ICP-MS法测定马来酸艾维替尼中钯、砷、镉、汞、铅的残留量

目的：建立电感耦合等离子体质谱法（ICP-MS法）测定马来酸艾维替尼原料药中钯、砷、镉、汞、铅的残留量。方法：用微波消解进行样品前处理，采用ICP-MS以锗、铟、铋为内标进行测定，射频功率1.55kW，碰撞气为氦气，载气为氩气，载气流量0.8 L·min^-1，泵速0.3 r·s^-1，数据采集重复次数3次。结果：各待测元素线性关系良好（r>0.994 0）；钯、砷、镉、汞、铅的平均加样回收率（n=3）范围分别为100.3%～111.9%、107.5%～111.9%、98.6%～101.4.%、90.5%～97.4%、116.9%～120.1%，RSD范围分别为2.8%～5.0%、1.4%～2.0%、0.50%～1.2%、1.1%～2.0%、1.9%～2.3%；精密度（重复性）、中间精密度的RSD<5%；检测下限为0.000 5～0.035 μg·g^-1，定量下限为0.002～0.106 μg·g^-1。3批样品（批号170501、A1000001、A1000002）中的钯含量分别为0.040 8、0.160 4、0.051 5 μg·g^-1，砷、镉、汞、铅含量测定结果均低于检测下限。结论：该方法可用于马来酸艾维替尼原料药中钯、砷、镉、汞、铅残留量的测定。

Objective: To establish a method for the determination of Pd,As,Cd,Hg,Pb residue in avitinib maleate. Methods: Sample was digested by microwave and was determined by inductively coupled plasma mass spectrometry with Ge,In and Bi as internal standards. The detection conditions were as follows:RF power of 1.55 kW,collision gas of He,argon gas (carrier) flow rate of 0.8 L·min^-1,pump speed of 0.3 r·s^-1,and data collection time of 3. Results: The linearity of the detected elements was good (r>0.994 0),the average recoveries of Pd,As,Cd,Hg,Pb were 100.3%-111.9%,107.5%-111.9%,98.6%-101.4.%,90.5%-97.4%,116.9%-120.1%,and RSDs were 2.8%-5.0%,1.4%-2.0%,0.50%-1.2%,1.1%-2.0%,1.9%-2.3%(n=3),respectively. The RSDs of precison (repeatability) and intermediate precision tests were less than 5.0%,the detection limit values were 0.000 5-0.035 μg·g^-1 and the quantitation limit values were 0.002-0.106 μg·g^-1. The results of Pd residue in three batches (lot No. 170501,A1000001,A1000002) of samples were 0.040 8,0.160 4,0.051 5 μg·g^-1,respectively. As,Cd,Hg and Pb were all less than respective limit of detection. Conclusion: The method is suitable for the determination of Pd,As,Cd,Hg and Pb in avitinib maleate.

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