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Exploring the Implementation of Compact Chromatographic Instrumentation in Common Analytical WorkflowsCompact instrumentation offers important advantages for many workflows, as illustrated by these examples.
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Moving Toward Green and Sustainable Sample PreparationMicroextraction techniques have evolved since their appearance three decades ago, moving toward the use of greener and sustainable materials and solvents.
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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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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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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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A Review of MOSH and MOAH Analysis in FoodAn overview of the analytical approaches proposed, from sample preparation to the final chromatographic determination, for the reliable risk assessment of mineral oil hydrocarbon (MOH) contaminants in food. The analysis of these contaminants in food is a challenging task and requires a comprehensive approach to tackle the cumbersome issues related to their determination.
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Efficient Pesticide Residue TestingThis application note describes the benefits of automated gravimetric liquid dispensing compared to traditional manual stock solution preparation in a volumetric flask.
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Leveraging an Enterprise Laboratory Informatics Platform to Maximize Scientific Data AdvantageAs data volumes and expectations for fast scientific discovery continue to increase, laboratory-based research organizations can no longer rely on a siloed approach to data management. To remain competitive, scientific organizations need to connect all their data, from discovery through manufacturing, in a unified informatics platform.
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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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Simultaneous Determination of 17 Residual Monomers in Adhesives by Gas Chromatography–Mass SpectrometryAdhesives often contain toxic materials like residual monomers; here, we demonstrate quantitative analysis of residual monomers in adhesives using GC–MS.
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Enter the Matrix: Improving the Interpretation of Separations Data Using Chemometrics in Analytical InvestigationsExamples from food science illustrate the usefulness of chemometrics techniques like pattern recognition, regression, and classification.
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Quantitative Analysis of PFAS in Milk, Infant Formula, and Related Ingredients Using LC–MSThis method for PFAS analysis in milk and infant formula is robust, reliable, and reproducible, with scope to expand the list of PFAS in the future.
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Postnova - Separation and Sizing of a Virus Mixture Using Asymmetrical Flow Field‐Flow Fractionation Coupled to Multi‐Angle Light ScatteringBiogen and Postnova present data on the analysis of adeno-associated viruses (AAV) using Asymmetrical Flow Field-Flow Fractionation coupled to Multi-Angle Light Scattering detection (AF4-MALS). AAV are promising gene therapy delivery vehicles, whose efficacy may be negatively affected by the presence of viral aggregates. Due to its gentle separation and broad applicable size range, AF4-MALS is able to characterize AAV and their aggregates with high resolution and precision, thereby overcoming the drawbacks that column-based chromatography techniques often face when dealing with samples larger than 50 nm in size.
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Leveraging an Enterprise Laboratory Informatics Platform to Maximize Scientific Data AdvantageAs data volumes and expectations for fast scientific discovery continue to increase, laboratory-based research organizations can no longer rely on a siloed approach to data management. To remain competitive, scientific organizations need to connect all their data, from discovery through manufacturing, in a unified informatics platform.
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Untargeted LC–MS Lipidomics with Data Independent Acquisition using Sequential Window Acquisition of All Theoretical Fragment-Ion SpectraA focus on untargeted UHPLC–MS/MS lipidomics with data independent acquisition using SWATH technology. This article explores the wide-ranging potential and peculiarities of SWATH–MS hyphenated with UHPLC for the profiling of lipidomes of various biological samples.
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A Novel Mass Spectrometry Paradigm to Analyze Classical and New Biotherapeutic ModalitiesA new fragmentation approach—tunable electron-activated dissociation (EAD) tandem mass spectrometry (MS/MS)—offers a solution to better improve the detection and characterization of impurities in lipid nanoparticles and impurities in other biopharmaceutical modalities.
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Total Polychlorinated Biphenyl Quantification by Rapid Dechlorination Under Mild ConditionsThe authors describe a method of reductive chlorination that enables the determination of total PCB content by gas chromatography with flame ionization detection.
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Stability and Recovery Influences of Benzo[a]pyrene, Benzo[a]anthracene, Benzo[b]fluoranthene, and Chrysene during Sample Preparation of Plant MatricesQuantification of European Union (EU)-priority polycyclic aromatic hydrocarbons (PAHs) in plant matrices is a crucial task. Various methods for enrichment and preconcentration, such as the preloaded-pipette tip solid‑phase extraction (SPE) (1), are available. Nevertheless, analyte recovery as a result of homogenization, sample preparation, and extraction are rarely discussed in the field of phytopharmacy. This study deals with the recovery in dry plant extracts, which are typically used in phytopharmaceuticals and reflect the actual polycyclic aromatic hydrocarbon content in the commercially available end product (2). The aim of this study was to monitor benzo[a]pyrene, benzo[a]anthracene, chrysene, and benzo[b]fluoranthene loss of spiked samples as a result of commonly-used sample pretreatment, extraction, filtering, and evaporating techniques in 1:1 (v/v) cyclohexane–ethyl acetate primulae flos and sambuci flos dry extracts. Results showed that improper sample preparation can lead to false results. In the case of benzo[a]pyrene with a deviation of 155% from the theoretical true value.
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Technical Note: Modifying a Standard HPLC Autosampler for On-Line Process MonitoringA simple modification of the standard HPLC autosampler flow path enables automated sampling and analysis of samples outside the autosampler unit when users cannot place the sample container inside because of size restrictions.
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Analysis of Organophosphorus Pesticides by HPLC Using Magnetic SPE with Nitrogen-Doped Reduced Graphene Oxide/Fe3O4 Nanocomposite as the AdsorbentIn this study, a method was developed for extraction and preconcentration of trace amounts of organophosphorus pesticides (OPPs), including fenitrothion, chlorpyrifos-methyl, and chlorpyrifos in environmental water.
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Chromatographic Attractions at Analytica 2022This year, Messe Munchen is hosting the world’s leading trade fair for laboratory technology, analysis, and biotechnology live and in person. The conference will take place 21–24 June 2022 in Munich, Germany. Here is a snapshot of what chromatographers can look forward to.
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Development of Gas Chromatography Instruments at ShimadzuThe guest authors summarize the history of this Japanese scientific instrument company and events in the development of its products.
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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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Polysorbate Analysis in Biopharmaceutical Applications—A Snapshot of the Analytical ToolboxAn overview of different approaches for the qualitative and quantitative analysis of polysorbates.
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Rapid Simultaneous Determination of Five Major Alkaloids from Menispermi Rhizoma in Rat Urine by Ultrahigh-Pressure Liquid Chromatography– Tandem Mass Spectrometry (UHPLC–MS/MS) and its Application to a Urinary Excretion StudyA UHPLC–MS/MS method is described for rapid quantification of five major bioactive alkaloids in rat urine. The results obtained help lay the foundation for the clinical application and safety evaluation of the bioactive ingredients of menispermi rhizoma, used in herbal medicines.
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Analysis of MCPD and Glycidyl Fatty Acid Esters in Refined Plant Oils by Supercritical Fluid Chromatography– High-Resolution Mass SpectrometryThe aim of this study was to develop an efficient method to enable a rapid determination of nine 3-MCPDEs and seven GEs in vegetable oils within a single run employing supercritical fluid chromatography coupled to high-resolution tandem mass spectrometry (SFC–HRMS/MS).
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Where Has My Efficiency Gone? Impacts of Extracolumn Peak Broadening on Performance, Part 4: Gradient Elution, Flow Splitting, and a Holistic ViewIn this instalment, we focus on the impact of elution mode (isocratic or gradient) and postcolumn flow splitting on the total level of extracolumn dispersion (ECD) in a liquid chromatography (LC) system, and demonstrate the use of a free, web-based calculator that can be used to guide decision making aimed at reducing ECD during method development.
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Turn Down the VolumeExtra column volume is the volume in an HPLC system external to the column that contributes to the total peak volume, which will impact peak width, resolution, and overall efficiency.
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Liquid Chromatography–Mass Spectrometry Analysis of Hop-Derived Humulone and Isohumulone Constituents in Beer: The Bitter Truth of Hops Utilization During BrewingA rapid LC–MS method using ESI coupled with SIM-MS for analysis of humulone and isohumulone content in beer is described.
