苯磺酸氨氯地平片主要杂质的定性与定量分析
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无锡市医院管理中心科研项目(YGM1011)


Identification and quantification of impurities in amlodipine besylate tablets
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    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0.5~10.0 μg/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。

    Abstract:

    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.

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赵 霞,李 博,陈伯玮,王岁楼.苯磺酸氨氯地平片主要杂质的定性与定量分析[J].南京医科大学学报(自然科学版),2013,(9):1314-1317

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  • 收稿日期:2013-03-29
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  • 在线发布日期: 2013-09-18
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