【摘要】 目的:建立电感耦合等离子体质谱（ICP-MS）法测定盐酸安舒法辛缓释片中铅（Pb）、镉（Cd）、砷（As）、汞（Hg）、钴（Co）、钒（V）、镍（Ni）7个元素杂质含量。方法:用微波消解进行样品前处理;以⁷³Ge,¹¹⁵In,²⁰⁹Bi为内标,采用ICP-MS进行测定,测量模式为碰撞池模式（KED）,碰撞气流速4.35 mL·min^-1,采样深度5.0 mm,辅助气流速0.8 L·min^-1,雾化器流速1.075 L·min^-1;对所建立的方法进行了方法学验证。结果:7个元素标准曲线的相关系数均大于0.99;加样回收率在92.2%～104.4%之间;重复性试验RSD≤1.2%（n=6）;中间精密度试验RSD≤3%,均满足USP<233>方法学验证的要求。样品检测的结果远小于国际人用药物注册技术协调会议《元素杂质指南Q3D》（ICHQ3D）中各元素杂质的每日允许暴露量（PDE）。结论:本文建立的方法样品用量少,分析速度快,灵敏度高,可用于盐酸安舒法辛缓释片中元素杂质的质量研究。更多还原

【Abstract】 Objective:To establish an inductively coupled plasma mass spectrometry（ICP-MS）method for determination of 7 kinds of elemental impurities（Pb,Cd,As,Hg,Co,V,Ni）in desvenlafaxine hydrochloride extended-release tablets.Methods:Microwave digestion was adopted for sample pretreatment.⁷³Ge,¹¹⁵In,²⁰⁹Bi were chosen as internal standard elements,and an inductively coupled plasma mass spectrometry method was established with following conditions:measurement mode was collision cell mode with kinetic energy discrimination（KED）,the Q Cell gas was 4.35 mL·min^-1,the sampling depth was 5.0 mm,the auxilliary flow was 0.8 L·min^-1 and the nebulizer flow was 1.075 L·min^-1.The method was validated.Results:Regression coefficients of standard curve of those seven elemental impurities are beyond 0.99.The recovery rates of spiked samples ranged from 92.2% to 104.4%.In repeatability,the RSD ≤ 1.2%（n=6）.The RSD ≤ 3% of intermediate precision test.The determined values were well below permitted daily exposure（PDE）of elemental impurities in International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use < Guideline For Elemental Impurities Q3D>（ICHQ3D）.Conclusion:The microwave digestion-ICP-MS method has a high sensitivity,a strong specificity,a fast analysis speed,and it only requires a small amount of sample which can support the determination of 7 elements in desvenlafaxine hydrochloride extended-release tablets.更多还原