高效液相色谱-电感耦合等离子体质谱测定蟾酥中铜、砷、镉、汞、铅含量及砷化学形态

Determination of Cu,As,Cd,Hg,Pb and Arsenic Species in Venenum Bufonis with High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry

建立了微波消解-电感耦合等离子体质谱(ICP-MS)测定蟾酥中Cu、As、Cd、Hg、Pb等元素含量的分析方法,检出限为0.28～5.7μg/L,元素加标回收率均在91.5%～115%。用1.2mol/LHCl浸提蟾酥中的As形态,利用高效液相色谱(HPLC)与电感耦合等离子体质谱(ICP-MS)联用技术对蟾酥样品中的As化学形态进行了初步探讨,发现其中As主要以有毒的无机As(Ⅴ)形态存在,并讨论了形态分析的方法及结果。本方法适用于蟾酥中药样品质量控制和安全评估的要求。

A method involving microwave digestion and inductively coupled plasma-mass spectrometric （ICP- MS） analysis was established for the determination of five elements （Cu, As, Cd, Hg, Pb） in Venenum Bufonis. Detection limits for these five elements were in the range of 0.28 μg/L to 5.7 μg/L, and the recov- eries ranged from 91.5% to 115%. The arsenic species in venenum bufonis were extracted using 1.2 mol/L hydrochloric acid, in addition, the chemical forms of arsenic including inorganic As（V） in Venenum Bufonis samples were quantified by the hyphenated technique of high performance liquid chromatography coupled with inductively coupled plasma-mass spectrometry（HPLC-ICP-MS）. The speciation results are presented and the analytical merits of the technique are discussed. The technique was applied for the quality control and safety evaluation of Venenum Bufonis samples.