Structural Identification and Analysis of Degradation Impurities in Nimodipine Oral Solution
10.13748/j.cnki.issn1007-7693.20222720
- VernacularTitle:尼莫地平口服溶液中降解杂质的结构鉴定及分析
- Author:
Hui YE
1
;
Fei JIA
1
;
Xiaoping CHEN
1
;
Xiaoxiao SONG
1
Author Information
1. Hangzhou Bio-Sincerity Pharma-Tech Co., Ltd., Hangzhou 310053, China
- Publication Type:Journal Article
- Keywords:
nimodipine , structural identification , degradation impurity , HPLC-MS
- From:
Chinese Journal of Modern Applied Pharmacy
2023;40(24):3404-3410
- CountryChina
- Language:Chinese
-
Abstract:
Abstract:OBJECTIVE To identify and analyze two unknown degradation impurities in nimodipine oral solution. METHODS The chemical structure of the unknown impurity was deduced by two-dimensional liquid chromatography-high resolution mass spectrometry(2DLC-HRMS), and the impurity monomer was obtained by directional synthesis. The structure of the impurity was confirmed by 1H-NMR and 13C-NMR, chromatographic separations were performed on an Thermo Syncronis C18(250 mm×4.6 mm, 5 μm) column. Using 5 mmol·L-1 potassium dihydrogen phosphate buffer(pH 2.8) as mobile phase A, while methanol-acetonitrile(50:50) was mobile phase B, with gradient elution. The mobile phase was pumped at 1.0 mL·min-1. The column temperature was 30℃. The detection wavelength was 235 nm. RESULTS Nimodipine and its related substances had good separation. The correction factors of every impurities ranged from 0.8 to 1.1. CONCLUSION The established method has good specificity and can effectively isolate and determine the related substances in nimodipine oral solution. This study provides a reference to guide the impurity control of nimodipine oral solution and other dosage forms.
