Quantitative analysis of Cefpodoxime Proxetil raw material and dry suspension using proton nuclear magnetic resonance

Abstract

This study established a simple, rapid, and accurate nuclear magnetic resonance (NMR) quantitative method to determine the cefpodoxime proxetil content in raw materials and dry suspensions, and evaluated the uncertainty. The relative content of cefpodoxime proxetil iso-A and iso-B was also analyzed based on 1H NMR. In this study, an internal standard method was used, with DMSO-d6 as the solvent and maleic acid and 1,3,5-trimethylbenzene as internal standards, to calculate the concentration of the samples. Quantitative analysis was performed using both the traditional quantitative NMR (traditional qNMR) and the quantitative Global Spectral Deconvolution (qGSD) method. The linearity range, quantitation limit, precision, robustness, and accuracy of these quantitative analysis methods were validated. The results indicated that both internal standards and integration methods met the requirements of the “9101 Guidelines for Analytical MethodValidation” in the 2020 edition of the Chinese Pharmacopoeia. Compared to the traditional qNMR, qGSD has unique advantages in accurate quantitative analysis in complex systems. By using the combined HPLC-SPE-NMR technique, cefpodoxime proxetil iso-A and iso-B were enriched and analyzed, and their NMR data were accurately assigned. The quantitative analysis results were in line with the requirements of the Chinese Pharmacopoeia.

Keywords

qNMR / qGSD / cefpodoxime proxetil / uncertainty / HPLC-SPE-NMR

Acknowledgments

This work was funded by the National Key R&D Program of China (2022YFE0199700).

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