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目的研究高砷区人尿中4种形态砷化物的测定方法。方法采用阴离子交换分析柱,以15 mmol/L(NH4)2HPO4(1.0 ml/min)为流动相,pH6.0,以1.5%KBH4/0.5%KOH(3.4 ml/min)为还原剂成功分离了亚砷酸[As(Ⅲ)]、二甲基砷酸(DMA)、一甲基砷酸(MMA)和砷酸[As(V)]。结果检出限分别为0.8μg/L[As(Ⅲ)]、1.7μg/L(DMA)、1.3μg/L(MMA)、3.6μg/L[As(V)]。尿样经过离心、0.22μm水系醋酸纤维素膜过滤2次上机测定。样品加标平均萃取回收率在74.5%～97.4%之间,RSD在1.8%～4.2%之间。结论该方法简便、快速,具有较好的精密度和准确度,适用于人尿中4种形态砷的测定。
Objective To study the method for the determination of four kinds of arsenic in human urine of high arsenic area. Methods An anion exchange column was successfully used to separate 15 mmol / L (NH4) 2HPO4 (1.0 ml / min) as mobile phase and pH 6.0 with 1.5% KBH4 / 0.5% KOH Arsenious acid [As (III)], dimethyl arsenate (DMA), monomethyl arsenate (MMA) and arsenic [As (V)]. The detection limits were 0.8μg / L [As (Ⅲ)], 1.7μg / L (DMA), 1.3μg / L (MMA) and 3.6μg / L [As (V)] respectively. Urine samples were centrifuged, 0.22μm aqueous cellulose acetate membrane filter 2 times on the machine measured. The average recovery of spiked samples ranged from 74.5% to 97.4% with RSD ranging from 1.8% to 4.2%. Conclusion The method is simple, rapid, has good precision and accuracy, and is suitable for the determination of four forms of arsenic in human urine.