仁青芒觉中可溶性砷形态的HPLC-ICP-MS研究  

Speciation analysis of solvable arsenic in Renqing Mangjue by HPLC-ICP-MS

作　　者：王英锋[1] 竺梅[2] 冯敏[1] 热增才旦[3] 张兰[1] 施燕支[1] 

机构地区：[1]首都师范大学分析测试中心,北京100048 [2]首都师范大学校医院,北京100048 [3]青海大学医学院中藏药研究中心,西宁810001

出　　处：《药物分析杂志》2011年第10期1884-1886,共3页Chinese Journal of Pharmaceutical Analysis

基　　金：北京市自然科学基金资助课题(No:2102011)

摘　　要：目的:采用HPLC-ICP-MS对藏药仁青芒觉中可溶性砷的形态进行研究。方法:采用Agilent G3154A阴离子交换柱,以0.2 mmol.L-1 EDTA和2 mmol.L-1磷酸二氢钠的溶液(pH 6.0)为流动相,流速1.0 mL.min-1,测定了仁青芒觉中砷的形态。前处理选择微波萃取,比较了1%盐酸、1%硝酸、2%醋酸、50%甲醇不同萃取剂的提取效率。结果:仁青芒觉在不同提取液中砷的形态主要以As(Ⅲ)和As(V)的形式存在,且1%盐酸、1%硝酸的提取效率较高。As(Ⅲ)和As(V)检出限(S/N=3)分别为0.39 ng.g-1和0.72 ng.g-1,样品加标平均萃取回收率(n=3)分别为95.6%和85.3%,精密度试验的RSD(n=8)分别为2.0%和3.2%。结论:藏药仁青芒觉中可溶性砷形态的研究,为藏药中砷的毒理学研究提供了依据。Objective：To study the speciation of solvable arsenic in Renqing Mangjue.Methods：High performance liquid chromatography with Agilent G3154A anion-exchange column coupled with inductively coupled plasma-mass spectrometry were adopted.The optimized mobile phase composition was 2.0 mmol·L^-1 sodium dihydrogen phosphate,0.2 mmol·L^-1 EDTA at pH 6.0.Micro wave-assisted extraction was chosed as pre-treatment method,the extract efficiencies of different extractants（1% hydrochloric acid,1% nitric acid,2% acetic acid,50% methanol） were compared.Results：The result indicated that the main speciation of As（Ⅲ） and As（V） was presented in extraction solutions of Renqing Mangjue and 1% hydrochloric acid and 1% nitric acid had high extract efficiency.The limits of detection（S/N=3） of As（Ⅲ） and As（V） were 0.39 ng·g-1 and 0.72 ng·g-1 respectively;Average spiked recoveries（n=3） were 95.6% and 85.3% respectively;RSDs of the precision test（n=8）were 2.0% and 3.2%.Conclusion：Speciation analysis of solvable arsenic in Renqing Mangjue by HPLC-ICP-MS has offered a reference for toxicology of arsenic in Tibetan medicine.

关 键 词：高效液相色谱-电感耦合等离子体-质谱 藏药 仁青芒觉 重金属 砷 形态分析 

分 类 号：R917[医药卫生—药物分析学]