电感耦合等离子体质谱法测定阿加曲班原料药中催化剂钯的残留量

目的：测定阿加曲班原料药中催化剂钯的残留量。方法：用微波消解法进行样品前处理；以铟为内标，采用电感耦合等离子体质谱法测定，发射功率1 600 W，等离子气流量18 L·min^-1，辅助气流量1.2 L·min^-1，泵速15 r·min^-1，进样延迟时间为30 s。结果：钯质量浓度在0.1~10 μg·L^-1的范围内，与钯强度和内标铟强度的比值呈良好的线性关系，重复性试验的RSD为2.2%，加标回收率为96.0%~103.1%，检测限为0.002 μg·g^-1；3批样品（批号0401、0402、0403）测定结果分别为70.02、80.14、71.31 ng·g^-1。结论：本方法可用于阿加曲班原料药中催化剂钯的残留量测定，同时为测定其他品种原料药中钯残留量测定提供参考和理论依据。

Objective: To determine the residue amount of palladium,which was used as a catalyst,in drug substances of argatroban.Methods: Microwave digestion was adopted for sample pretreatment.¹¹⁵In was chosen as internal standard element,and an inductively coupled plasma mass spectrometry method was established with following conditions: the RF power was 1 600 W,the plasma flow was 18 L·min -1,the auxiliary flow was 1.2 L·min -1,the pump speed was 15 r·min^-1,and the injection delay time was 30 s.Results: The ratio of intensity of palladium to the internal standard element and the concentration of palladium showed a good linear relationship in the 0.1-10 μg·L^-1 concentration range,with the relative standard deviation of repeatability 2.2%.The recovery was ranged in 96.0%-103.1%,and the limit of detection was 0.002 μg·g^-1.The results of palladium residue amount for three batches(lot No.0401,0402,0403)samples were 70.02,80.14 and 71.31 ng·g^-1,respectively.Conclusion: The method can be used for the determination of catalyst palladium residues in drug substances of argatroban,which provided a reference and method for further research of other crude product.