固相萃取-气相色谱-串联质谱检测方法测定水果中甲基异柳磷

Determination of Isofenphos-methyl in Fruit by Solid Phase Extraction-gas Chromatography-tANDem Mass Spectrometry

建立了固相萃取-气相色谱-串联质谱测定水果中甲基异柳磷的检测方法。样品经乙腈提取、盐析、离心后,取上层有机相,经固相萃取柱净化后浓缩,选用HP-5MS超惰性毛细管柱对待测物进行分离,经EI离子源电离后经多反应监测(MRM)模式检测。该方法在2~50ng/mL范围内线性关系良好,相关系数0.999,定量限为0.2μg/kg,平均加标回收率范围为83.2%~109.5%,相对偏差在2.5%~8.8%之间。该方法准确、灵敏,抗干扰性高,适用于水果快速定性和定量分析。

A method for determination of isofenphos- methyl in fruits by solid phase extraction-gas chromatography-tandem mass spectrometry was established. The samples were extracted by acetonitrile,salted out and centrifuged.The upper organic phase was taken and concentrated after purification by solid phase extraction column.HP-5 MS super-inert capillary column was used for the separation of the measured substance, then detected by multiple-reaction monitoring (MRM) in electron ionization mode.The calibration curve was linear in the range of 2~50 ng/mL,r≥0.999,The limits of quantification was 0.2 μg/kg.The average recoveries were in the range of 83.2 %~109.5 % and the relative standard deviation was in the range of 2.5 %~8.8 %.This method is accurate,sensitive,high anti-interference and suitable for fast qualitative and quantitative analysis of fruit.