摘要
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,快速分离富集桔子和蚯蚓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(250mm×4.6mm,粒径:5μm)液相色谱柱,以甲醇∶水∶三乙胺=79∶20∶1(v/v)为流动相,流速0.6mL/min,270 nm波长下检测。得到方法的线性范围0.005～0.2μg/mL,最低检出限为5 ng/mL,加标回收率92.5%～105%,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降解情况的检测方法。
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 method was developed chromatography was carried out on an SB-Phenyl C18（250mm ×4.6mm,5μm） column,methanol-water –triethylamine=79∶ 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（0.005~0.2 μg/mL） with r2= 0.9996,a low detection limit（5 ng/mL,S/N = 3） and the addition recovery was obtained in the range of 92.5%~105%.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.
出处
《安徽农学通报》
2011年第9期32-35,44,共5页
Anhui Agricultural Science Bulletin
关键词
蚍虫啉
农药残留
高效液相色谱法
前处理
Imidacloprid
Pesticide residue
High performance liquid chromatography
Preparation technique
