凝胶渗透色谱-气相色谱-质谱方法测定茶叶中五种高毒有机磷农药残留  被引量:3

Determination of Five High-toxic Organic Phosphorus Pesticides Residues in Tea by Gel Permeation Chromatography and Gas Chromatography-mass Spectrometry

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作  者:邹孝[1,2] 高熹[1] 刘小文[1] 肖昭竟 段云鹏 胡羽 吴国星[1] 叶敏[1] 肖春[1] 李正跃[1] 

机构地区:[1]云南农业大学植物保护学院,云南昆明650201 [2]重庆市计量质量检测研究院,重庆400200

出  处:《广东化工》2011年第10期135-136,113,共3页Guangdong Chemical Industry

基  金:国家自然科学基金项目(30960221);云南省基金项目(2008CD135);云南省森林灾害预警与控制重点实验室开放基金(ZK10A305)

摘  要:本研究建立了以凝胶渗透色谱(gel permeation chromatography,GPC)为样品前处理方法,同时以气相色谱-质谱联用(gas chromatography-mass spectrometry,GC-MS)技术分析茶叶中五种高毒有机磷农药残留量的方法。样品用丙酮提取,共提物用乙酸乙酯:环己烷(1:1,V/V)作流动相的GPC净化,脱水浓缩定容,采用气相色谱-质谱联用,在选择离子监测模式下进行检测,用外标法定量。结果表明,浓度与其峰面积在0.005~0.500 mg/L范围内具有良好的线性关系,3个添加水平的平均回收率分别为:99.68%~106.31%,94.14%~98.11%,93.86%~98.21%,相对标准偏差(RSD)均小于10%,检出限为0.0005~0.0020 mg/kg。A multiresidue method based on gel permeation chromatography(GPC) for the sample preparation and gas chromatography-mass spectrometry analysis was developed to determine five high-toxic organic phosphorus pesticides residues in tea.The sample were extracted using acetone.Then the extracts were eluted with ethyl acetate/cyclohexane(1:1) by GPC.After dehydrated and concentrated to a definite volume,the pesticides were finally determined by gas chromatography-mass spectrometry in selective-ion Monitor(SIM) simultaneously,and quantified by external standard method.The results showed a good linear relationship was obtained between concentration and peak area within the 0.005~0.500 mg/L range.Average recoveries of 5 pesticides at three fortified levels were 99.68 %~106.31 %,94.14 %~98.11 % and 93.86 %~98.21 %,respectively.The relative standard deviation of the method was less than 10 % in every case,respectively.The limits of detection of 5 pesticides were ranging from 0.0005~0.0020 mg/kg.

关 键 词:凝胶渗透色谱 气相色谱-质谱联用 茶叶 高毒有机磷农药 多残留 

分 类 号:O657[理学—分析化学]

 

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