ICP-MS法测定盐酸安舒法辛缓释片中7个元素杂质含量

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&#183;min^-1，采样深度5.0 mm，辅助气流速0.8 L&#183;min^-1，雾化器流速1.075 L&#183;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。

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&#183;min^-1,the sampling depth was 5.0 mm,the auxilliary flow was 0.8 L&#183;min^-1 and the nebulizer flow was 1.075 L&#183;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.

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