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作 者:许珺辉[1] 王洪玮[1] 崔蓉[1] 王旗[1] 赵京辉[1] 林瑞超[2]
机构地区:[1]北京大学公共卫生学院,北京100083 [2]中国药品生物制品检定所,北京100050
出 处:《药物分析杂志》2007年第3期395-399,共5页Chinese Journal of Pharmaceutical Analysis
基 金:国家"十五"科技攻关课题(编号2001BA701A57)
摘 要:目的:建立一种中药中砷的形态分析方法,分离并测定雄黄及含雄黄中成药中4种形态的砷化合物:无机 As(Ⅲ)、As(V)和有机单甲基胂酸(MMA)、二甲基胂酸(DMA)。方法:以稀盐酸溶液(pH 2)浸提雄黄及含雄黄中成药中的可溶性砷,用阴、阳离子固相萃取小柱进行分离,氢化物发生-原子荧光光谱法测定4种形态砷含量。结果:4种形态砷能实现完全分离,测定精密度、准确度良好。结论:本方法较为简便,准确、可靠,适用于分离测定雄黄及含雄黄的中成药中4种形态砷含量。Objective :To develop a method for analysis of arsenic species, i. e. arsenite As( Ⅲ ), arsenite As( V),monomethylarsonic acid (MMA) , and dimethylarsinic acid (DMA) in Realgar and in Chinese traditional patent medicine containing Realgar. Method:Arsenic species in samples were extracted with dilute hydrochloric acid solution ( pH 2) and the separation were performed on a silica-based strong cation - exchange (SCX) cartridge, and a resin-based strong anion -exchange (SAX) cartridge. Then hydride generation atomic fluorescence spectrometry was used to determine the speciation of arsenic in samples. Results: Calibration curves were linear with regression coefficients of more than 0. 999 for all four arsenic species, and the linear ranges of As( V ) .MMA and DMA were 0 -20 ng· mL^-l and of As( Ⅲ ) was 0 -40 ng · mL^-1. The average recoveries of all four arsenic species were ranged from 81% to 105.4% and precision (RSD) were within 8.7% for DMA,12% for MMA,4. 7% for As(V) and 3% for As( Ⅲ ). Conclution:The proposed method is simple, accurate and is suitable for As speciation analysis in Realgar and in Chinese traditional patent medicine containing Realgar.
关 键 词:氢化物发生-原子荧光光谱法 雄黄 砷 形态分析
分 类 号:R917[医药卫生—药物分析学]
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