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气相色谱-负离子化学电离质谱法对咖啡中8种有机氯农药的检测

Determination of 8 Organochlorine Pesticides in Coffee by Gas Chromatography-Negative Chemical Ionization Mass Spectrometry

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【作者】 周瑞泽佟玲李重九马晓东

【Author】 ZHOU Rui-ze~1,TONG Ling~2,LI Chong-jiu~1,MA Xiao-dong~1 (1.College of Science,China Agricultural University,Beijing 100193,China; 2.National Research Center for Geoanalysis,Beijing 100037,China)

【机构】 中国农业大学理学院国家地质实验测试中心

【摘要】 <正>近年来,食品中的农药残留问题受到越来越多的重视。国内外关于水果蔬菜等食品中的农药残留研究多集中于对食品原料的报道。尽管有机氯农药已禁用多年,但因其化学性质稳定、脂溶性强、易在环境和生物体中富集,至今仍能在大气、水体及土壤中检出。咖啡为一种加工的、在日常生活中直接泡饮的食品,在其加工过程中的各个环节都可能受到污染。迄今为止,国内外有关咖啡的残留分析研究报道不多,首先因为人们对咖啡的关注较少,其次咖啡比一般的植物性产品成分复杂,颗粒较细,油脂及色素含量较高,样品中被测物浓度较低。

【Abstract】 An efficient and selective analytical method for the determination of 8 organochlorines pesticides residues (α-666,β-666,γ-666,δ-666,o,p’-DDT,p,p’-DDT,p,p’-DDD,p,p’-DDE) in coffee has been developed. The coffee samples were extracted with hexane - acetone(1:1,by volume) according to a selective extraction step using accelerated solvent extraction(ASE),followed by a clean-up by gel permeation chromatography (GPC) and a column combined with Florisil and GCB.Identification and quantification were performed using gas chromatography with negative chemical ionization mass spectrometric detection(GC - NCI MS).The method detection limits varied between 0.002 and 0.069 ng/g.The calibration curves showed a good linearity for all OCPs(r≥0.999 5) under a concentration of 0.20-50.0μg/L.When the spiked levels were 0.5μg/L and 5μg/L,the average recoveries were range of 94%- 110%with RSD of 3.5%- 10.6%.The method was accurate,sensitive and suitable for the analysis of pesticides.

【Key words】 GC-NCI MSorganochlorine pesticidescoffee
【基金】 中国农业大学本科生科研训练计划(URP)资助项目
  • 【会议录名称】 2008年全国有机质谱学术会议论文集
  • 【会议名称】2008年全国有机质谱学术会议
  • 【会议时间】2008-11-14
  • 【会议地点】中国浙江宁波
  • 【分类号】TS273
  • 【主办单位】中国分析测试协会
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