分散固相萃取-气相色谱-质谱法测定大豆油中102种农药残留量

Determination of Residual Amounts of 102 Pesticides in Soybean Oil by Gas Chromatography-Mass Spectrometry

建立了分散固相萃取-气相色谱-质谱法快速检测大豆油中102种农药残留的分析方法。样品用正己烷溶解,乙腈反萃取,C18和PSA粉末分散固相萃取净化后供气相色谱-质谱仪(GC-MS)分析。采用选择离子扫描方式,外标法定量。该方法简便、快速,通过优化前处理和上机条件,在最优条件下进行测试,方法的定量下限(S/N≥10)为0.01～0.05 mg/kg,在加标水平为0.05 mg/kg时,方法回收率为60.8%～124%,相对标准偏差为2.7%～14%。

A method was reported that muhiresidual pesticides in soybean oil were pretreated quickly and results were determinated hy gas chromatography hyphenated with mass spectrometry, （GC-MS）.The soybean oil was dissolved by n-hexane,extraeted with acetonitrile.The clear supematant liquid purified by C18 and PSA powder was ready for GC-MS analysis.Determinations were performod hy using selected ion monitoring （SIM） mode and external standard method was used in the quantification.After investigating the conditions of pretreatment and determination,the method was convenient and rapid. Under the optimal conditions,the detection limits for the method （S/N≥ 10）of pesticides were in the ranges of 0.01 ~ 0.05 mg/kg,Tests tor recovery were made by addition of mix standards of 0.05 mg/kg, the results were 60.8% ~ 124%,the relative standard deviations were 2.7% - 14%.