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.
出处
《分析测试学报》
CAS
CSCD
北大核心
2007年第6期808-812,共5页
Journal of Instrumental Analysis