【文洋】基质固相分散法分析茶鲜叶中的农药残..docVIP

基质固相分散法分析茶鲜叶中的10种有机氯和拟除虫菊酯农药残留 文洋2 谭君1,2 刘仲华1,* （1国家植物功能成分利用工程技术研究中心·长沙·410000；2湖南农业大学园艺园林学院·长沙·410128） 摘 要：本文采用气相色谱/电子捕获检测器(GC/ECD)的方法同时检测10种有机氯和拟除虫菊酯类农药，建立了基质固相分散（MSPD）的方法对茶树鲜叶进行样品预处理，对MSPD过程中的分散剂种类、分散剂用量、柱层析方法、洗脱剂、洗脱体积等因素进行了考察，最终确定的最优方案为：1.0g鲜叶与4.0g 中性Al2O3分散剂研磨后，以预填2.0g无水Na2SO4+2.0g Florisil+0.1g活性炭的层析柱净化预分离，其洗脱剂选用20mL乙酸乙酯:正己烷(40%, v:v)混合溶剂。经试验验证，该方法快速、准确、简便、环保，灵敏度高，选择性强，准确度高，重现性好，适用于茶树鲜叶中有机氯和拟除虫菊酯类农残的准确分析。 关键词：茶鲜叶；有机氯；拟除虫菊酯；气相色谱/电子捕获检测器 The Analysis of Ten Organochlorine and Pyrethroid Pesticide Residues in Fresh Tea Leaves by Matrix Solid-phase Dispersion WEN Yang2 , TAN Jun 1,2, LIU Zhonghua 1,* (1. National Research Center of Engineering Technology for Utilization of Botanical Functional Ingredients, Changsha 410128; 2. College of Horticulture and Gardening, Hunan Agricultural University, Changsha 410000) Abstract: GC/ECD was used to determine ten organochlorine and pyrethroid pesticides simultaneously. The Matrix Solid Phase Dispersion (MSPD) method was established to pretreat fresh tea leaves. During the process, the dispersant variety, dispersant dosage, column clean-up, eluant variety and eluant volume were discussed, and the final method was determined. 1.0g fresh tea leaf sample was milled with 4.0g neutral Al2O3. After full dispersion, it was transferred into a glass column pre-packed with 2.0g anhydrous Na2SO4, 2.0g Florisil and 0.1g active carbon. The elution was done by 20mL mixture of ethyl acetate and hexane (40%, v:v). After verified by experiment, the method is rapid, accurate, simple and environmental with high sensitivity, strong selectivity, high accuracy and good repeatability. It is suitable for accurate analysis of organochlorine and pyrethroid pesticide residues in fresh tea leaves. Key words: Fresh tea leaves; Organochlorine; Pyrethroid; Gas chromatography with electron capture detector (GC/ECD)茶叶是我国的重要出口产品之一，但我国茶叶的农药残留量超标问题严重[1]，欧盟等国家地区已经将我国列入农药残留水平较高的国家之一，使我国茶叶出口面临巨大压力[2]，在加大对我国茶叶进口的检查力度的同时，每年都制定了更为严格的农药最高残留限量标准(MRL)[3-5]，使我国茶叶出