食品科学 ›› 2012, Vol. 33 ›› Issue (4): 148-152.doi: 10.7506/spkx1002-6630-201204030

• 分析检测 • 上一篇    下一篇

薏苡仁中多种农药残留的测定

李 俊,王 震,庞宏宇,郭晓关,任玉娟,吴旭刚   

  1. 贵州省农产品质量安全监督检验测试中心,农业部农产品质量安全监督检验测试中心(贵阳)
  • 出版日期:2012-02-25 发布日期:2012-02-14

Determination of Multiple Pesticide Residues in Coix Seed

LI Jun,WANG Zhen,PANG Hong-yu,GUO Xiao-guan,REN Yu-juan,WU Xu-gang   

  1. Guizhou Provincial Supervision and Testing Center for Agricultural Product Quality, Supervision and Testing Center for Agricaltural Product Quality, Ministry of Agriculture (Guiyang), Guiyang 550004, China
  • Online:2012-02-25 Published:2012-02-14

摘要: 建立薏苡仁中多种杀虫剂、杀螨剂等杀菌剂农药残留的分析方法。用快速溶剂萃取仪提取,分别采用固相萃取和凝胶渗透色谱净化,气相质谱联用测定。通过固相萃取净化处理的样品添加回收率为72.45%~111.74%,RSD为1.47%~5.06%;凝胶渗透色谱处理的样品添加回收率为74.70%~106.49%,RSD为1.58%~5.08%;相关系数为0.9902~0.9995,最低检出限为0.002~0.02mg/kg,最低定量限为0.005~0.05mg/kg。方法具有高效、准确、灵敏的特点,适用于薏苡仁中多种农药残留的检测分析。

关键词: 薏苡仁, 农药残留, 快速溶剂萃取仪, 固相萃取(SPE), 凝胶渗透色谱(GPC), 气相质谱联用仪(GC-MS)

Abstract: A method to simultaneously determine 43 pesticide residues in coix seed is described in this paper. Samples were extracted by accelerated solvent extraction (ASE), cleaned up by either solid phase extraction (SPE) or gel permeation chromatography (GPC), and analyzed by gas chromatography-mass spectrometry (GC-MS). The spike recoveries obtained by SPE and GPC were 72.45%-111.74% and 74.70%-106.49%, and the RSDs 1.47%-5.06% and 1.58%-5.08%, respectively.  Correlation coefficients between 1.47% and 5.06% were found for the established calibration curves. The limits of detection (LOD) of the method varied from 0.002 to 0.02 mg/kg, and the limits of quantification (LOQ) from 0.005 to 0.05 mg/kg. The method was efficient, accurate, sensitive and applicable for the simultaneous determination of multiple pesticide residues in coix seed.

Key words: coix seed, pesticide residue, accelerated solvent extraction (ASE), solid phase extraction (SPE), gel permeation chromatography (GPC), gas chromatography-mass spectrometry (GC-MS)

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