters in Cloudy Canola OilCanola largely contains unsaturated fatty acids, thus rendering it clear in most cases after extraction and refining.
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A New Method for Quality by Design Robust Optimization in Liquid ChromatographyA new method to optimize liquid chromatography (LC) methods using a Quality by Design (QbD) approach is presented. This method is based on the use of design of experiments (DOE) and independent component analysis (ICA) to accurately estimate the modeled responses (that is, the retention times at the beginning, the apex, and the end) of each peak, even for coeluted peaks. This method was applied to the optimization of the separation of nine compounds in a mixture, yielding the design space and the demonstration of robustness of the method.
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Micellar Liquid Chromatography: How to StartMicellar liquid chromatography (MLC) is a reversed-phase liquid chromatographic mode with a solution of surfactant forming micelles as the mobile phase. The interaction of solutes with the stationary phase coated with surfactant monomers, combined with the increased solubilization capability of micelles, have profound implications with regard to retention, selectivity and efficiency. Practical steps that a chromatographer involved in MLC should consider when developing an analytical procedure are described, including mobile phase preparation, column conditioning and cleaning.
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Rapid and Direct Quantitation of Pharmaceutical Drugs from Urine Using MALDI-MSAn application of MALDI-MS in qualitative and quantitative analysis of pharmaceutical compounds spiked in urine is demonstrated.
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Analysis of Four Phthalate Monoesters in Human Urine Using Liquid Chromatography Tandem Mass SpectrometryA fast, sensitive and accurate quantitative method was developed using HPLC–MS–MS for analysis of phthalate metabolites in urine samples.
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Applying LC with Low-Resolution MS/ MS and Subsequent Library Search for Reliable Compound Identification in Systematic Toxicological AnalysisSystematic toxicological analysis is an important step in medicolegal investigations of death, poisoning, and drug use. The primary goal is the detection and confirmation of potentially toxic compounds in evidence. This article describes a workflow using nontargeted liquid chromatography–tandem mass spectrometry (LC–MS/MS) for reliable compound identification.
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Determination of Halogens and Sulphur in Complex MatricesThis article presents a method that combines combustion digestion and ion chromatography into a single analysis (combustion ion chromatography [CIC]) making it possible to detect halogens and sulphur in complex matrices. The method is suitable for use in a wide range of application areas.
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Analysis of Rare Sugars Using ShodexTM HILICpakTM VG-50 4EThis application note demonstrates how the use of DCM in particular had a dramatic effect on the separation and afforded conditions that could be further adapted to a preparative scale application.
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The Inert Flow Path Story for GC and GC–MS: Eliminating the Weakest LinksFor the next improvements, we must look beyond the column.
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Evaluation of Retention and Selectivity Using Biphenyl Stationary PhasesIn reversed-phase liquid chromatography (LC), C18 alkyl-based stationary phases have been the favourite of method developers. Phenyl stationary phases are an alternative that are thought to benefit from additional π-π mechanisms. Recently, there has been a growing interest in the use of phases based on the biphenyl moiety. This instalment of “Column Watch” looks at the retention mechanisms of biphenyl phases and contrasts them with those of more-common alkyl phases.
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Efficient Quantitation of Biotherapeutics in Biological Matrices Through the Application of LC–MS‑Related TechniquesBiotherapeutics must endure in-depth testing to validate their efficacy and safety before their release to the medical community. Characterization and quantitation of these large molecule medicines is traditionally performed with ligand binding assays or radiolabeling procedures. Issues with selectivity, accuracy, and unavailability of applicable assays for the characterization and quantitation of certain biotherapeutics means that liquid chromatography–mass spectrometry (LC–MS) is becoming an increasingly selected method for biotherapeutics testing. Typically used for small molecules, LC–MS can be adapted for larger molecule analysis with additional high throughput and multiplexing capabilities. New method development has turned LC–MS into a highly sensitive option for biotherapeutics validation.
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Application of Pyrolysis–Gas Chromatography–Mass Spectrometry for the Identification of Polymeric MaterialsThe pyrolysis–GC–MS method enables direct analysis of solid or liquid polymers without sample pretreatment, as illustrated here for various materials, including a dental filling material and a car wrapping foil.
Latest:
A Multimodal Liquid and Supercritical Fluid Chromatography Chiral Separation Screening and Column Maintenance Strategy Designed to Support Molecules in Pharmaceutical Development (Part 1)Chiral separation screening has become a widely accepted approach for the rapid identification of an appropriate chiral stationary phase for use in more focused enantioseparation optimization. A set of extended screens encompassing various chromatographic modes using HPLC and SFC is presented.
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Agilent Bio-Monolith Protein A Monitors Monoclonal Antibody Titer from Cell CulturesAgilent Technologies
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Online Ion-Exchange Solid-Phase Extraction Cleanup for PFAS in Food of Animal OriginOnline SPE–LC–MS/MS combined with the method presented enabled automated cleanup of food extracts and determination of PFAS compounds in the ng/kg range.
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Morphological Comparison of Silica-Based Monolithic and Particulate Beds by Confocal Laser Scanning MicroscopyThis analysis offers insight for optimizing the structure of monoliths.
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Optimizing SEC for Protein CharacterizationThe ability of size-exclusion chromatography (SEC) to measure critical protein characteristics, such as molecular weight and size, makes the technique valuable from the early stages of novel protein research and development through to formulation and manufacturing support, especially in oligomeric purity and aggregation studies. However, informational output, ease of analysis, and sample requirements all vary considerably depending on whether a system has been truly optimized for protein characterization. This article examines how SEC works and considers how to maximize the productivity, sensitivity, and value of an SEC setup for biopharmaceutical development.
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Practical and Popular Sample Preparation Techniques for Ion ChromatographyThe authors present the most common and fundamental techniques that address common matrix issues and discuss the critical chemistry considerations.
