QuEChERS/液相色谱-串联质谱法测定热带水果中抑霉唑和嘧霉胺的残留量

Determination of Imazalil and Pyrimethanil in Tropical Fruits with Liquid Chromatography Tandem Mass Spectrometry Using QuEChERS

建立了QuEChERS/高效液相色谱-串联质谱法同时测定木瓜、菠萝、龙眼、芒果等4种热带水果中抑霉唑、嘧霉胺残留量的方法。待测样品用含1%冰乙酸的乙腈提取,乙二胺-N-丙基硅烷(PSA)吸附剂除杂,采用电喷雾离子源(ESI)、多反应监测正离子模式扫描,外标法定量。抑霉唑、嘧霉胺0 ng/mL^20 ng/mL范围内质量浓度与峰面积呈良好的线性关系,方法的检出限为0.005 mg/kg。添加水平为0.005 mg/kg,0.010 mg/kg,0.020 mg/kg时抑霉唑、嘧霉胺的平均回收率在85.2%~101%,相对标准偏差在3.7%~11%,符合农药残留检测要求。方法快速、简便、准确,可用于热带水果中抑霉唑、嘧霉胺残留量的定性、定量检测。

A performance liquid chromatography tandem mass spectrometry method using QuEChERS was established forthe simultaneous determination of imazalil and pyrimethanil in several tropical fruit matrixes, such as pawpaw, pineapple,longan and mango. The sample was extracted with acetonitrile containe 1% glacial acetic acid. And PSA was used for cleaning-up.Then the analysis was carried out with electron spray ionization （ESI） under the multiple reaction monitoring （MRM） modesby employing external method. The calibration curve was linear in the range of 0 ng/mL-20 ng/mL. The limits of detection（LOD） for two pesticides were 0.005 mg/kg. The average recoveries and the relative standard derivation （RSDs） of the targetpesticides were between 85.2% -101% and 3.7%-11% when the spiked level were 0.005 mg/kg, 0.010 mg/kg and 0.020 mg/kg. The method could satisfy the residue request. And it was fast, convenient and accurate. It could be used as a reliablemeans for simultaneous quantitative determination of imazalil and pyrimethanil in tropical fruits.