Multinuclear NMR screening of pharmaceuticals using standardization by 2H integral of a deuterated solvent
- NMR standardization approach that uses the 2H integral of deuterated solvent for quantitative multinuclear analysis of pharmaceuticals is described. As a proof of principle, the existing NMR procedure for the analysis of heparin products according to US Pharmacopeia monograph is extended to the determination of Na+ and Cl- content in this matrix. Quantification is performed based on the ratio of a 23Na (35Cl) NMR integral and 2H NMR signal of deuterated solvent, D2O, acquired using the specific spectrometer hardware. As an alternative, the possibility of 133Cs standardization using the addition of Cs2CO3 stock solution is shown. Validation characteristics (linearity, repeatability, sensitivity) are evaluated. A holistic NMR profiling of heparin products can now also be used for the quantitative determination of inorganic compounds in a single analytical run using a single sample. In general, the new standardization methodology provides an appealing alternative for the NMR screening of inorganic and organic components in pharmaceutical products.
| Author: | Yulia MonakhovaORCiD, Bernd W.K. Diehl |
|---|---|
| DOI: | https://doi.org/10.1016/j.jpba.2021.114530 |
| ISBN: | 0731-7085 |
| Parent Title (English): | Journal of Pharmaceutical and Biomedical Analysis |
| Publisher: | Elsevier |
| Document Type: | Article |
| Language: | English |
| Year of Completion: | 2022 |
| Date of the Publication (Server): | 2022/11/07 |
| Tag: | Heparin; Inorganic ions; NMR spectroscopy; Standardization |
| Volume: | 209 |
| Issue: | Article number: 114530 |
| Link: | https://doi.org/10.1016/j.jpba.2021.114530 |
| Zugriffsart: | bezahl |
| Institutes: | FH Aachen / Fachbereich Chemie und Biotechnologie |
| collections: | Verlag / Elsevier |
