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拟建立检测尿液中As(Ⅲ)、DMA(Ⅴ)、MMA(Ⅴ)和As(Ⅴ)4种砷化合物形态的HPLC-DRC-ICP-MS的方法。采用DRCTM(反应气为O2)与HPLC联用作为检测器,Phenomenex ODS-3作为分离柱,5 mmol/L四丁基羟胺,3 mmol/L丙二酸,5%(体积分数)甲醇为流动相(pH=5.0~6.0),建立了同时分析尿液中As(Ⅲ)、DMA(Ⅴ)、MMA(Ⅴ)和As(Ⅴ)的方法。实验结果显示:该分析方法对上述4种砷化合物的检测限均在0.1μg/L以下,在1~20μg/L范围内线性关系良好,准确度和精密度良好,回收率为89%~106%,样品中的Cl-1对测定没有影响。所建立的HPLC-DRC-ICP-MS分析方法稳定、可靠,适用于快速、批量测定尿砷形态。
To establish a HPLC-DRC-ICP-MS method for the determination of four As (Ⅲ), As (Ⅲ), DMA (Ⅴ), MMA (Ⅴ) and As (Ⅴ) Phenomenex ODS-3 was used as the separation column with 5 mmol / L tetrabutylhydroxylamine, 3 mmol / L malonic acid and 5% methanol as the mobile phase using DRCTM (O2 as reaction gas) A method for the simultaneous determination of As (Ⅲ), DMA (Ⅴ), MMA (Ⅴ) and As (Ⅴ) in urine was established. The experimental results show that the detection limits of the above four arsenic compounds are less than 0.1μg / L, the linearity is good in the range of 1 ~ 20μg / L, the accuracy and precision are good, the recoveries are 89% ~ 106 %, Cl-1 in the sample had no effect on the assay. The established HPLC-DRC-ICP-MS analysis method is stable and reliable, suitable for rapid, batch determination of urinary arsenic.