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    超高效液相色谱-串联质谱法同时测定水产品中9种有机磷农药残留量

    Simultaneous UHPLC-MS/MS Determination of Residual Amounts of 9 Organophosphorus Pesticides in Aquatic Products

    • 摘要: 采用超高效液相色谱-串联质谱法同时测定水产品中吡菌磷、伏杀硫磷、乙硫磷、甲基嘧啶磷、速灭磷、杀扑磷、亚胺硫磷、二嗪磷、治螟磷等9种有机磷农药残留量。水产品样品用冰乙酸-乙腈(1+99)混合液提取,加入乙二胺-N-丙基硅烷(PSA)吸附剂净化,所得样液用超高效液相色谱分离,电喷雾串联四极杆质谱进行检测。9种有机磷农药的质量浓度均在18 μg·L-1以内与峰面积呈线性关系,方法的检出限(3S/N)为0.005 mg·kg-1。以水产品样品为基体进行回收试验,方法的回收率在87.5%~102%之间,相对标准偏差(n=10)在3.7%~13%之间。

       

      Abstract: UHPLC-MS/MS was applied to the determination of residual amounts of 9 organophosphorus pesticides, including pyrazophos, phosalone, ethion, pirimiphos methyl, mevinphos, methidathion, phosmet, diazinon and sulfotep, in aquatic products. The sample was extracted with a mixture of glacial acetic acid-acetonitrile (1+99) and purified by adsorbing agent PSA. The sample solution obtained was separated by UHPLC and analyzed by MS/MS. Linear relationships between values of peak area and mass concentration of the 9 organophosphorus pesticides were found in the same range within 18 μg·L-1, with their detection limits (3S/N) of 0.005 mg·kg-1. Using aquatic products as matrixes, test for recovery was made by standard addition method, giving recovery in the range of 87.5%-102% with RSD′s (n=10) in the range of 3.7%-13%.

       

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