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    气相色谱-串联质谱法测定辣根中37种农药残留量

    GC-MS/MS Determination of Residual Amounts of 37 Pesticides in Horseradish

    • 摘要: 采用气相色谱-串联质谱法测定辣根中37种农药的残留量。样品用乙酸乙酯-乙腈(15+85)混合液提取,经N-丙基乙二胺(PSA)、活性炭和无水硫酸钠净化,高速离心所得上清液浓缩后用1.0 mL甲苯定容。经VF-5MS色谱柱分离,串联质谱测定,内标法定量。37种农药的测定下限(10S/N)在0.005~0.1 mg·kg-1之间。以空白辣根样品为基体,加入4种不同浓度的标准溶液进行回收试验,其回收率在61.1%~120%之间,相对标准偏差(n=7)在2.9%~19%之间。

       

      Abstract: GC-MS/MS was applied to the determination of residual amounts of 37 kinds of pesticides in horseradish. The sample was extracted with a mixture of ethyl acetate and acetonitrile (15+85), and the extract was purified with PSA, activated carbon and anhydrous sodium sulfate. After speedy centrifugation, the supernatant was concentrated and made up to 1.0 mL with methylbenzene. VF-5MS column was used for separation, and MS/MS was used for determination with internal standard method for quantification. Values of lower limits of determination (10S/N) found were in the range of 0.005-0.1 mg·kg-1. Tests for recovery were made by addition of pesticide standards at 4 different concentration levels to blank sample of horseradish as matrixes, values of recovery found were in the range of 61.1%-120%, with values of RSD′s (n=7) in the range of 2.9% to 19%.

       

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