电感耦合等离子体质谱法测定磷酸西格列汀原料药中催化剂铑的残留量

Determination of Catalyst Rhodium Residue in Sitagliptin Phosphate Crude Product by ICP-MS

目的:考察磷酸西格列汀原料药中催化剂铑的残留量。方法:样品以稀盐酸溶解,以钇和铟为内标,采用电感耦合等离子体质谱法测定磷酸西格列汀中铑的残留量。结果:铑在0~10μg/L的质量浓度范围内,其离子强度与浓度呈良好的线性关系;重复性试验的RSD为1.2%;加标回收率为91.3%~100.8%;检出限为0.039μg/L。结论:该方法简便、快速、灵敏准确,可用于磷酸西格列汀原料药中痕量铑含量的测定。

Objective:To develop the residue amount of rhodium which was used as a catalyst in drug substance of Sitagliptin Phosphate.Methods:Sample was dissolved by diluted hydrochloric acid,yttrium(Y)and indium(In)were chosen as interal standard elements,and an inductively coupled plasma mass spectrometry method was established.Results:The ratio of intensity of rhodium to the interal standard elements and the concentration of rhodium showed a good linear relationship in the 0~10μg/L concentration range,with the relative standard deviation of repeatability 1.2%.The recovery was ranged in 91.3%~100.8%,and the limit of detection was 0.039μg/L.Conclusion:This is a simple,rapid,sensitive and accurate method for the determination of trace Rh in Sitagliptin Phosphate.