高效液相色谱-电感耦合等离子质谱法分析雄黄在大鼠脏器中代谢的砷形态

Analysis of Arsenic Metabolites of Realgar in Rat Viscera by HPLC-ICP-MS

采用HPLC-ICP-MS联用技术建立了大鼠脏器中AsB,As（Ⅲ）,MMA,DMA和As（Ⅴ）等砷形态的分析方法.采用超声水浴提取对样品进行前处理,Dionex IonPac AS19阴离子交换柱,20 mmol/L （NH4）2C03（pH 9.7）为流动相,对雄黄染毒后大鼠肝肾中的砷形态进行分析.实验表明,方法不受40Ar35Cl＋干扰,常见的5种砷形态化合物的线性范围为1～300 μg/L,相关系数（R2）均大于0.999,检出限为0.3 ～0.5（μg/L）,RSD均小于5％,加标回收率为83.8％～111.7％.通过对肝肾的形态分析,表明经雄黄染毒后大鼠肝脏中的砷形态主要为DMA、As（Ⅲ）和未知物2;肾脏中的砷形态主要为DMA、MMA、As（Ⅲ）、未知物1、未知物2和未知物3.综合表明,此方法适用于雄黄代谢后的主要砷形态分析.

HPLC-ICP-MS method was established to separate AsB, As（I I I）, monmethyl arsenic （MMA）, dimethyl arsenic （DMA） and As（V） in rat viscera. Ultrasonic water bath extraction was used for sample pretreatment. Dionex IonPac AS19 anion-exchange column and 20 mmol/L （NH4 ）2CO3 （pH = 9.7 ） were used to analyze arsenic species in rat liver and kidney after realgar infected. The results showed that the method was not interfered by 40Ar3sCl＋ peak, the linear ranges for five arsenic species were all between 1 and 300 μg/L with linear coefficients more than 0. 9990, and the detection limits were between 0.3 and 0.5 μg/L. The relative standard deviations （RSDs） for the determination of five species were less than 5% and the recoveries were between 83.8% and 111.7%. After speciation analysis, DMA, As（liD and unknown compound 2 were found in liver; DMA, MMA, As（liD, unknown compound 1, unknown compound 2 and unknown compound 3 were found in the kidney. The results indicated that this method could be used for arsenic species analysis of realgar metabolism.