Nuclear Magnetic Resonance Spectrometry Combined with Chemometric Methods of Data Processing as a Method for the Study of the Composition and Properties of Heparin Preparations
- Authors: Monakhova Y.B.1,2,3, Rubtsova E.M.1, Diehl B.W.3, Mushtakova S.P.1
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Affiliations:
- Institute of Chemistry, Saratov State University
- Institute of Chemistry, St. Petersburg State University
- Spectral Service AG
- Issue: Vol 74, No 9 (2019)
- Pages: 945-953
- Section: Articles
- URL: https://journals.rcsi.science/1061-9348/article/view/183312
- DOI: https://doi.org/10.1134/S1061934819090065
- ID: 183312
Cite item
Abstract
The composition and properties of heparin preparations are studied by NMR spectrometry. Approaches to the determination of the most important heparin quality indicators (biological origin and manufacturing company) based on multivariate modeling of the NMR profile of a sample are considered. Chemometric modeling of two-dimensional (2D) NMR spectra (DOSY, HSQC, HMBC) by the principal component and discriminant analysis is performed to increase the efficiency of analysis. Multivariate regression models (partial least squares) are built for the first time to determine the average molecular weight of heparin. Quantitative NMR spectrometry is applied to the determination of water, calcium and sodium cations, and also chloride and acetate anions in heparin preparations. The determination of all characteristics requires five consecutive measurements by NMR (1H, 2D, 35Cl, 23Na, and 2D DOSY) spectrometry and one sample preparation. The duration of analysis of one sample, including measurements and signal processing, takes no more than 20 min. The proposed approach is universal and can be used in the analysis of other medicinal preparations.
Keywords
About the authors
Yu. B. Monakhova
Institute of Chemistry, Saratov State University; Institute of Chemistry, St. Petersburg State University; Spectral Service AG
Author for correspondence.
Email: yul-monakhova@mail.ru
Russian Federation, Saratov, 410012; St. Petersburg, 199034; Cologne, 50996
E. M. Rubtsova
Institute of Chemistry, Saratov State University
Email: yul-monakhova@mail.ru
Russian Federation, Saratov, 410012
B. W. K. Diehl
Spectral Service AG
Email: yul-monakhova@mail.ru
Germany, Cologne, 50996
S. P. Mushtakova
Institute of Chemistry, Saratov State University
Email: yul-monakhova@mail.ru
Russian Federation, Saratov, 410012