食品科学 ›› 2009, Vol. 30 ›› Issue (24): 351-354.doi: 10.7506/spkx1002-6630-200924078

• 分析检测 • 上一篇    下一篇

ASE-GPC-GC 法测定大豆及豆制品中六六六、滴滴涕农药残留

魏冬旭1,2,江连洲1,3,*,郭 伟1,孟冰冰2,胡少新1   

  1. 1.东北农业大学食品学院 2.黑龙江出入境检验检疫局检验检疫技术中心 3.中国大豆工程技术中心
  • 收稿日期:2008-12-23 修回日期:2009-08-13 出版日期:2009-12-15 发布日期:2010-12-29
  • 通讯作者: 江连洲 E-mail:jlzname@163.com

Simultaneous Determination of 8 HCH and DDT Residues in Soybean and Soybean Products with ASE-GPC Coupled with Gas Chromatography

WEI Dong-xu1,2,JIANG Lian-zhou1,3,* GUO Wei1,MENG Bing-bing2,HU Shao-xin1   

  1. 1. School of Food, Northeast Agricultural University, Harbin 150030, China;
    2. Inspection and Quarantine Center, Heilongjiang Entry-Exit Inspection and Quarantine Bureau, Harbin 150001, China;
    3. National Research Centre of Soybean Engineering and Technology, Harbin 150086, China
  • Received:2008-12-23 Revised:2009-08-13 Online:2009-12-15 Published:2010-12-29
  • Contact: JIANG Lian-zhou1,3,* E-mail:jlzname@163.com

摘要:

建立一种同时测定大豆及豆制品中α -HCH、β -HCH、γ -HCH、δ -HCH、ρ,ρ′-DDE、ρ,ρ′-DDD、ο,ρ′-DDT、ρ,ρ′-DDT 8 种有机氯农药残留的气相色谱分析方法。样品经加速溶剂系统萃取(ASE)和凝胶渗透色谱净化(GPC)后,采用气相色谱配备电子捕获检测器进行分离测定。0.005~0.100mg/kg 范围内各残留药物线性良好,相关系数r 均在0.9990 以上;在0.005、0.020、0.050mg/kg 3 个加标水平下进行了方法验证,平均回收率为78.3%~107.6%,相对标准偏差为2.1%~5.5%;方法检测限(LOD)为0.2~1.8μg/kg。该方法重现性好、灵敏度高、分析迅速,各项指标均满足国内外法规要求,适用于大豆及豆制品中六六六和滴滴涕残留的分析检测。

关键词: 大豆及豆制品, 加速溶剂萃取, 凝胶渗透色谱, 气相色谱, 六六六, 滴滴涕

Abstract:

A method for the determination of 8 HCH and DDT in soybean and soybean products was established with accelerated solvent extraction (ASE), auto gel permeation chromatography purification (GPC) and gas chromatography quantification. The calibration curves presented good linear relationship in the range of 0.005-0.100 mg/kg, and the correlation coefficients were above 0.9990 for all compounds. Recoveries of all added were 78.3%-107.6% respectively, and relative standard deviations (RSD) were 2.1%-5.5% with spiked at 0.005, 0.020, 0.050 mg/kg of HCH and DDT in blank samples. The limit of detection of the method were 0.2 - 1.8μg/kg. The method was of good reproducibility, high sensitivity, shorter analysis time, and its performance could meet the requirements of the domestic and international legislation.

Key words: soybean and soybean products, accelerated solvent extraction (ASE), gel permeation chromatography (GPC), gas chromatography (GC), hexachlorocyclohexane (HCH), dichlorodiphenyl trichloroethane (DDT)

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