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    高效液相色谱-电感耦合等离子体质谱法同时测定海产品中9种砷形态化合物

    Simultaneous Determination of Nine Arsenic Species in Marine Products by HPLC-ICP-MS

    • 摘要: 1.000 0 g样品经38 mL的0.5 mmol·L-1(NH42CO3溶液-甲醇(99+1)混合液(pH 8.5)超声萃取2 h后,加入乙酸2 mL,用水定容至50 mL,离心后,上清液在Hamilton PRP-X100阴离子分析柱(250 mm×4 mm,10 μm)上分离,以0.5 mmol·L-1碳酸铵溶液-甲醇(99+1)混合液为流动相A(pH 8.5),50 mmol·L-1碳酸铵溶液-甲醇(99+1)混合液(pH 8.5)为流动相B进行梯度洗脱,9种砷形态化合物在20 min内达到完全分离,经电感耦合等离子体质谱法测定。9种砷形态化合物的质量浓度在一定范围内与峰面积呈线性关系,测定下限(10S/N)在50~100 μg·kg-1之间。加标回收率在74.0%~109%之间,测定值的相对标准偏差(n=6)在5.4%~13%之间。方法用于海产品中9种砷形态化合物的测定,结果表明样品中的砷主要以无毒的砷甜菜碱形式存在。

       

      Abstract: After 1.000 0 g of the sample was ultrasonically extracted with 38 mL of a mixed solution (pH 8.5) of 0.5 mmol·L-1 (NH4)2CO3 solution and methanol (99+1) for 2 h, 2 mL of acetic acid was added into the extract and the solution was diluted to 50 mL with water. After centrifugation, the supernatant was seperated on a Hamilton PRP-X100 anion analytical column (250 mm×4 mm, 10 μm), with a mixture (pH 8.5) of 0.5 mmol·L-1 (NH4)2CO3 solution and methanol (99+1) as mobile phase A, and a mixture (pH 8.5) of 50 mmol·L-1 (NH4)2CO3 solution and methanol (99+1) as mobile phase B, for gradient elution. Nine arsenic species were separated within 20 mins and detemined by ICP-MS. Linear relationships were found between the peak areas and the mass concentrations of nine arsenic species in definite ranges, with lower limits of determination (10S/N) in the range of 50-100 μg·kg-1. Recovery obtained by standard addition method were in the range of 74.0%-109%, and RSDs (n=6) were in the range of 5.4%-13%. The proposed method was used to analyze marine products and it was found that the main arsenic specie in the sample was non-toxic arsenic betaine.

       

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