环境水、蔬菜中有机磷杀虫剂农药残留的分离检测
摘要
目前,全世界有机磷农药达30多种,广泛应用于农业、工业中。研究表明,通过食物链的富集,有机磷杀虫剂(OPPs)能使动物和人中毒,影响人体内激素的代谢平衡。我国虽然对一些有机磷杀虫剂的使用进行了限制,但由于有机磷杀虫剂药效高、在自然环境中容易降解而继续使用。为了保证食品安全,各国政府对食品中OPPs残留限量的要求越来越严格。因此,建立有效的监测水体和食品中有机磷农药残留的方法具有重要的意义。
本论文共包括四个部分:
(一)总结了食品中有机磷杀虫剂残留分析方法,对样品的前处理方法和样品的检测方法进行了详细的介绍。
(二)建立了环境水样中乐果、敌敌畏、甲基对硫磷、马拉硫磷和对硫磷的毛细管电泳的分离检测方法。通过考察缓冲溶液种类、浓度和pH、SDS浓度、甲醇体积、分离电压等实验参数对分离的影响,确定了最佳分离条件。乐果、敌敌畏、甲基对硫磷、马拉硫磷和对硫磷五种有机磷杀虫剂得到很好的分离。该方法可用于环境水样中这五种有机磷农药残留的检测,结果令人满意。以五种有机磷杀虫剂为代表,比较了一种固相萃取填料碳纳米管与传统C18填料的富集效果。
(三)采用毛细管电泳法对水果蔬菜中五种有机磷杀虫剂—乐果、敌敌畏、甲基对硫磷、马拉硫磷和对硫磷进行了检测。
(四)采用了GC-MS对水果蔬菜中的五种有机磷杀虫剂—乐果、敌敌畏、甲基对硫磷、马拉硫磷和对硫磷进行了检测。
(五)对毛细管电泳法和GC-MS法在有机磷杀虫剂残留测定中的应用进新了简单的比较。
At present,there are about more than 30 kinds of organphosphorus pesticides (OPPs) in the world. Although our government had made some restriction in some pesticides because of their higher toxicity to human and animals which affecting the metabolism of hormone in body according to the enrichment of food-chain on research,they are extensively employed for agricultural and industrial use in the last years mainly due to their high effective and relatively low persistence in the environment. In order to insure the food safety , some countries had made very strict restriction on OPPs residue limit. The development of advanced analytical methods for the detection and quantitation of organophosphorous pesticides in water and foods, is therefore a critical issue .
The paper contains four parts:
Part 1 Analytical techniques for organophosphorus pesticide residues in food and their recent development were reviewed, including the application of sample pretreatment technique.
Part 2 A method of capillary eletrophoresis was established for the separation of dichiorvos, dimethoate, methyl-parathion, malathion and parathion in environmental water. Baseline separation was obtained for the five analytes with the optimum conditions according to studying the concentration of buffer,SDS and methanol, pH,applied voltage,etc.and the result was satisfactory.
Part 3 A method of micellar electrokinetic capillary chromatography was established for the separation of dichiorvos,dimethoate,methyl-parathion,malathion and parathion in vegetable.
Part 4 Analysis of five kinds of organophosphorus pesticides in vegetables by gas chromatography-mass spectrometry.
Part 5 A simple comparision between CE and GC-MS in the determination of OPPs.
本论文共包括四个部分:
(一)总结了食品中有机磷杀虫剂残留分析方法,对样品的前处理方法和样品的检测方法进行了详细的介绍。
(二)建立了环境水样中乐果、敌敌畏、甲基对硫磷、马拉硫磷和对硫磷的毛细管电泳的分离检测方法。通过考察缓冲溶液种类、浓度和pH、SDS浓度、甲醇体积、分离电压等实验参数对分离的影响,确定了最佳分离条件。乐果、敌敌畏、甲基对硫磷、马拉硫磷和对硫磷五种有机磷杀虫剂得到很好的分离。该方法可用于环境水样中这五种有机磷农药残留的检测,结果令人满意。以五种有机磷杀虫剂为代表,比较了一种固相萃取填料碳纳米管与传统C18填料的富集效果。
(三)采用毛细管电泳法对水果蔬菜中五种有机磷杀虫剂—乐果、敌敌畏、甲基对硫磷、马拉硫磷和对硫磷进行了检测。
(四)采用了GC-MS对水果蔬菜中的五种有机磷杀虫剂—乐果、敌敌畏、甲基对硫磷、马拉硫磷和对硫磷进行了检测。
(五)对毛细管电泳法和GC-MS法在有机磷杀虫剂残留测定中的应用进新了简单的比较。
At present,there are about more than 30 kinds of organphosphorus pesticides (OPPs) in the world. Although our government had made some restriction in some pesticides because of their higher toxicity to human and animals which affecting the metabolism of hormone in body according to the enrichment of food-chain on research,they are extensively employed for agricultural and industrial use in the last years mainly due to their high effective and relatively low persistence in the environment. In order to insure the food safety , some countries had made very strict restriction on OPPs residue limit. The development of advanced analytical methods for the detection and quantitation of organophosphorous pesticides in water and foods, is therefore a critical issue .
The paper contains four parts:
Part 1 Analytical techniques for organophosphorus pesticide residues in food and their recent development were reviewed, including the application of sample pretreatment technique.
Part 2 A method of capillary eletrophoresis was established for the separation of dichiorvos, dimethoate, methyl-parathion, malathion and parathion in environmental water. Baseline separation was obtained for the five analytes with the optimum conditions according to studying the concentration of buffer,SDS and methanol, pH,applied voltage,etc.and the result was satisfactory.
Part 3 A method of micellar electrokinetic capillary chromatography was established for the separation of dichiorvos,dimethoate,methyl-parathion,malathion and parathion in vegetable.
Part 4 Analysis of five kinds of organophosphorus pesticides in vegetables by gas chromatography-mass spectrometry.
Part 5 A simple comparision between CE and GC-MS in the determination of OPPs.
引文
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[1]王江,王辛,梁晓聪,连玮.固相萃取-气相色谱法检测蔬菜中17种残留的有机磷农药[J].2008,118(2):255-257
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