石墨炉原子吸收测定乌苯美司中钯的残留量  

Determination of Palladium Residues in Ubenimex by Graphite Furnace Atomic Absorption Spectrometry

作　　者：赵明娟 程磊 朱培曦 黄柳倩 顾霄 郑金琪 ZHAO Ming-juan;CHENG Lei;ZHU Pei-xi;HUANG Liu-qian;GU Xiao;ZHENG Jin-qi(Zhejiang University of Technology,Hangzhou 310014,China;Zhejiang Institute for Food and Drug Control,Hangzhou 310052,China)

机构地区：[1]浙江工业大学,浙江杭州310014 [2]浙江省食品药品检验研究院,浙江杭州310052

出　　处：《海峡药学》2020年第3期77-80,共4页Strait Pharmaceutical Journal

基　　金：浙江省药品监督管理局2020年度科技计划项目(2020014)。

摘　　要：目的建立乌苯美司中钯残留的测定方法。方法采用四种不同溶剂对样品进行前处理,选用冰醋酸超声溶解,再用0.5%硝酸稀释定容,通过石墨炉原子吸收光谱法进行测定。检测波长为247.6nm,狭缝宽度为0.2nm,空心阴极灯工作电流强度为6mA,测量模式为峰高,进样量为20μL。结果浓度在0~150μg·L^-1内呈现良好线性关系(r=0.9983);检出限为5.058μg·L^-1;仪器精密度为RSD=3.76%;重复性为3.60%;回收率在95%~105%之间,RSD=6.92%。结论数据准确、可靠,成功地完成对全国5家乌苯美司原料药厂家的15批样品中钯的测定。OBJECTIVE To establish a method for the determination of palladium residues in Ubenimex.METHODS The sample was pretreated with four different solvents.It was dissolved in glacial acetic acid,and then diluted with 0.5%nitric acid to determine the volume by GFAAS.The detection wavelength was 247.6nm,the slit width was 0.2nm,the operating current intensity of the HCL was 6mA,the measurement mode was the peak height,and the injection volume was 20μL.RESULTS The concentration showed a good linear relationship(r=0.9983)in the range of 0-150μg·L^-1;the detection limit was 5.058μg·L^-1;the instrument precision was RSD=3.76%;the repeatability was 3.60%;the recovery rate was 95%-105%,RSD=6.92%.CONCLUSION The data were accurate and reliable,and successfully determined the palladium in 15 batches of five Ubenimex manufacturers of raw materials.

关 键 词：乌苯美司 钯 石墨炉原子吸收光谱法 原料药 

分 类 号：R969.4[医药卫生—药理学]