电感耦合等离子体质谱法测定盐酸坦洛新缓释胶囊中9种杂质元素含量  

Determination of 9 Elemental Impurities in Tamsulosin Hydrochloride Sustained Release Capsules by ICP-MS

作　　者：王娇娇 杏朝刚 齐东梅 陈文波 毛翎姿 袁京群 WANG Jiaojiao;XING Chaogang;QI Dongmei;CHEN Wenbo;MAO Lingzi;YUAN Jingqun(Analysis Center of Agrobiology and Environmental Sciences of Zhejiang University,Hangzhou 310058;Zhejiang Helisheng Pharmaceutical Co.Ltd.,Zhoushan 316013;University of California,Berkeley,94720 USA)

机构地区：[1]浙江大学农生环测试中心,浙江杭州310058 [2]浙江海力生制药有限公司,浙江舟山316013 [3]加州大学伯克利分校,美国伯克利94720

出　　处：《分析科学学报》2021年第3期356-360,共5页Journal of Analytical Science

基　　金：浙江大学实验技术研究项目(No.SJS202017)。

摘　　要：建立电感耦合等离子体质谱法(ICP-MS)同时测定盐酸坦洛新缓释胶囊中As、Pb、Cd、Hg、Co、V、Ni、Pd和Cr 9种杂质元素含量。采用整颗胶囊微波消解,无需研磨或其它处理。以^(74)Ge、^(115)In、^(209)Bi为内标,采用ICP-MS法进行测定。结果表明:9种杂质元素标准曲线的相关系数均大于0.999;加标回收率在85.54%~119.01%之间;定量限远小于ICH Q3D规定限量值。该方法重复性和精密度良好,且简单、便捷、准确。In this work,we established an inductively coupled plasma mass spectrometric method(ICP-MS)for simultaneous determination of 9 elemental impurities(As,Pb,Cd,Hg,Co,V,Ni,Pd and Cr)in tamsulosin hydrochloride sustained relesase capsules,so as to provide a reference for standard improvement and quality supervision for the related medicines.The whole capsule was digested by microwave without grinding or other treatments.^(74)Ge,^(115)In and ^(209)Bi were chosen as internal standard elements,and ICP-MS method was established with following conditions:measurement mode:cell mode with kinetic energy discrimination(KED),radio frequency power:1500 W,plasma gas flow:17.0 L·min^(-1),atomizing gas flow rate:0.96 L·min^(-1),auxiliary gas flow rate:1.20 L·min^(-1),He gas flow rate:3.0 mL·min^(-1),integration time:1000 ms,repeat times:3 times.The results showed that the regression coefficients of standard curve of those nine elemental impurities were beyond 0.999,and the recovery rates of spiked samples ranged from 85.54%to 119.01%.The quantitation limits were far below the recommended residue limits in ICH Q3D,and the repeatability and intermediate precision were good.The developed method is simple,convenient,accurate and provides some references for future work of elemental impurities in tamsulosin hydrochloride sustained relesase capsules.

关 键 词：盐酸坦洛新缓释胶囊 元素杂质 残留限度 电感耦合等离子体质谱法 

分 类 号：O657.63[理学—分析化学]