Similarity analysis of the phenolic fingerprints of a large number of aqueous extracts of Cyclopia subternata, obtained by high-performance liquid chromatography (HPLC), was evaluated as a potential tool to screen extracts for relative bioactivity. The assessment was based on the (dis)similarity of their fingerprints to that of a reference active extract of C. subternata, proven to enhance glucose uptake in vitro and in vivo. In vitro testing of extracts, selected as being most similar (n = 5; r ≥ 0.962) and most dissimilar (n = 5; r ≤ 0.688) to the reference active extract, showed that no clear pattern in terms of relative glucose uptake efficacy in C2C12 myocytes emerged, irrespective of the dose. Some of the most dissimilar extracts had higher glucose-lowering activity than the reference active extract. Principal component analysis revealed the major compounds responsible for the most variation within the chromatographic fingerprints, as mangiferin, isomangiferin, iriflophenone-3-C-β-D-glucoside-4-O-β-D-glucoside, iriflophenone-3-C-β-D-glucoside, scolymoside, and phloretin-3',5'-di-C-β-D-glucoside. Quantitative analysis of the selected extracts showed that the most dissimilar extracts contained the highest mangiferin and isomangiferin levels, whilst the most similar extracts had the highest scolymoside content. These compounds demonstrated similar glucose uptake efficacy in C2C12 myocytes. It can be concluded that (dis)similarity of chromatographic fingerprints of extracts of unknown activity to that of a proven bioactive extract does not necessarily translate to lower or higher bioactivity.
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J Chromatogr A
January 2025
National Institute of Oceanography and Fisheries, NIOF, Cairo, Egypt. Electronic address:
The comprehensive identification of peaks in untargeted lipidomics using LC-MS/MS remains a significant challenge. Confidence in lipid annotation can be greatly improved by integrating a highly accurate machine learning-based retention time prediction model. Such an approach enables the identification of lipids for understanding pathogenic mechanisms, biomarker discovery, and drug screening.
View Article and Find Full Text PDFJ Chem Inf Model
January 2025
School of Pharmaceutical Sciences, Zhejiang Chinese Medical University, Hangzhou 310053, People's Republic of China.
Proteolysis-targeting chimeras (PROTACs) are heterobifunctional molecules that target undruggable proteins, enhance selectivity and prevent target accumulation through catalytic activity. The unique structure of PROTACs presents challenges in structural identification and drug design. Liquid chromatography (LC), combined with mass spectrometry (MS), enhances compound annotation by providing essential retention time (RT) data, especially when MS alone is insufficient.
View Article and Find Full Text PDFCrit Rev Anal Chem
January 2025
Department of Inorganic Chemistry, Analytical Chemistry and Electrochemistry, Faculty of Chemistry, Silesian University of Technology, Gliwice, Poland.
Pesticides are commonly found in plant-based foods, which inevitably reduces food quality and poses significant health risks to consumers. The extensive variety of crops and the wide range of pesticides used means that no single analytical approach can provide clear and comprehensive information on the pesticide-protection status of a crop. Since most pesticide analyses in food rely on chromatographic techniques combined with various MS platforms, this article focuses exclusively on LC-MS and GC-MS system methodologies.
View Article and Find Full Text PDFJ Sep Sci
January 2025
Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, Shijiazhuang, China.
A novel dual-wavelength ultrahigh performance liquid chromatography (UHPLC) fingerprint was established, 56 common peaks were confirmed and attributed to the source of the medicinal materials, and 13 chromatographic peaks of them were identified by UHPLC quadrupole time-of-flight (Q-TOF)-MS/MS and UHPLC-UV method. Furthermore, a simple and sensitive HPLC-quadrupole trap (Q-TRAP)-MS/MS was developed for the simultaneous determination of 16 active components with electrospray ionization (ESI) source switching between positive and negative modes in a single run. The above two methods were successfully applied for the quality evaluation of Guanxinjing capsule (GXJC).
View Article and Find Full Text PDFACS Omega
December 2024
Department of Chemistry, Humboldt Universität zu Berlin, Brook-Taylor-Str. 2, Berlin 12489, Germany.
In this study, we extended a previously developed one-pot double derivatization reaction to establish the first routine isotope-coded multiplex derivatization for vitamin D and its metabolites for application in clinical environments, using commercial reagents, without the need for specialized reagents and advanced synthesis requirements. The original derivatization process consisted of using both a Cookson-type reagent and derivatization of hydroxyl groups. Initially, the analytes are derivatized by a Diels-Alder reaction using 4-phenyl-1,2,4-triazoline-3,5-dione (PTAD), followed by acetylation using acetic anhydride, catalyzed by 4-dimethylaminopyridine at room temperature.
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