摘要
目的:建立电感耦合等离子体质谱(ICP-MS)法测定苯磺酸氨氯地平片中V、Co、Ni、As、Cd、Hg、Pb 7种元素杂质的含量。方法:供试品经微波消解后,以Ge、In、Bi为内标元素,采用电感耦合等离子体质谱(ICP-MS)法测定,并进行方法学验证,用该方法测定54家企业生产的苯磺酸氨氯地平片中7种元素杂质的含量。结果:V、Co、Ni、As、Cd、Hg、Pb元素分别在1~100、1~100、1~100、1~100、1~100、0.5~4、1~100 ng·mL^(-1)范围内呈现良好的线性关系,相关系数r均≥0.9994;检测限:0.0004~0.0184 ng·mL^(-1),定量限:0.0014~0.0612 ng·mL^(-1);精密度RSD均≤1.81%,重复性RSD均≤6.15%;加样回收率(n=9)85.4%~106.5%、RSD≤4.74%。54批样品检测结果均小于规定的限度值。结论:该方法操作简单,分析快速,准确,可靠,灵敏度高,可用于苯磺酸氨氯地平片中7种元素杂质的质量控制。
Objective:To establish a method for simultaneous determination of 7 elemental impurities(V,Co,Ni,As,Cd,Hg Pb)in amlodipine besylate tablets based on inductively coupled plasma mass spectrometry(ICP-MS).Methods:After the samples were treated by microwave digestion,the solution was analyzed by ICP-MS.Ge,In,Bi were selected as the internal standards.The established method was validated.The contents of 7 elemental impurities in amlodipine besylate tablets from 54 enterprises were determined by this method.Results:The content of V,Co,Ni,As,Cd,Hg,Pb had good linear relationship in the ranges of 1-100,1-100,1-100,1-100,1-100,0.5-4,1-100 ng·mL^(-1),respectively.The correlation coefficients(r)all above 0.9994.The detection limits and quantification limits were in the range of 0.0004-0.0184 ng·mL^(-1)and 0.0014-0.0612 ng·mL^(-1).The RSD of precision was less then 1.8%.The RSD of repeatability was less then 6.1%.The average recoveries(n=9)were between 85.4%-106.5%,while their RSD was less then 4.7%.The content of 7 elemental impurities in 54 sample batches were in accordance with the limit value.Conclusion:The method is simple,rapid,accurate,reliable and highly sensitive,and can be used for the quality control of elemental impurities in amlodipine besylate tablets.
作者
朱乃军
金伟斌
张华锋
ZHU Naijun;JIN Weibin;ZHANG Huafeng(Suzhou Institute for Drug Control,Suzhou 215104,China)
出处
《中国药品标准》
CAS
2024年第3期257-264,共8页
Drug Standards of China
基金
苏州市科技发展计划项目(SYSD2019221)。
关键词
苯磺酸氨氯地平片
元素杂质
内标
微波消解
电感耦合等离子体质谱(ICP-MS)
质量控制
amlodipine besylate tablets
elemental impurity
internal standards
microwave digestion
inductively coupled plasma mass spectrometry(ICP-MS)
quality control
