新型铂类抗癌药舒尼铂原料药中催化剂钯残留量的测定

Determination of Residual Catalyst Palladium in Shuniplatin Crude Product by ICP-MS

采用封闭体系微波消解法,电感耦合等离子体质谱法测定了舒尼铂原料药中催化剂钯的残留量,并进行方法学验证。实验结果表明钯质量浓度在0.01~150μg·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2.40%,加标回收率为96.79%~112.98%,检测限为0.0025μg·g-1,定量限为0.0084μg·g-1;三批样品测定结果分别为2.21、3.61、1.78μg·g-1。本方法便捷、准确、精度高,可满足舒尼铂原料药中催化剂钯残留量测定的要求。

A method to determine the residual catalyst palladium in Shuniplatin was developed and applied to the study of quality control.The samples were digested by closed-vessel microwave system and analyzed by ICP-MS.The linear relationship was good in concentration range 0.1~150μg·L-1,the relative standard deviation of repeatability was 2.2%,the recoveries of palladium were 96.79%~112.98%,the limit of detection was 0.0025μg·g-1,and the limit of quantitation was 0.0084μg·g-1.The results of residual catalyst palladium in three samples were 2.21,3.61 and 1.78μg·g-1.The ICP-MS method is sensitive and accurate,feasible for palladium determination in Shuniplatin.