We report the use of band-selective 2D HSQC NMR spectroscopy to rapidly determine the stereoregularity of polymers usually analyzed by 1D C NMR spectroscopy. This approach reduced the time required to characterize the triad stereosequences of polyacrylonitrile from about an hour to a few minutes, and can be performed with sufficient C resolution to resolve higher-order stereosequences, such as the pentads of polypropylene.
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http://dx.doi.org/10.1021/acsmacrolett.5b00866 | DOI Listing |
ACS Omega
June 2024
National Institutes for Food and Drug Control, Beijing 102629, P.R. China.
Tripterygium glycoside tablets (TGTs) are preparations extracted and purified from Hook. F and are extensively utilized in the treatment of autoimmune diseases, such as rheumatoid arthritis (RA). However, variations in production processes among manufacturers can lead to challenges in quality control and clinical utilization of TGTs.
View Article and Find Full Text PDFMetabolomics
December 2023
Division of Biological and Environmental Sciences and Engineering (BESE), Smart-Health Initiative (SHI) and Red Sea Research Center (RSRC), King Abdullah University of Science and Technology (KAUST), Thuwal, Makkah, 23955-6900, Saudi Arabia.
Introduction: Nuclear Magnetic Resonance (NMR) spectroscopy stands as a preeminent analytical tool in the field of metabolomics. Nevertheless, when it comes to identifying metabolites present in scant amounts within various types of complex mixtures such as plants, honey, milk, and biological fluids and tissues, NMR-based metabolomics presents a formidable challenge. This predicament arises primarily from the fact that the signals emanating from metabolites existing in low concentrations tend to be overshadowed by the signals of highly concentrated metabolites within NMR spectra.
View Article and Find Full Text PDFAnal Chim Acta
September 2023
National Institutes for Food and Drug Control, Beijing, 102629, PR China. Electronic address:
Sesquiterpene pyridine alkaloids (SPAs) are bioactive analogues derived from the genus Tripterygium and have anti-inflammatory and anti-rheumatic properties. Attributed to the similar sesquiterpene structures, the total SPAs showed severe peak overlap in 1D NMR and HPLC, leading to difficulties in identification and quantification. Interestingly, the application of band-selective HSQC NMR that specifically excited the region corresponding to the H-3 of SPAs prompted a signal separation of the total SPAs.
View Article and Find Full Text PDFMolecules
May 2023
Institute of Meteria Medica, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100050, China.
The quality of products available in the market is threatened by adulteration with different species, such as (), (), and (). In this paper, we established a 2D band-selective heteronuclear single quantum coherence (bs-HSQC) NMR method to discriminate species and detect adulteration of . The method involves selective excitation of the anomeric carbon resonance region of saponins and non-uniform sampling (NUS) to obtain high-resolution spectra in less than 10 min.
View Article and Find Full Text PDFMolecules
October 2022
Pharmazeutisches Institut, Abteilung Pharmazeutische und Medizinische Chemie, Christian-Albrechts-Universität zu Kiel, Gutenbergstraße 76, 24118 Kiel, Germany.
In the present work, a two-dimensional qNMR method for the determination of sennosides was established. Using band-selective HSQC and the cross correlations of the characteristic 10-10' bonds, we quantified the total amount of the value-determining dianthranoids in five minutes, thus, rendering the method not only fast, but also specific and stability indicating. The validation of the method revealed excellent accuracy (recovery rates of 98.
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