As 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.
This 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.
The experts conclude the panel by addressing additional regulatory challenges and exploring how the industry can collaborate to tackle these issues moving forward.
Adhesives often contain toxic materials like residual monomers; here, we demonstrate quantitative analysis of residual monomers in adhesives using GC–MS.
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Examples from food science illustrate the usefulness of chemometrics techniques like pattern recognition, regression, and classification.
This 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.
Biogen 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.
As 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.
New gene therapy modalities, such as CRISPR guide RNA (single guide ribonucleic acid [sgRNA]) and messenger RNA (mRNA), continue to make progress in both primate and first-in-human trials. As this progress builds, the industry remains accountable for characterizing these molecules to meet the requirements of regulatory authorities.
A 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.
A 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.
The authors describe a method of reductive chlorination that enables the determination of total PCB content by gas chromatography with flame ionization detection.
Quantification 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.
A 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.
In 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.
This 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.
The guest authors summarize the history of this Japanese scientific instrument company and events in the development of its products.
An unexpected retention order for ketamine analogs was observed when using a biphenyl stationary phase for liquid chromatography-mass spectrometry (LC–MS).
An overview of different approaches for the qualitative and quantitative analysis of polysorbates.
A 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.
The 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).
In 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.
Extra 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.
A rapid LC–MS method using ESI coupled with SIM-MS for analysis of humulone and isohumulone content in beer is described.
Untargeted GC–MS metabolomics with sample derivatization is shown here to be effective for measuring the chemical profiles of traditional and plant-based meat products.
Low-pressure gas chromatography (LPGC)–MS should be the first option in many GC–MS applications to provide fast, sensitive, and robust analyses; and the installation, instrumentation, and implementation of LPGC is possible in any GC–MS system.
A novel liquid chromatography–tandem mass spectrometry (LC–MS/MS) method with a dual electrospray ionization (ESI) and atmospheric-pressure chemical ionization (APCI) source was developed for analysis of 66 pesticides and 5 mycotoxins regulated by the State of California in medium-chain triglyceride (MCT) oil cannabis tinctures. The limits of quantitation (LOQs) of all of the pesticides and mycotoxins were well below California state action limits of these analytes in cannabis-based non-inhalable or edible products. A total of 62 (out of 66) pesticides and 5 mycotoxins were analyzed using LC–MS/MS with an ESI source, and the remaining 4 pesticides were determined using LC–MS/MS with an APCI source. A simple, fast, and cheap acetonitrile solvent extraction method was used for sample preparation to get good recovery and achieve high throughput for this analysis. For late-eluted analytes, a number of internal standards were used to compensate for ion suppression effects from the hydrophobic matrix.
Better sample preparation and miniaturized separations are enhancing these analyses.
This application demonstrates the LC-MS/MS analysis of 46 PFAS and 25 surrogate compounds in solid matrices using a newly developed, cost-effective workflow.