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建立了采用水-甲醇(1∶1)溶液微波提取,高效液相色谱与电感耦合等离子体质谱仪联用进行烟叶中砷形态分析的方法.采用阴离子色谱柱,以p H 6.0、15 mmol/L(NH4)2HPO4溶液为流动相,成功分离了As(Ⅲ)、As(V)、甲基砷(MMA)和二甲基砷(DMA),分离保留时间相对标准偏差As(Ⅲ)0.50%、As(V)0.34%、MMA 0.82%、DMA0.53%.方法的检出限以砷计As(Ⅲ)0.13μg/L、As(V)0.21μg/L、MMA 0.13μg/L、DMA 0.11μg/L,测定相对标准偏差As(Ⅲ)2.60%、As(V)1.44%、MMA 3.86%、DMA 1.54%,加标回收率As(Ⅲ)92.7%~94.8%、As(V)97.2%~105.4%、MMA 93.5%~95.3%、DMA 95.4%~101.2%.该方法灵敏度高,分离重复性好,微波一次提取分析烟叶中砷形态,同三次超声提取方法比较,结果吻合.
A method was developed for the determination of arsenic in tobacco leaves by microwave extraction of water-methanol (1: 1) solution and high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (ICP-MS). An anion chromatographic column was developed with p H 6.0 and 15 mmol / As (Ⅲ), As (V), Methyl Arsenate (MMA) and Dimethyl Arsenate (DMA) were successfully separated from the mobile phase of L (NH4) 2HPO4 and the relative standard deviation of retention time was 0.50% , As (V) 0.34%, MMA 0.82% and DMA 0.53% .The detection limits of As (Ⅲ) 0.13μg / L, As (V) 0.21μg / L, MMA 0.13μg / 0.11μg / L, As (Ⅲ) 2.60%, As (V) 1.44%, MMA 3.86% and DMA 1.54% respectively. The recoveries were 92.7% ~ 94.8% % To 105.4%, MMA 93.5% to 95.3%, DMA from 95.4% to 101.2% .This method has the advantages of high sensitivity, good repeatability, and the first time microwave extraction and analysis of arsenic in tobacco leaves.