高效液相色谱串联质谱法测定蔬果中啶酰菌胺和环酰菌胺残留

Determination of Boscalid and Fenhexamid Residues in Fruits and Vegetables by HPLC-MS/MS

建立蔬菜和水果中啶酰菌胺和环酰菌胺的高效液相色谱串联质谱检测方法。将试样中残留的啶酰菌胺和环酰菌胺用含1%乙酸的乙腈溶液均质提取,提取液混合使用乙二胺-N-丙基硅烷和十八烷基硅烷键合相基质分散净化,用高效液相色谱串联质谱检测和确证,外标法定量;方法通过空白基质溶液稀释标准建立校正的标准曲线,以消除基质效应。结果表明:啶酰菌胺和环酰菌胺在1～100μg/L范围内具有良好的线性关系,相关系数分别为0.9996和0.9997;在5～50μg/kg范围内,平均添加回收率在77.7%～93.8%之间,相对标准偏差在2.1%～6.3%之间。啶酰菌胺和环酰菌胺方法定量限分别为1.32μg/kg和1.20μg/kg,检出限分别为0.395μg/kg和0.361μg/kg。

A liquid chromatography-tandem mass spectrometry method was established to determine boscalid and fenhexamid residues in fruits and vegetables.Analytes were extracted from samples using 1% acetic acid acetonitrile,and then purified by solid phase extraction cartridge packaged with sorbent primary secondary amine（PSA） and C18.The residues were determined by high-performance liquid chromatography coupled with tandem MS（HPLC-MS/MS） using external standard method,and the interference of matrix was deducted by the matrix-matched calibration standards curve.A good linearity of calibration curve was exhibited over a concentration range of 1μg/L to 100μg/L for boscalid and fenhexamid with a correlation coefficient of 0.9996 and 0.9997,respectively.Average recoveries for boscalid and fenhexamid in 4 samples at spiked levels of 5-50 μg/kg were between 77.7% and 93.8%,with a relative standard deviations between 2.1% and 6.3%.For boscalid and fenhexamid,the limit of quantification were 1.32,1.20 μg/kg and the limit of detection were 0.395,0.361 μg/kg,respectively.