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  

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

作　　者：王素利[1] 潘灿平[1] 李莉[1] 江树人[1] 钱传范[1] 刘丰茂[1] 

机构地区：[1]中国农业大学理学院

出　　处：《分析测试学报》2007年第6期808-812,共5页Journal of Instrumental Analysis

摘　　要：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—5mg／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—0．2mg／kg和0．002—0．01mg／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。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.

关 键 词：基质固相分散(MSPD) 杀菌剂 蔬菜 水果 高效液相色谱 液相色谱-质谱 

分 类 号：O657.72[理学—分析化学] S482.2[理学—化学]