分散固相净化与气相色谱测定竹笋中21种农药残留

发布时间：2018-12-18 00:51

【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%。
[Abstract]:By comparing the effects of different adsorbents on the purification of bamboo shoot extract and the baseline of electron capture detector (electron capture detector,ECD), a gas chromatographic method for the determination of 21 organochlorine and pyrethroid pesticide residues in bamboo shoots was established. Bamboo shoot samples were extracted with acetonitrile and added anhydrous magnesium sulfate, Florisil soil, N-propyldiethylamine (primary secondary amine,PSA), strong cations, graphitized carbon black for solid phase dispersion purification, gas chromatography-ECD determination. The results showed that there was a good linear relationship between 21 organochlorine and pyrethroid pesticides in bamboo shoots, the detection limit was 0.079 ~ 1.77 渭 g / kg, the quantitative limit was 0.26 ~ 5.89 渭 g / kg, and the average recovery by PSA was 92.97%. The relative standard deviation was 1.06 and 6.07. The method was applied to the quality and safety risk monitoring of bamboo shoot production areas in China. In 230 samples, except fenvalerate, the other pesticides were detected in varying degrees, among which the highest detectable rate was Phanophane Didi (33.48%). 未 -hexachlorohexane (26.52%) and cypermethrin (26.09%); Thiazinone was found to have the highest content and over standard rate of 9 508.9 渭 g/kg and 6. 96 渭 g/kg respectively.
【作者单位】：中国林业科学研究院亚热带林业研究所;杭州市富阳区食品安全检验检测中心;
【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)
【分类号】：O657.71;TS255.7

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