This article introduces optimization of the two separate standard methods, BS148:2009 and ASTM D5837-15, to offer simultaneous analysis in one assay.
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.
This application note demonstrates the use of Thermal Desorption as greener approach for sampling of terpenes in air for workplace exposure or terpene profiling
This article highlights an advantage of porous graphitic carbon columns, that is their resistance at high temperatures, for the analysis of parabens in foodstuffs.
This application notes showcases greener HPLC with less solvent using smaller inner diameter columns while maintaining the quality of separation
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.
Pepsin digestion and guanidine hydrochloride post-digestion can improve sequence coverage in antibody peptide mapping compared with trypsin digestion.
When should multidimensional GC approaches be used for analyzing complex samples and analytes?
Sustainability concerns are renewing interest in SFC, often as a substitute for HPLC. With the broader application of SFC, we need a better understanding of selectivity in SFC, where stationary phase classification is not well established. This study assessed and measured the selectivity differences afforded by three prototype SFC phases.
Commercially available trypsin IMERs can digest proteins with high sequence coverage and robustness, facilitating online multidimensional LC–MS.
We assess recent advances in cleaning verification methods for small-molecule pharmaceuticals, and propose a workflow.
The current challenges and future perspectives of the purification of cannabinoids from cannabis extracts are presented in this review article.
HS-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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Online 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.
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.
Integrating electric fields into extraction techniques increases sensitivity and selectivity. These approaches are compatible with miniaturized, portable, and many biological samples.
The study of the thermal behaviour and pyrolysis products of these terpenoids could possibly suggest flavour precursors that could be used to provide specific flavours to tobacco.
The success of screening column and mobile phase combinations that generate dissimilar selectivity is highlighted in a typical method development strategy.
Long chain fatty acids (LCFAs) function as a source of metabolic energy, substrates for membrane biogenesis, and storage of metabolic energy. Oxylipins, oxygenated derivatives of LCFAs, regulate the activity of many cellular processes. Existing methods for the analysis of LCFAs and oxylipins have limited compound coverage and sensitivity that, therefore, prevent their application in biological studies. In this work, we developed a high-throughput LC–MS method for analysis of 51 LCFAs and oxylipins. LCFAs and oxylipins were first extracted from biological samples via solid-phase extraction. The extracted molecules were analyzed by targeted comparative metabolomics. Saturated and monounsaturated LCFAs were analyzed in single ion reaction mode, while polyunsaturated LCFAs and oxylipins were analyzed in multiple reaction monitoring mode. Using this method, we successfully quantified 31 LCFAs and oxylipins from mouse livers.
This month's "Directions in Discovery" gives a brief overview of turbulent- flow liquid chromatography, a technique for fast separations. Two examples demonstrate the use of the technology for high-throughput bioanalytical separations in drug discovery.
This review article summarizes the results obtained from the combined efforts of a joint academic and industrial initiative to solve the real-life challenge of determining low levels of peptide-related impurities in the presence of the related biologically-active peptide at a high concentration.
A generalized approach using DoE is presented for the optimization of DHS extraction parameters.
What experimental details need to be considered when analyzing PEGs?
This simple, rapid, and accurate HPLC-UV method can facilitate routine therapeutic drug monitoring in neonates.
Displacement chromatography is a viable alternative to elution chromatography, but the biotechnology industry has yet to fully exploit this technique. The authors present results of a pilot-scale ion-exchange displacement process developed for the removal of variants from recombitant human brain-derived neutrotrophic factor.
Per- and poly-fluoroalkyl substances (PFAS) are a family of potentially thousands of synthetic compounds that have long been used in the manufacture of a variety of common products with stain-repellent and nonstick properties. Their signature strong fluorine and carbon bonds make them difficult to break down and, as a result, they are among the most persistent of today’s environmental pollutants. Alarmingly, PFAS can be found in drinking water and have been shown to accumulate in the body with the potential to cause multiple health problems, such as hormone disruption and cancer. Advances in mass spectrometry have facilitated the detection of known PFAS contaminants as well as the identification of poorly studied and novel compounds in watersheds. This article explores the detection of known and novel PFAS contaminants in aqueous film-forming foams and raw drinking water sources in North Carolina, using new advances in mass spectrometry and data acquisition to improve identification and quantitation.
Better sample preparation and miniaturized separations are enhancing these analyses.
The 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.