食品科学 ›› 2017, Vol. 38 ›› Issue (16): 268-273.doi: 10.7506/spkx1002-6630-201716043

• 安全检测 • 上一篇    下一篇

分散固相净化与气相色谱测定竹笋中21 种农药残留

沈丹玉,袁新跃,刘毅华,钟冬莲,莫润宏,汤富彬   

  1. (1.中国林业科学研究院亚热带林业研究所,浙江?杭州 311400;2.杭州市富阳区食品安全检验检测中心,浙江?杭州 311400)
  • 出版日期:2017-08-25 发布日期:2017-08-18
  • 基金资助:
    浙江省公益技术研究项目(2015C32071);公益性行业(林业)科研专项(201304705)

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

SHEN Danyu, YUAN Xinyue, LIU Yihua, ZHONG Donglian, MO Runhong, TANG Fubin   

  1. (1. Research Institute of Subtropical Forestry, Chinese Academy of Forestry, Hangzhou 311400, China; 2. Testing Center for Food Safety of Fuyang District of Hangzhou, Hangzhou 311400, China)
  • Online:2017-08-25 Published:2017-08-18

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%。

关键词: 净化, 竹笋, 农药残留

Abstract: An analytical method was developed for the determination of 21 pesticide 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 the 21 pesticides could be completely separated with an excellent linear relationship. The limits of detection (LODs) and quantification (LOQs) for the 21 pesticides were in the range of 0.079–1.77 and 0.26–5.89 μg/kg, respectively. For all spiked samples, mean recoveries were 92.97% with relative standard deviations (RSDs, n = 3) of less than 6.07%. The presented method was successfully applied to analyze 230 samples from China’s main bamboo shoot-producing regions. Apart?from fenvalerate, all the pesticides were detected from the 230 samples. p,p’-DDE (33.48%), δ-BHC (26.52%) and cyhalothrin (26.09%) showed high detection rates. Buprofezin was detected in the highest concentration of 9 508.9 μg/kg, which showed the largest percentage increase (6.69%) compared to the maximum residue limit.

Key words: clean-up, bamboo shoot, pesticide residues

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