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    液相色谱-原子荧光光谱法测定大米中4种砷形态的含量

    LC-AFS Determination of 4 Kinds of Arsenic Species in Rice

    • 摘要: 采用液相色谱-原子荧光光谱法测定大米中亚砷酸盐[As(Ⅲ)]、砷酸盐[As(Ⅴ)]、一甲基胂酸(MMA)和二甲基胂酸(DMA)等4种砷形态的含量。大米样品(1.00 g)中加入0.10 mol·L-1硝酸溶液10 mL,置于95 ℃水浴中热浸提取120 min,使4种形态砷的化合物溶出。提取液冷却后在Hamilton PRP X-100阴离子交换柱上进行色谱分离。用调节至pH 6.0的20 mmol·L-1 NH4H2PO4溶液作流动相(流量为1.2 mL·min-1)淋洗可使上述4种形态的砷化合物很好分离。用原子荧光光谱法分别测定各形态砷的含量。砷的质量浓度在5.00~500 μg·L-1范围内与其峰面积呈线性关系。上述4种形态砷的检出限(3S/N)依次为0.099,0.18,0.15,0.040 μg·L-1。加标回收率在94.7%~104%之间,测定值的相对标准偏差(n=6)在3.0%~7.4%之间。

       

      Abstract: LC-AFS was applied to the determination of 4 kinds of arsenic species including arsenite [As (Ⅲ)], arsenate [As (Ⅴ)], monomethylarsonic acid (MMA) and dimethylarsonic acid (DMA) in rice. Four chemical species of arsenic in rice were extracted from 1.00 g of rice sample by soaking the sample in 10 mL of 0.10 mol·L-1 HNO3 solution in a water-bath at 95 ℃ for 120 min. After cooling, the extract was introduced into the LC-AFS instrument and chromatographic separation was carried on a Hamilton PRP X-100 anion exchange column, by using 20 mmol·L-1 NH4H2PO4 solution (pre-adjusted to pH 6.0) as mobile phase (at a flow-rate of 1.2 mL·min-1), the 4 species of arsenic was separated nicely and determined separately by AFS. Linear relationship between values of peak area and mass concentration of arsenic was obtained in the range of 5.00-500 μg·L-1. Detection limits (3S/N) found for the 4 arsenic species were 0.099, 0.18, 0.15, 0.040 μg·L-1 respectively. Test for recovery was done by standard addition method, giving results in the range of 94.7%-104%, and values of RSDs (n=6) found were ranged from 3.0% to 7.4%.

       

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