微波消解-ICP-MS法测定舒尼铂原料药中银的残留量  

Determination of Residual Silver Content in Shuniplatin API by Microwave Digestion-ICP-MS

作　　者：张晓南 普冰清 陈雪江 徐红贵 王京昆 刘伟平[2] 杨晓燕 ZHANG Xiao-nan;PU Bing-qing;CHEN Xue-jiang;XU Hong-gui;WANG Jing-kun;LIU Wei-ping;YANG Xiao-yan(Yunnan Institute of Materia Medica,Yunnan Province Company Key Laboratory for TCM and Ethnic Drug of New Drug Creation,Yunnan Baiyao Group Innovation and R&D Center,Kunming 650111,China;Kunming Institute of Precious Metals,Kunming 650106,China)

机构地区：[1]云南省药物研究所云南省中药和民族药新药创制企业重点实验室,云南白药集团创新研发中心,昆明650111 [2]昆明贵金属研究所,昆明650106

出　　处：《贵金属》2020年第2期62-65,共4页Precious Metals

基　　金：国家重大新药创制专项(2009ZX09103-109);云南省新药开发专项(2014BC010)。

摘　　要：采用微波消解法进行样品前处理,以电感耦合等离子体质谱法(ICP-MS)测定了舒尼铂原料药中的银残留量。结果表明,银质量浓度在0.1~150μg/L的范围内,与银信号强度和内标铟信号强度的比值呈良好的线性关系,重复性试验的RSD为2.32%,加标回收率为95.89%~104.81%,检出限为0.0109μg/g,定量限为0.0365μg/g;3批样品测定结果分别为2.42、1.54和1.96μg/g。方法可满足舒尼铂原料药中银残留量测定的要求。The content of residual silver in Shuniplatin active pharmaceutical ingredients(Shuniplatin API)was determined by ICP-MS after sample digested by closed-vessel microwave system.The results indicated that the ratio of the signal intensity of silver to the internal indium standard showed a good linear relationship in the concentration ranges of 0.1~150μg/L.The relative standard deviation was 2.32%,and the recovery of silver was 95.89%~104.81%.The limit of detection was 0.0109μg/g,while the limit of quantitation was 0.0365μg/g.The determined silver content in three batches of samples was 2.42,1.54 and 1.96μg/g,respectively.It suggests that the method can meet the requirements of silver residue determination in Shuniplatin API.

关 键 词：分析化学 抗癌药 舒尼铂 银残留量 微波消解 电感耦合等离子体质谱(ICP-MS) 

分 类 号：R917[医药卫生—药物分析学] O6576.63[医药卫生—药学]