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≥0.999 4;检测限:0.000 4～0.018 4 ng·mL-1,定量限:0.001 4～0.061 2 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.
Abstract
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 0.999 4.The detec-tion limits and quantification limits were in the range of 0.000 4-0.018 4 ng·mL-1 and 0.001 4-0.061 2 ng·mL-1.The RSD of precision was less then 1.8％.The RSD of repeatability was less then 6.1％.The average re-coveries(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.
维普
万方数据