TY  - JOUR
A1  - Monakhova, Yulia
A1  - Diehl, Bernd W.K.
T1  - Nuclear magnetic resonance spectroscopy as an elegant tool for a complete quality control of crude heparin material
T2  - Journal of Pharmaceutical and Biomedical Analysis
N2  - Nuclear magnetic resonance (NMR) spectrometric methods for the quantitative analysis of pure heparin in crude heparin is proposed. For quantification, a two-step routine was developed using a USP heparin reference sample for calibration and benzoic acid as an internal standard. The method was successfully validated for its accuracy, reproducibility, and precision. The methodology was used to analyze 20 authentic porcine heparinoid samples having heparin content between 4.25 w/w % and 64.4 w/w %. The characterization of crude heparin products was further extended to a simultaneous analysis of these common ions: sodium, calcium, acetate and chloride. A significant, linear dependence was found between anticoagulant activity and assayed heparin content for thirteen heparinoids samples, for which reference data were available. A Diffused-ordered NMR experiment (DOSY) can be used for qualitative analysis of specific glycosaminoglycans (GAGs) in heparinoid matrices and, potentially, for quantitative prediction of molecular weight of GAGs. NMR spectrometry therefore represents a unique analytical method suitable for the simultaneous quantitative control of organic and inorganic composition of crude heparin samples (especially heparin content) as well as an estimation of other physical and quality parameters (molecular weight, animal origin and activity).
KW  - NMR spectroscopy
KW  - Heparin
KW  - Crude heparin
KW  - USP
KW  - Ions
Y1  - 2022
UR  - https://opus.bibliothek.fh-aachen.de/opus4/frontdoor/index/index/docId/10186
SN  - 0731-7085
VL  - 219
IS  - Article number: 114915
PB  - Elsevier
CY  - New York, NY
ER  -