电感耦合等离子体质谱法测定癸氟奋乃静中24种元素杂质

Determination of twenty-four elemental impurities in fluphenazinedecanoate by inductively coupled plasma-mass spectrometry

张叶 ¹孙逸舒 ²叶晓霞 ¹张雪 ¹乐健 ¹杨永健¹

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作者信息

1. 上海市食品药品检验研究院,国家药品监督管理局化学药品制剂质量分析重点实验室,上海 201203
2. 复旦大学药学院,上海 201203
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摘要

目的:建立电感耦合等离子体质谱法(ICP-MS)测定癸氟奋乃静中24种元素杂质的方法.方法:用有机溶剂溶解样品,以45Sc、72Ge、115In、125Te、175Lu、209Bi为内标,采用ICP-MS方法测定,RF功率1 550 W,雾化器流量0.6升/分钟,氩氧混合辅助气比例30％,采样深度8.0 mm,S/C温度-5 ℃.并对所建立的方法进行方法学验证.结果:各元素在线性范围内线性关系良好(r＞0.997),低、中、高三个浓度加样回收率(n=9)均在84％-135％之间,定量限均小于0.3 J.测定样品10批,其中检出少量铬(Cr)、砷(As)、铱(Ir)及汞(Hg),其他20种元素检出量均小于检测限.结论:该方法分析快速、灵敏度高、准确度好,适用于癸氟奋乃静元素杂质的质量控制.

Abstract

Objective:To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for the simultaneous determination of elemental impurities in fluphenazinedecanoate.Methods:Sample was dissolvedwith-organic solution.With 45Sc,72Ge,115In,125Te,175Lu and 209Bi used as internal standards,an ICP-MS method was developed and established with the following conditions:RF power of 1 550 W,atomizer flow rate of 0.6 L·min-1,argon oxygen mixed auxiliary gas ratio of 30％,sampling depth of 8.0 mm,and S/C temperature of-5 ℃.Results:The linear range of each element was good within the linear range(r＞0.997),the recovery rates at low,medium and high concentrations were 84％-135％,and the limit of detection was less than 0.3 J.Ten batches of samples were tested,trace contents of chromium(Cr),arsenic(As),iridium(Ir)and mercury(Hg)were detected,and the other 20 elements were less than the limit of detection.Conclusion:The method is fast,sensitive,and accurate for screening and the quality control of elemental impurities in fluphenazinedecanoate.

关键词

癸氟奋乃静/元素杂质/电感耦合等离子体质谱法/有机溶剂/ICH/Q3D

Key words

fluphenazinedecanoate/element impurities/inductively coupled plasma mass spectrometry/organic solution/ICH Q3D

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出版年

2024

中国药品标准

国家药典委员会

中国药品标准

影响因子：0.372

ISSN：1009-3656

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