茶叶科学2017，Vol.37Issue(3)：243-250,8.
超声辅助-漂浮固化分散液液微萃取-气相色谱法测定茶叶中5种拟除虫菊酯类农药残留
Ultrasound-assisted Dispersive Liquid-liquid Microextraction Based on the Solidification of a Floating Organic Droplet Followed by Gas Chromatography for the Determination of Five Pyrethroid Pesticides in Tea Samples
摘要
Abstract
A novel ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet method (UA-DLLME-SFO) which combined with gas chromatography coupled with ECD detector was developed for the determination of five pyrethroid pesticides (fenpropathrin, cyfluthrin, cyhalothrin, fenvalerate, deltamethrin) in tea. The optimal liquid-liquid microextraction experiment conditions were as follows: 20 μL hexadecane was used as extraction solvent. After ultrasound for 30 min under 35℃, 800 μL of acetone (disersive solvent) were rapidly transferred. The NaCl Mass Fraction was 4% and pH was adjusted to 4. The sample solution was then centrigugated at 10000 r·min-1 for 5 min under -3℃ and then injected for gas chromatography analysis. It was shown that a good linearity for these pyrethroids was obtained at concentrations of 1.0 to 150.0 μg·kg-1 with correlation coefficients higher than 0.9994. The average recoveries of the 5 pesticides in liquid milk were in the range of 92.3% to 99.6% at spiked levels between 1 to 5 μg·kg-1, with intra-day relative standard deviations lower than 3.5%(n=6)and inter-day relative standard deviations lower than 5.9% (n=3). The limits of detection and quantification were 0.11-0.24 μg·kg-1 and 0.36-0.81 μg·kg-1 , respectively. The proposed method is simple, fast, safe, reliable and applicable for analyzing pyrethroid pesticides in tea samples.关键词
超声辅助/漂浮固化分散液液微萃取/气相色谱/拟除虫菊酯Key words
ultrasound-assisted/DLLME-SFO/gas chromatography/pyrethroid pesticides分类
轻工纺织引用本文复制引用
高玉玲,郭秀娟,乔石,孙鹏..超声辅助-漂浮固化分散液液微萃取-气相色谱法测定茶叶中5种拟除虫菊酯类农药残留[J].茶叶科学,2017,37(3):243-250,8.基金项目
牡丹江市科技计划指导项目(Z2016n0017)、大庆市科技计划指导项目(szdfy-2015-50)、校内培育课题资助计划(XZR2014-17) （Z2016n0017）
