文献类型：期刊文献

中文题名：分散固相净化与气相色谱测定竹笋中21种农药残留

英文题名：Determination of 21 Pesticide Residues in Bamboo Shoots by Dispersive Solid Phase Extraction Cleanup and Gas Chromatography

作者：沈丹玉[1] 袁新跃[2] 刘毅华[1] 钟冬莲[1] 莫润宏[1] 汤富彬[1]

第一作者：沈丹玉

通信作者：Tang, Fubin

机构：[1]中国林业科学研究院亚热带林业研究所;[2]杭州市富阳区食品安全检验检测中心

年份：2017

卷号：38

期号：16

起止页码：268-273

中文期刊名：食品科学

外文期刊名：Food Science

收录：CSTPCD;;EI(收录号：20174104259828);Scopus;北大核心:【北大核心2014】；CSCD:【CSCD_E2017_2018】；

基金：浙江省公益技术研究项目(2015C32071);公益性行业(林业)科研专项(201304705)

语种：中文

中文关键词：净化;竹笋;农药残留

外文关键词：clean-up; bamboo shoot; pesticide residues

分类号：TS207.5

摘要：通过比较不同吸附剂对竹笋提取液的净化效果和对电子捕获检测器(electron capture detector,ECD)基线的影响,建立竹笋中21种有机氯和拟除虫菊酯类农药残留的气相色谱分析方法。竹笋样品用乙腈提取,加入无水硫酸镁、弗罗里硅土、N-丙基二乙胺(primary secondary amine,PSA)、强阳离子、石墨化炭黑进行分散固相净化,气相色谱-ECD测定。方法学结果表明,竹笋中21种有机氯和拟除虫菊酯农药具有良好的线性关系,检出限为0.079~1.77 μg/kg,定量限为0.26~5.89 μg/kg,经PSA净化平均回收率为92.97%,相对标准偏差为1.06%~6.07%。方法应用于我国竹笋主产区的质量安全风险监测,230个样品中,除了氰戊菊酯,其余农药均有不同程度的检出,其中检出率最高的是p,p′-滴滴伊(33.48%)、δ-六六六(26.52%)和氯氟氰菊酯(26.09%);检出含量和超标率最高的是噻嗪酮,为9 508.9 μg/kg和6.96%。
An analytical method was developed for the determination of21pesticide residues in bamboo shoot using dispersive solid phase extraction clean-up combined with gas chromatography(GC).To optimize this method,we compared the effects of different adsorbents on the purification of bamboo shoot extract and clean-up and the baseline of electron capture detector(ECD).Bamboo shoot samples were extracted with acetonitrile,followed by clean-up by dispersive solid phase extraction with anhydrous MgSO4,Florisil,primary secondary amine(PSA),strong cation exchange(SCX)or Pesticarb and subsequent determination by GC-ECD.All the21pesticides could be completely separated with an excellent linear relationship.The limits of detection(LODs)and quantification(LOQs)for the21pesticides were in the range of0.079-1.77and0.26-5.89μg/kg,respectively.For all spiked samples,mean recoveries were92.97%with relative standard deviations(RSDs,n=3)of less than6.07%.The presented method was successfully applied to analyze230samples from China's main bamboo shoot-producing regions.Apart from fenvalerate,all the pesticides were detected from the230samples.p,p'-DDE(33.48%),δ-BHC(26.52%)and cyhalothrin(26.09%)showed high detection rates.Buprofezin was detected in the highest concentration of9508.9μg/kg,which showed the largest percentage increase(6.69%)compared to the maximum residue limit.