仁青芒觉中可溶性砷形态的HPLC-ICP-MS研究

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.