液相微萃取—高效液相色谱法测定环境中的吡虫啉.doc

液相微萃取—高效液相色谱法测定环境中的吡虫啉摘 要本文研究了基于三相中空纤维磁力搅拌的新型液相微萃取(LPME)模式，采用磷酸二氢钾作接受液，快速分离富集稻谷、稻叶、水和土壤中吡虫啉农药残留的前处理技术，以高效液相色谱（HPLC）为检测手段。系统地优化了LPME技术的有机溶剂、搅拌速率和萃取时间等条件。最佳色谱条件为：SB-Phenyl C18（250×4.6mm i.d.,5μm）液相色谱柱，以甲醇：水：三乙胺(80：20：1，v：v)为流动相，流速0.8 ml／min,270 nm波长下检测。得到方法的线性范围0.0001～0.2 μg/m，最低检出限为5g/ml（S/N=3），加标回收率98. 3%～101. 5%，富集倍数19.2倍。建立了一种简单、快速、准确、环境友好的农药残留检测方法。关键词吡虫啉 农药残留 中空纤维 前处理 液相微萃取 The Determination of Imidacloprid in Environment Based on Three-phase Hollow Fiber Liquid Phase Microextraction-High Performance Liquid Chromatography Chen chenglong (Applied Chemistry Department ,Eastchina Institute of Techonology ,Fuzhuo,JX344000) Abstract: A novel method for fast separate and enrichment imidacloprid in paddy，leaf，water and soil was established by using high performance liquid chromatography (HPLC) coupled with a three-phase hollow fiber based liquid phase microextraction (TP-HF-LPME) technique for sample preparation. Parameters related to TP-HF-LPME (organic solvent， stirring speed，pH of donor and acceptor phase， extraction time) were also optimized experimentally. The proposed method integrates extraction，enrichment and clean-up into a single step. The method was developed chromatography was carried out on an SB-Phenyl C18 (250mm ×4.6mm i.d.，5μm ) column，methanol-water –triethylamine，(80∶20：1, V ：V) as mobile phase and detection at 270nm. It has been demonstrated to be a very fast，effective and virtually “green” sample preparation technique, which provided a good linear range (0.0001～0.2 μg/ml) with r2 = 0.9997 a low detection limit(5 ng/ml, S/N = 3)，RSD=1.2% and the addition recovery was obtained in the range of 98.30-101.5%. The proposed method integrates extraction, enrichment and clean-up into a single step， which is a simple，effective，veracious and environmental method for detecting pesticide residue. Keywords： imidacloprid pesticide residue hollow fiber pretreatment liquid phase microextraction 目录 1．前言.. 5 1．1 吡虫啉简介. 5 1．2 液相微萃取(LPME) 5 1．2．1 液相微萃取的发展历史 5 1．2