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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
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)
关键词
氢化物发生-原子荧光光谱法
雄黄
砷
形态分析
hydride generation atomic fluorescence spectrometry
Realgar
arsenic
speciation analysis
