ICP-MS法测定富马酸福莫特罗原料药中催化剂钯的残留量  

Determination of Catalyst Palladium Residue in Formoterol Fumarate Dihydrate Crude Product by ICP-MS

作　　者：李春盈[1] 张静[1] 钟依雯 曾敏珊 LI Chunying;ZHANG Jing;ZHONG Yiwen;ZENG Minshan(Guangzhou Institute of Drug Control,Guangzhou,Guangdong 510160,China)

机构地区：[1]广州市药品检验所,广东广州510160

出　　处：《今日药学》2020年第11期767-768,774,共3页Pharmacy Today

摘　　要：目的建立富马酸福莫特罗中催化剂钯(Pd)残留的检测方法。方法通过直接溶解样品,以电感耦合等离子质谱法(ICP-MS)测定样品中钯的含量。结果测定了3批富马酸福莫特罗中钯的含量。ICP-MS条件经优化后,测得钯在2~50μg·L-1浓度范围内相关系数为0.999 9(n=6),线性关系良好,方法检测限为0.03μg·L-1,回收率在98.0%~101.4%之间,RSD为1.1%(n=6)。结论本方法操作简便、快捷、灵敏度高,适用于富马酸福莫特罗中钯残留量的检测。OBJECTIVE To establish a method for determinating the residual content of palladium which was used as a catalyst in drug substance of formoterol fumarate dihydrate. METHODS The samples were prepared through dissolving directly and analyzed by inductively coupled plasma mass spectrometry(ICP-MS). RESULTS The content of palladium residue in 3 batches of formoterol fumarate dihydratewere determined.Optimized by ICP-MS,the calibration curves of palladium were at good linear of the concentration range of 2-50 μg·L-1,with correlation coefficient(r) was 0.999 9(n=6). Detection limits of the method was 0.03 μg·L-1. The recoveries were in the range of 98.0%-101.4%,and RSD was 1.1%(n=6). CONCLUSION The method is highly sensitive,rapid and accuracy for determination of catalyst palladium residue in formoterol fumarate dihydrate crude product.

关 键 词：电感耦合等离子质谱法 钯残留量 富马酸福莫特罗 

分 类 号：R917[医药卫生—药物分析学]