【作者】 车自力；

【导师】 张云怀；

【作者基本信息】 重庆大学 ， 环境科学， 2007， 硕士

【摘要】 基质固相分散(MSPD)是近几年发展起来的一种新的样品前处理技术,对固体、半固体或粘性液体样品中目标物质分析具有独特的特性,在现代农药残留分析中应用越来越广泛。本文研究了含硫蔬菜中有机磷农药残留检测分析技术,解决了目前含硫蔬菜中有机磷农药残留分析中的有机硫干扰对分析的干扰,建立了藠头中多种有机磷农药基质固相分散/气相色谱法测定方法。1、实验对固相萃取和基质固相分散萃取两种处理方法进行了比较,结果表明基质固相分散方法对藠头样品进行处理,可以有效去除其中的有机硫对分析检测的干扰,添加回收率高。2、实验选用了采用弗罗里硅土、中性氧化铝两种固体吸附剂以及石油醚、正已烷、二氯甲烷、乙醚、乙酸乙酯五种常用的有机溶剂进行洗脱。通过实验得出:○1甲拌磷、治螟磷、乐果、毒死蜱、马拉硫磷、对硫磷6种有机磷农药在中性氧化铝柱上大多有机磷农药残留的添加回收率低于在弗罗里硅土柱上的添加回收率;○2 6种有机磷农药在乙酸乙酯和乙醚中的回收率比其它的要高,洗脱剂的洗脱用量在30ml时效果;○3 6种有机磷农药的添加回收率在85.8.%~101.1%之间,相对标准偏差为3.3?8.5。3、建立了藠头中甲拌磷、治螟磷、二嗪磷、乙拌磷、异稻瘟净、皮绳磷、毒死蜱、马拉硫磷、对硫磷、甲基异柳磷、稻丰散、乙硫磷、三硫磷、三唑磷、苯硫磷、喹硫磷16种有机磷农药残留的分析检测方法。固体吸附选用弗罗里硅土5.0g,洗脱剂为乙酸乙酯/正已烷(V/V=2/1)30ml,藠头样品2.0g,16种有机磷农药的添加回收率在73.8.%~112.8%之间,相对标准偏差为3.6?9.3 ,最低检测限为0.009?0.032mg/kg,相关系数为0.9905~0.9994。4、对洋葱、青葱、韭菜等含硫蔬菜用基质固相分散方法进行处理,该方法对洋葱、青葱、韭菜等蔬菜中有机硫干扰物的去除效果好;青葱、韭菜类叶绿素含量高的蔬菜样品的处理时必需串接活性炭,才能去除其中叶绿素,活性炭最佳用量为2g。更多还原

【Abstract】 Matrix solid-phase dispersion (MSPD) is one kind of new pretreatment technology developing over the past few years,which has unique property in solid, half solid or viscidity liquid. Its application is broader in modern pesticide residue analysis. The analysis technology of organic phosphorous pesticides residues in sulfur-containing vegetables was studied. It resolved the problem of organic sulphur during the analysis process of organic phosphorus pesticide residues in sulfur-containing vegetables. The determination method of multi-organic phosphorus pesticide residues in allium chinese with MSPD/GC were established.1. Through the comparison to the solid phase extract and the matrix solid phase dispersion, the experimental result indicated that the method of the matrix solid phase dispersion can effectively clear up the organic sulphur in sulfur-containing vegetables, and obtain a high adds recovery.2. Two solid-phase sorbets (florisil and neutral aluminum oxide), five eluents (petroleum ether, hexane, methylene dichloride, aether, ethyl acetate) was selected in the experiments. Obtaining the bellowing conclusions through the experiment :( a) Six kinds of organic phosphorus pesticide residues (Phorate, sulfotepp, dimethoate, chlorpyrifos, malathion, parathion) has higher recovery in flosiril than neutral aluminum oxide. (b) The effect of recovery with six kinds of organic phosphorus pesticide residues was better in aether and ethyl acetate than in the others. The best dosage of eluent was 30ml. (c) The adds recovery of six organic phosphorus pesticide residues was 85.8%~ 101.1%, and the RSD was 3.3?8.5。3. The determination method of 16 organic phosphorus pesticide residues (Phorate, sulfotepp, diazinon, disulfotion, iprobenfos, fenchlorphos, chlorpyrifos, malathion, parathion, quinalphos, phenthoate, ethion, carbophenothion, triazophos, EPN, isofenphos methyl) in allium chinese with MSPD/GC was established. The optimized analysis condition: solid-phase sorbets of florisil 5.0g, ethyl acetate / hexane (V/V=2/1) 30ml, allium chinese sample 2.0g. The adds recovery of sixteen organic phosphorus pesticide residues was 73.8.%~112.8%, the RSD was3.6?9.3,MRL was 0.009?0.032mg/kg,and correlation coefficient was 0.9905~0.9994。4. With the matrix solid-phase dispersion method processing onion, the blue onion, the leek, etc,the matrix solid phase dispersion can removes the disturbance organic sulphur from sulfur-containing vegetables. The blue onion, the leek, and so on, include more chlorophyll, therefore this kind of vegetables sample processing need connect the activated charcoal and can achieve a better processing effect, the activated charcoal best amount was 2g.更多还原