QuEChERS-超高效液相色谱-串联质谱方法快速测定小麦中的咪鲜胺残留

Simplified Method for Determination of Fungicide Prochloraz Residues in Wheat Using QuEChERS and UPLC-MS/MS

建立了简便、快速测定咪鲜胺在小麦籽粒中残留量的方法。前处理采用以乙腈作提取剂、PSA(primary secondary amine,N-丙基乙二胺)为分散净化剂的QuEChERS方法,并利用超高效液相色谱-串联质谱(UPLC-MS/MS)在多反应离子监测模式下进行检测,外标法定量。在0.001～0.1mg/kg范围内线性关系良好,相关系数为0.9994。结果表明,在3个添加水平(0.001、0.01和0.1mg/kg)范围内的平均回收率为91.8%～98.3%,相对标准偏差为3.7%～7.0%,咪鲜胺在麦粒中的定量限为0.0001mg/kg。

A simple and rapid method was developed for determining prochloraz residue in wheat.Prochloraz was extracted with acetonitrile and cleaned up with dispersive method on primary secondary amine,detected by ultra liquid chromatography-mass spectrometry under multiple reaction monitoring mode,and quantified by matrix-match standard solution.The correlation coefficient of the calibration curves was 0.999 4 within 0.001 mg/kg to 0.1 mg/kg.The mean recoveries of prochloraz in wheat were 91.8%～98.3%,at three spiked levels （0.001,0.01 and 0.1 mg/kg）.The relative standard deviations （RSD） were 3.7%～7.0% and the limit of quantification （LOQ） of prochloraz in wheat was 0.000 1 mg/kg at the signal/noise （S/N） ratio of 10.