水果蔬菜中多种杀菌剂的基质固相分散液相色谱测定方法研究

采用基质固相分散(MSPD)代替液液分配和固相萃取,从蔬菜水果中提取、净化10种常用杀菌剂农药残留,用C18硅胶交联剂作为固相吸附剂,乙酸乙酯作为洗脱液,用HPLC/PDA和LC-MS进行分析检测。10种杀菌剂在0.5~5 mg/kg含量的添加回收率在65%~110%之间,相对标准偏差小于10%,使用HPLC、PDA和LC-MS的检出限分别在0.02~0.2 mg/kg和0.002~0.01 mg/kg之间。该方法节省溶剂,提取和净化一步完成,适用于新鲜水果和蔬菜中10种杀菌剂的残留分析。

Determination of Multiple Fungicide Residues in Fruits and Vegetables by Matrix Solid-phase Disperse and Liquid Chromatography with a Photodiode Array Detector(PDA)

An effective and simple analytical method for determination of 10 fungicide residues in fruits and vegetables using matrix solid-phase disperse(MSPD) and liquid chromatography with a photodiode array detector(PDA) was developed.The conventional liquid-liquid extraction and the solid phase extraction were replaced by MSPD for extraction and clean-up of the fungicide residues in fruits and vegetables.The method employed C18 bonded silica as dispersant and ethyl acetate as eluting solvent.The fungicides were identified and quantified using LC/PDA and LC-MS.The recoveries of fortified samples were 65%-110% with lower relative standard deviation(<10%) in the concentration range of 0.5-5 mg/kg.Detection limits ranged from 0.02 to 0.2 mg/kg for HPLC/PDA and 0.005 to 0.02 mg/kg for LC-MS,respectively,and linearity ranged up to 10 mg/kg.The MSPD method in which sample homogenization,extraction and clean-up were carried out simultaneously was low solvent-consuming.It was proved that most fruit and vegetable samples were suitable to be analyzed by this method in this study.