Jimenez de Blas O, Vicente Gonzalez S, Seisdedos Rodriguez R, Hernandez Mendez J
University of Salamanca, Faculty of Chemistry, Department of Analytical Chemistry, Nutrition, and Food Sciences, Spain.
J AOAC Int. 1994 Mar-Apr;77(2):441-5.
A flow injection-hydride generation/atomic absorption spectroscopic method for the measurement of total urinary arsenic and for the selective determination of inorganic arsenic, monomethylarsonic acid (MMAA), and dimethylarsinic acid (DMAA) was developed. Destruction of the organic matrix is necessary to measure total arsenic content of urine samples. Digestion of this matrix with HNO3-H2SO4-H2O2 is described. The separation of inorganic, monomethylated, and dimethylated arsenic compounds in urine was performed with ion-exchange chromatography on AG 50 W-X8 resin. Detection limits of 2 ppb for each arsenic form and of 3 ppb for total arsenic in urine analyzed after mineralization were found. Recoveries in triplicate urine samples spiked with 10 ppb inorganic arsenic, 20 ppb MMAA, and 40 ppb DMAA were 93, 91, and 85%, respectively. The precision (relative standard deviation) of the method obtained in 10 replicate analyses of urine samples spiked with arsenic metabolites varied from 3.2 to 4.6%. This method is applicable to urine samples in studies relating to arsenic exposure and its monitoring.
开发了一种流动注射-氢化物发生/原子吸收光谱法，用于测定尿中总砷以及选择性测定无机砷、一甲基胂酸（MMAA）和二甲基胂酸（DMAA）。为了测量尿样中的总砷含量，必须破坏有机基质。本文描述了用HNO3-H2SO4-H2O2对该基质进行消解的方法。采用AG 50 W-X8树脂离子交换色谱法对尿中的无机、一甲基化和二甲基化砷化合物进行分离。矿化后分析尿样中每种砷形态的检测限为2 ppb，总砷的检测限为3 ppb。在添加了10 ppb无机砷、20 ppb MMAA和40 ppb DMAA的尿样中进行三次重复加标回收试验，回收率分别为93%、91%和85%。在对添加了砷代谢物的尿样进行10次重复分析时，该方法的精密度（相对标准偏差）在3.2%至4.6%之间。该方法适用于与砷暴露及其监测相关研究中的尿样。
