农药学学报2016，Vol.18Issue(4)：497-502,6.DOI:10.16801/j.issn.1008-7303.2016.0069
漂浮固化分散液-液微萃取-气相色谱法测定液态奶中5种拟除虫菊酯类农药残留
Dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet followed by gas chromatography for the determination of five pyrethroid pesticides residues in liquid milk samples
摘要
Abstract
A novel dispersive liquid-liquid microextraction based on solidification of floating organic droplet method (DLLME-SFO) combined with gas chromatography coupled with ECD detector was developed for the determination of five pyrethroid pesticides (fenpropathrin, cyhalothrin, cyfluthrin, fenvalerate, deltamethrin) in liquid milk. The following procedure was used for the sample pretratment:25 μL hexadecane (extraction solvent), 600 μL acetone(dispersive solvent), and NaCl (6 wt%) were added, followed by vortex oscillation extraction time 3 min. Then centrifugal for 3 min at –5℃ and 10 000 r/min, and dislodge water phase. After thawed, the sample was analysis by gas chromatography. Good linearity was obtained at concentrations from 5.00 to 250 μg/kg with correlation coefficients higher than 0.999 0 for these pyrethroids. The average recoveries of the 5 pesticides in liquid milk were in the range between 90% and 104% at spiked levels of 5 to 20 μg/kg, with intra-day relative standard deviations lower than 5.9% (n = 6) and inter-day relative standard deviations lower than 7.8% (n = 3). The limits of detection and quantification were 0.75-2.17 μg/kg and 2.52-7.22 μg/kg, respectively. This new method is simple, solvent saving, accurate, reliable and applicable for the analysis of pyrethroid pesticides in liquid milk samples.关键词
漂浮固化分散液-液微萃取/气相色谱/液态奶/拟除虫菊酯类农药/残留Key words
dispersive liquid-liquid microextraction based on solidification of floating/gas chromatography/liquid milk/pyrethroid pesticides/residue分类
农业科技引用本文复制引用
孙鹏,高玉玲,王金梅,刘秀娟..漂浮固化分散液-液微萃取-气相色谱法测定液态奶中5种拟除虫菊酯类农药残留[J].农药学学报,2016,18(4):497-502,6.基金项目
大庆市指导性科技计划项目(szdfy-2015-50)；校内培育课题资助计划(XZR2014-17) （szdfy-2015-50）
