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3.0g置于不锈钢萃取池中,加入6g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100mL,经0.45μm滤膜过滤。采用Dionex IonPac AS-17色谱柱(250mm×4.0mm,10μm)分离滤液中的6种砷形态,以20mmol·L~(-1) NH_4HCO_3溶液为流动相在1.0mL·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0.5~50.0μg·L~(-1)内与对应的响应强度呈线性关系,检出限(3S/N)在0.15~0.24μg·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。
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 0.45μm filter membrane.The 6 arsenic species were seperated on a Dionex IonPac AS-17 column(250 mm×4.0 mm,10μm),with 20 mmol·L~(-1) NH_4HCO_3 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 0.5-50.0μg·L~(-1),with detection limits(3 S/N) in the range 0.15-0.24μg·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%.
引文
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