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

Determination of catalyst palladium residue in argatroban crude product by ICP-MS

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0.1~10μg·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0.002μg·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.115 In 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^（-1）0 μg·L^（-1） concentration range,with the relative standard deviation of repeatability 2.2%.The recovery was ranged in 96.0%^（-1）03.1%,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.