敌敌畏、三唑酮的电化学分析及水中十一种农药的固相萃取方法研究
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摘要
众所周知，农药的使用对农业生产作出了巨大贡献。但是农药在环境和农产品中的残留对人们的健康带来潜在的危害已引起人们的重视。为了保护人们的健康，许多国家都严格限制农药的使用量和通过立法制定农药最大残留允许限量标准(MRLs)，用以控制食品中的农药残留量。为了监控农药的使用对环境的污染状况和防止农药残留量超标的农产品进入市场，需要开展农药残留检测工作。国际上通用的比较成熟的农药残留分析方法为AOAC方法，该方法能检测325种左右的农药及其相关的化合物，其主要存在问题是方法太复杂，有毒溶剂消耗大，费时费力，不能用于现场快速检测。为此，本文主要用电化学手段和固相萃取技术进行农药残留快速检测方法的研究。
利用敌敌畏(DDVP)可以催化过硼酸钠(SPB)氧化联苯胺反应的特性，建立测定DDVP的单扫描极谱分析方法，此方法的灵敏度高，其对应的线性范围是3.0μg／L～7.5mg／L(R~2=0.9992)，检测限为1.0μg／L。用于测定植物样品中DDVP的残留量，结果令人满意。另外，实验指出了DDVP的催化作用并研究了SPB-联苯胺氧化产物的电极还原机理。
用电化学方法结合HPLC和HPLC-MS研究了Cu~(2+)对三唑酮的降解反应，实验发现，三唑酮能被Cu~(2+)降解生成1-(1，2，4-三唑-1-羟基)-3，3-二甲基-2-丁酮(简称1羟基-唑酮，简写THDB)和对氟苯酚。在0.35mol／L(PH=8.2)的NH_3-NH_4Cl底液中，Cu~(2+)与THDB形成有电化学活性的配位物[Cu(NH_3)_2THDB]~(2+)，用单扫描极谱法可在峰电位E_p=-0.566V(vs.SCE)获得一灵敏的还原峰，该峰电流和三唑酮的浓度在4.0×10~(-7)～1.92×10~(-5)mol／L范围内有良好的线性关系(r=0.9998)，其检出下限为1.0×10~(-7)mol／L。与直接利用三唑酮位于-1.326V还原峰进行分析三唑酮相比，灵敏度提高了近100倍。用此建立了一种间接测定三唑酮含量的新方法，将其用于三唑酮制剂和在水果中的残留检测，结果满意。与其它方法比较，该方法操作简单、快速，有机试剂用量少。另外，本文还对三唑酮的降解过程和体系的电极反应机理进行了探讨。
敌敌畏、三哇酮的电化学分析及水中十一种农药的固相萃取方法研究
用Supe 1 olean侧LC一18固相苹取小柱对自来水和长江水中痕量农药进行富集，用
反相高效液相色谱法进行分析。n种农药(灭多威、毗虫琳、吮虫清、三环哇、克百
威、漆草酮、杭蚜威、芬去津、敌草隆、草除灵、苯喀草胺)在浓度为smg/L一10拼g/L
范围时，线性相关系数均在0.9997以上，实际水样的添加回收率除了灭多威较低外，
其余均大于80%，检测限为0.0118一0.0610拜g/L(s/N一3，富集因子:100)，低于欧共体
所要求的饮用水标准(单种农药浓度小于0.1拼g/L)。
The use of pesticides provides unquestionable benefits in increasing agricultural production. However, it has the drawback of pestide residues which remain in environment and agricultural products, constituting a potential risk to people because of their toxicity. To protect consumers' health, many countries have restricted the usage of pesticides and have established legal directives to control their levels in food, through the Maximum Residue Levels (MRLs). To monitor enviroment pesticide pollution and provent agricultural production that contain pesticide residue levels higher than the MRLs from entering the marketplace, determination of pesticide residues is indispensable. The method of the Association of Official Analytical Chemists (AOAC), the internationl recognized pesticide residual analysis can detect approximately 325 pesticides and pesticide-related compounds and most of them have undergone rigorous multiaboratory calibration studies, such as those needed to obtain the official acceptance by the
AOAC. However, these methods still present disadvanges because their procdures are time consuming, labour intensive and large amount of toxic solvent consuming. So the paper is mainly study the rapid detection of pesticide with electrochemical and solid phase extraction techniques.
A Single-sweep polarography was described for the determination of trace dichlorvos (DDVP) with sodium perborate (SPB) and benzidine. The detection limit and the linear range were 1.0ug /mL and 3.0ug/L~7.5mg/mL (R2=0.9992) respectively. The method had been used for determining trace DDVP in plant with satisfactory results. The catalysis of DDVP was indicated by the experimentation, and the mechanism of electrode reduction was also discussed in this paper.
The degradation reaction of triadimefon in copper(II) ion solution was examined by electrochemical, HPLC and HPLC-MS method. The results show that triadimefon can be degraded into l-(l,2,4-triazol-l-hydroxyl)-3,3-dimethyl-butan-2-one (THDB) and 4-chlorophenol by copper (II) ion. A electrochemical active complex of copper (II)-THDB formed in the supporting electrolyte of 0.35 mol/L NH3-NH4Cl (pH=8.2), a sensitive
reduction peak of the complex was found at -0.566V(vs.SCE) by using single-sweep polarography, which detection sensitivity is nearly 100 times as that of tiradimefon at -1.326V(vs.SCE), the peak current is directly proportional to the concentration of triadimefon over the range of 4.0x10-7 to 1.92x10-5mol/L, the detection limit is 1.0x10-7mol/L. A new sensitive method for indirect determination of triadimefon was established, which has been used for determining triadimefon commodity and its residue in fruit with satisfactory results. Compared with other verify techniques, the method is faster, easier and less reagent consuming. The degradation process of triadimefon and the electrode reaction mechanism of the system were also discussed in this paper.
A method was proposed for the simultaneous determination of eleven micro-pesticides (methomyl, imidacloprid, acetamiprid, tricyclazole, carbofuran, metribuzin, pirimicarb, atrazine, diuron, benazolin-ethyl, mefenacet) in tap water and Yangtse river water, using solid-phase extraction (SPE) with Supelclean?LC-18 cartridge and reversed phase high performance liquid chromatography technique. In the concentration range 5mg/L~10ug/L, the correlation coefficients were all up to 0.9997. The fortified recoveries of 11 pesticides were all up to 80% except methomyl, the detection limits of the whole procedure achieved were 0.0118-0.0610 ug/L (S/N=3, enrichment factor: 100), less than 0.1ug/L, which the maximum limit permitted by the European Community standard for drinking water.
利用敌敌畏(DDVP)可以催化过硼酸钠(SPB)氧化联苯胺反应的特性，建立测定DDVP的单扫描极谱分析方法，此方法的灵敏度高，其对应的线性范围是3.0μg／L～7.5mg／L(R~2=0.9992)，检测限为1.0μg／L。用于测定植物样品中DDVP的残留量，结果令人满意。另外，实验指出了DDVP的催化作用并研究了SPB-联苯胺氧化产物的电极还原机理。
用电化学方法结合HPLC和HPLC-MS研究了Cu~(2+)对三唑酮的降解反应，实验发现，三唑酮能被Cu~(2+)降解生成1-(1，2，4-三唑-1-羟基)-3，3-二甲基-2-丁酮(简称1羟基-唑酮，简写THDB)和对氟苯酚。在0.35mol／L(PH=8.2)的NH_3-NH_4Cl底液中，Cu~(2+)与THDB形成有电化学活性的配位物[Cu(NH_3)_2THDB]~(2+)，用单扫描极谱法可在峰电位E_p=-0.566V(vs.SCE)获得一灵敏的还原峰，该峰电流和三唑酮的浓度在4.0×10~(-7)～1.92×10~(-5)mol／L范围内有良好的线性关系(r=0.9998)，其检出下限为1.0×10~(-7)mol／L。与直接利用三唑酮位于-1.326V还原峰进行分析三唑酮相比，灵敏度提高了近100倍。用此建立了一种间接测定三唑酮含量的新方法，将其用于三唑酮制剂和在水果中的残留检测，结果满意。与其它方法比较，该方法操作简单、快速，有机试剂用量少。另外，本文还对三唑酮的降解过程和体系的电极反应机理进行了探讨。
敌敌畏、三哇酮的电化学分析及水中十一种农药的固相萃取方法研究
用Supe 1 olean侧LC一18固相苹取小柱对自来水和长江水中痕量农药进行富集，用
反相高效液相色谱法进行分析。n种农药(灭多威、毗虫琳、吮虫清、三环哇、克百
威、漆草酮、杭蚜威、芬去津、敌草隆、草除灵、苯喀草胺)在浓度为smg/L一10拼g/L
范围时，线性相关系数均在0.9997以上，实际水样的添加回收率除了灭多威较低外，
其余均大于80%，检测限为0.0118一0.0610拜g/L(s/N一3，富集因子:100)，低于欧共体
所要求的饮用水标准(单种农药浓度小于0.1拼g/L)。
The use of pesticides provides unquestionable benefits in increasing agricultural production. However, it has the drawback of pestide residues which remain in environment and agricultural products, constituting a potential risk to people because of their toxicity. To protect consumers' health, many countries have restricted the usage of pesticides and have established legal directives to control their levels in food, through the Maximum Residue Levels (MRLs). To monitor enviroment pesticide pollution and provent agricultural production that contain pesticide residue levels higher than the MRLs from entering the marketplace, determination of pesticide residues is indispensable. The method of the Association of Official Analytical Chemists (AOAC), the internationl recognized pesticide residual analysis can detect approximately 325 pesticides and pesticide-related compounds and most of them have undergone rigorous multiaboratory calibration studies, such as those needed to obtain the official acceptance by the
AOAC. However, these methods still present disadvanges because their procdures are time consuming, labour intensive and large amount of toxic solvent consuming. So the paper is mainly study the rapid detection of pesticide with electrochemical and solid phase extraction techniques.
A Single-sweep polarography was described for the determination of trace dichlorvos (DDVP) with sodium perborate (SPB) and benzidine. The detection limit and the linear range were 1.0ug /mL and 3.0ug/L~7.5mg/mL (R2=0.9992) respectively. The method had been used for determining trace DDVP in plant with satisfactory results. The catalysis of DDVP was indicated by the experimentation, and the mechanism of electrode reduction was also discussed in this paper.
The degradation reaction of triadimefon in copper(II) ion solution was examined by electrochemical, HPLC and HPLC-MS method. The results show that triadimefon can be degraded into l-(l,2,4-triazol-l-hydroxyl)-3,3-dimethyl-butan-2-one (THDB) and 4-chlorophenol by copper (II) ion. A electrochemical active complex of copper (II)-THDB formed in the supporting electrolyte of 0.35 mol/L NH3-NH4Cl (pH=8.2), a sensitive
reduction peak of the complex was found at -0.566V(vs.SCE) by using single-sweep polarography, which detection sensitivity is nearly 100 times as that of tiradimefon at -1.326V(vs.SCE), the peak current is directly proportional to the concentration of triadimefon over the range of 4.0x10-7 to 1.92x10-5mol/L, the detection limit is 1.0x10-7mol/L. A new sensitive method for indirect determination of triadimefon was established, which has been used for determining triadimefon commodity and its residue in fruit with satisfactory results. Compared with other verify techniques, the method is faster, easier and less reagent consuming. The degradation process of triadimefon and the electrode reaction mechanism of the system were also discussed in this paper.
A method was proposed for the simultaneous determination of eleven micro-pesticides (methomyl, imidacloprid, acetamiprid, tricyclazole, carbofuran, metribuzin, pirimicarb, atrazine, diuron, benazolin-ethyl, mefenacet) in tap water and Yangtse river water, using solid-phase extraction (SPE) with Supelclean?LC-18 cartridge and reversed phase high performance liquid chromatography technique. In the concentration range 5mg/L~10ug/L, the correlation coefficients were all up to 0.9997. The fortified recoveries of 11 pesticides were all up to 80% except methomyl, the detection limits of the whole procedure achieved were 0.0118-0.0610 ug/L (S/N=3, enrichment factor: 100), less than 0.1ug/L, which the maximum limit permitted by the European Community standard for drinking water.
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