苯磺酸氨氯地平片主要杂质的定性与定量分析  

Identification and quantification of impurities in amlodipine besylate tablets

作　　者：赵霞[1] 李博[2,3] 陈伯玮[2] 王岁楼[2] 

机构地区：[1]无锡市第二人民医院医疗发展部,江苏无锡214002 [2]中国药科大学食品质量与安全教研室,江苏南京210009 [3]中国药科大学教育部药物质量与安全预警重点实验室,江苏南京210009

出　　处：《南京医科大学学报（自然科学版）》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)

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.

关 键 词：苯磺酸氨氯地平片 杂质 定性 定量 

分 类 号：R972[医药卫生—药品]