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    搅拌棒吸附萃取-液相色谱-串联质谱法测定微山湖水中的有机磷农药残留

    Determination of Organophosphorus Pesticide Residues in Weishan Lake Water by LC-MS/MS Combined with Stir Bar Sorptive Extraction

    • 摘要: 采用搅拌棒吸附萃取结合液相色谱-串联质谱法测定微山湖水中的马拉硫磷、三唑磷、喹硫磷、伏杀硫磷等4种有机磷农药残留。对影响有机磷农药残留吸附萃取效率的萃取涂层、样品溶液的酸度、振荡速率、萃取时间、溶液的离子强度、解吸液、解吸时间和解吸模式等因素进行了优化,确定了最佳吸附萃取条件。样品经搅拌棒萃取、解吸后,采用ZORBAX Eclipse Plus C18色谱柱分离,在多反应监测模式下检测,外标法定量。4种有机磷农药的质量浓度在一定范围内与峰面积呈线性关系,检出限(3S/N)在0.16~0.73 μg·kg-1之间。加标回收率在72.3%~107%之间,测定值的相对标准偏差(n=6)在7.8%~11%之间。

       

      Abstract: LC-MS/MS coupled with stir bar sorptive extraction (SBSE) was applied to the determination of 4 organophosphorus pesticides residues, including malathion, triazophos, quinalphos and phosalone, in Weishan Lake water. The optimum extraction condition was achieved by optimizing the factors of SBSE efficiency, such as extraction coating, acidity of the sample solution, stirring speed, extraction time, ionic strength of the solution, desorption solution, desorption time and desorption mode. After the sample was extracted by SBSE and desorption, the analytes were separated on a ZORBAX Eclipse Plus C18 chromatographic column. The MS analysis was carried out in the multi reaction monitoring mode and external standard method was used for quantification. Linear relationships were found between the peak areas and the mass concentrations of the 4 organophosphorus pesticides in definited ranges with the detection limits (3S/N) in the range of 0.16-0.73 μg·kg-1. Recovery rates obtained by standard addition method were in the range of 72.3%-107% and RSDs (n=6) were in the range of 7.8%-11%.

       

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