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    加速溶剂萃取联合高效液相色谱-电感耦合等离子体质谱法测定畜肉制品中的6种砷形态

    Determination of 6 Arsenic Species in Livestock Products by HPLC-ICP-MS Combined with Accelerated Solvent Extraction

    • 摘要: 采用高效液相色谱联用电感耦合等离子体质谱法(ICP-MS)测定畜肉制品中的一甲基砷、二甲基砷、三价砷、五价砷、砷甜菜碱和砷胆碱。称取经组织粉碎机粉碎的样品约3.0 g置于不锈钢萃取池中,加入6 g石英砂,搅拌均匀,以甲醇(2+1)溶液为提取溶剂,进行加速溶剂萃取。提取完成后,将提取液用甲醇(2+1)溶液定容至100 mL,经0.45 μm滤膜过滤。采用Dionex IonPac AS-17色谱柱(250 mm×4.0 mm,10 μm)分离滤液中的6种砷形态,以20 mmol·L-1 NH4HCO3溶液为流动相在1.0 mL·min-1流量下进行洗脱,采用ICP-MS测定洗脱液中6种砷形态。结果表明:6种砷形态质量浓度均在0.5~50.0 μg·L-1内与对应的响应强度呈线性关系,检出限(3S/N)在0.15~0.24 μg·kg-1之间。加标回收率在86.0%~108%之间,测定值的相对标准偏差(n=6)在2.6%~3.9%之间。

       

      Abstract: A method of HPLC-ICP-MS was applied to the determination of methyl arsenic, dimethyl arsenic, arsenic(Ⅲ), arsenic(Ⅴ), arsenic choline and arsenic betaine in livestock products. About 3.0 g of the sample pulverized by a tissue pulverizer was added into a stainless steel extraction tank, and 6 g of quartz sand was added. The mixture was stirred uniformly, and methanol (2+1) solution was used as extraction solvent to carry out accelerated solvent extraction. After the extraction was completed, the extract was made up to 100 mL with methanol (2+1) solution, and filtered through a 0.45 μm filter membrane. The 6 arsenic species were seperated on a Dionex IonPac AS-17 column (250 mm×4.0 mm, 10 μm), with 20 mmol·L-1 NH4HCO3 solution as mobile phase for elution at a flow rate of 1.0 mL·min-1. ICP-MS was used to determine the 6 arsenic species in the eluate. The result showed that linear relationships were found between response intensity and mass concentration of the 6 arsenic species in the same range of 0.5-50.0 μg·L-1, with detection limits (3S/N) in the range 0.15-0.24 μg·kg-1. Values of recovery obtained by standard addition method were in the range of 86.0%-108%, and RSDs (n=6) were in the range of 2.6%-3.9%.

       

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