固相萃取-超高效液相色谱-串联质谱法测定花生中10种农药残留

建立了花生中10种农药残留的快速分析方法。样品用乙腈水均质提取,盐析分配,提取液经Envi-18和LC-NH2复合固相萃取小柱净化后供超高效液相色谱-串联质谱仪(UPLC-MS/MS)分析,电喷雾离子化正离子方式(ESI+)及多反应监测模式(MRM)进行测定,基质匹配标准溶液外标法定量。在最优条件下进行测试,所测项目方法的定量限(S/N≥10)均小于0.01 mg/kg。在加标水平为0.01 mg/kg、0.05 mg/kg和0.20 mg/kg时,方法回收率为71.1%～112%,相对标准偏差为4.5%～17.8%。

Determination of 10 Pesticide Residues in Peanut by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A method for the determination of 10 pesticide residues in peanut was developed by ultra performance liquidchromatography-tandem mass spectrometry （UPLC-MS/MS）. The samples were extracted with acetonitrile-water and separated with salting out method. And then the supernatants were purified using solid-phase extraction prior to the UPLC-MS/MS analysis. The analytes were separated C18 column, indentified by positive electrospray ionization （ESI＋） and multiple reaction monitoring （MRM） mode. The matrix-matched external standard calibration curves were used for quantitative analysis. Under the optimal conditions, the detection limits of the method （S/N ≥ 10） were 0.01 mg/kg. Tests for recovery were carried by addition of standard at concentration of 0.01 mg/kg, 0.05 mg/kg and 0.20 mg/kg,the results were 71.1%-112%, and the relative standard deviations were in the range of 4.5% - 17.8%.