【作者】 张娟；

【导师】 杨明敏；

【作者基本信息】 南京农业大学 ， 农药学， 2006， 硕士

【摘要】 近年来，农产品、饮用水、环境中有关于农药残留的问题越来越引起人们的重视，为了保护人们的身体健康，WHO／FAO-CAC对食品中农药残留作了相应的最高残留限量（MRL）的规定。开发一种针对我国食品中农兽药残留问题和国际食品贸易要求的简单、快速、有效的样品前处理技术以及具有高灵敏度和高选择性的多残留检测技术就显得十分重要。 本论文共分三个部分： 第一部分：胶束液相色谱法在农药多残留分析中的应用 建立了以0.06mol／L SDS（十二烷基硫酸钠）水溶液为流动相，分离测定吡虫啉、甲基硫菌灵、杀螟丹、克百威、三环唑、敌草隆、叶蝉散、甲霜灵、虫酰肼、苯噻草胺共十种农药的高效液相色谱新方法。在浓度为0.05mg／L-60mg／L范围时，线性相关系数均在0.9898以上，检测限为0.0017～0.0253mg／L，本法具有良好的灵敏度和重现性。液相色谱的条件是：pH4.28 0.06mol／L SDS，SDS：乙腈=10：1（v／v）为流动相：流速为0.6mL／min；在UV-220nm波长下检测。研究了浊点萃取法处理水样的最佳条件，采用上述方法测定自来水中十种农药的添加回收率。 第二部分：硝普钠（SNP）-铜（Ⅱ）体系的极谱法研究 应用循环伏安法（CV）、线性扫描伏安法（LSV）、控制电位电解库仑法（BE）对硝普纳-铜（Ⅱ）体系的电化学行为进行了研究。在0.2mol／L克拉克-鲁布斯（pH=3.0）底液中，分别对SNP、Cu²⁺以及SNP-Cu²⁺溶液进行扫描，发现SNP和SNP-Cu²⁺于-0.47V（vs．SCE）处均产生灵敏的极谱还原峰，但SNP-Cu²⁺体系的灵敏度是单独SNP的100倍左右，其峰电流与硝普纳的浓度在2.0×10¹⁷-4.0×10^-5mol／L范围内呈良好的线性关系（r=0.9997），检出限为1.0×10^-7mol／L。对5.0×10^-6mol／LSNP-Cu²⁺体系进行6次平行实验，RSD为0.33％。实验结果表明，SNP-Cu²⁺体系在极谱电极上有吸附性质，采用控制电位电解库仑法电解SNP-Cu²⁺混合溶液，测得了电极反应的电子转移数为2。 第三部分：吡虫啉、绿磺隆、杀虫单与金属离子、氧化剂反应的研究 应用单扫描极谱法对吡虫啉、绿磺隆、杀虫单与金属离子、氧化剂的反应的电化学行为进行了初步研究。在不同pH值的HAC-NaAC缓冲液中，K₂S₂O₈和NaBO₃对吡虫啉的峰电流有明显的增敏作用，而K₂S₂O₈则会降低绿磺隆的峰电流值；NaClO₃在适当的缓更多还原

【Abstract】 Residue of pesticides found in agriculture products, drinking water and environmental exposure has raised much concern from the general public in recent years. In order to protect persons’ healthy, the maximum residue levels （MRL） in food were constituted by WHO/FAO-CAC. It is important to exploit simply, fast, efficient pre-treatment technologies for samples and high sensitive, high selective multi-pesticide detections technologies based on pesticide and veterinary drug residues in food and the requirement for international trade on food.The thesis includes three parts:In chapter I : The application of micellar liquid chromatography on pesticide residues Under the condition of 0.06mol/LSDS solution, ten pesticides, including imidacloprid thiophanate-methyl cartap carbofuran ricylazole diuron isoprocarb metalaxyl teufenozide mefenacet, were separated and determined. The HPLC conditions were: 0.06 mol/L SDS and 10%acetonitrile（v/v） were used as liquid phase; the flow rate is 0.6ml/min; the detection wave-lenghth was 220nm. The linear relation of ten kinds of pesticides in the range from 0.05 to 60mg/L（r≥ 0.9997） with the detection limit from 0.0017 to 0.0253mg/L. Then we studied the optimal conditions for extracting water by cloud-point extraction. It were added 5% tween-20, 5% NaCl , heating five minutes at 90℃ and then centrifuge at 3500rpm for 5 minutes. The methods had been applied to determine the recoveries of ten pesticides in tap water.In chapter II: The study of sodium nitroprusside by single-sweep oscillopolarography The electrochemical behavior of sodium nitroprusside（SNP）-Cu（ II） was studied by using cyclic voltammetry, linear scanning voltammetry and bulk electrolysis with coulometry. In a base solution of 0.2 mol/L Clark-Bruce at pH3.0, both of SNP and SNP-Cu（II） system all produced sensitive reduction peak at -0.47V（vs.SCE）.But the sensitivity of SNP-Cu（II） system was 100 times higher than SNP. The linear relation holds between the peak current and SNP concentration in the range from 2.0×10^-7 to 4.0×10^-5mol/L（r=0.9997） with the detection limit of 1.0×10^-7mol/L. The relative standard更多还原