摘要
目的:建立苯磺酸氨氯地平片中主要杂质的定性与定量分析方法。方法:采用LC-MS、NMR及色谱方法确认苯磺酸氨氯地平片中主要杂质结构。以C18柱为固定相,pH3.0缓冲液-甲醇-乙腈50∶35∶15为流动相,检测波长237 nm,外标法定量测定苯磺酸氨氯地平片中杂质。结果:苯磺酸氨氯地平片中主要杂质为氨氯地平氧化脱氢的产物(杂质A)。杂质A定量方法分离良好,杂质A与氨氯地平及其他杂质峰完全分离;在0.5-10.0μg/ml的范围内杂质A的峰面积和浓度线性相关,方法定量限10 ng/ml,回收率98.2%(n=9),RSD为0.2%(n=6)。结论:苯磺酸氨氯地平片中主要杂质为氨氯地平氧化脱氢的产物(杂质A)。该分析方法准确可靠,简便易行,可用于苯磺酸氨氯地平片中杂质A的测定。
Objective:To identify and determine the impurities in amlodipine beslyate tablets.Methods:The main impurities in amlodipine beslyate tablets were identified with LC-MS,NMR and chromatographic methods.Then the main impurities were determined with C18 column as stationary phase and buffer(pH 3.0)-methanol-acetontrile 50∶35∶15 as mobile phase.Results:The main impurity in amlodipine beslyate tablets was proved to be the dehydration product of amlodipine(Impurity A,IM A).IM A could be completely separated with the established method.It was a linear correlation between the area and the concentration in the range of 0.5~10.0 μg / ml.The Limit of Quantification of the method was 10 ng / ml,recovery was 98.2%(n = 9) and the RSD of the method was 0.2%(n = 6).Conclusion:The main impurity in amlodipine beslyate tablets was IM A.The established method is accurate,simple and is suitable for determination of IM A in amlodipine beslyate tablets.
出处
《南京医科大学学报（自然科学版）》
CAS
CSCD
北大核心
2013年第9期1314-1317,共4页
Journal of Nanjing Medical University(Natural Sciences)
基金
无锡市医院管理中心科研项目(YGM1011)
关键词
苯磺酸氨氯地平片
杂质
定性
定量
amlodipine beslyate tablets
impurity
identification
quantification
