嗪草酮等农药的残留分析方法和残留规律研究
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摘要
农药残留对人类和环境的危害引起了世界各国的关注。为开展对农药残留的风险评估,本文围绕农药残留分析方法和降解规律开展研究,建立了嗪草酮、丙酯草醚、甲基二磺隆、氟虫腈、嘧霉胺和氟喹唑等农药在农作物和土壤环境中的残留分析方法,研究了它们在农作物和土壤环境中的降解规律。采用原位聚合法合成了嗪草酮分子印迹整体柱,考察了嗪草酮与其结构类似物在印迹柱和空白柱上的保留特性,.证明印迹柱具有良好的亲和性和特异选择性,遂把印迹柱用于农药残留检测样品前处理,建立了分子印迹柱在线富集测定土壤样品中嗪草酮残留的分析方法,研究了嗪草酮在玉米和土壤中的残留降解规律,提出了嗪草酮用于防治玉米杂草的合理使用准则及嗪草酮在玉米上的’残留限量(MRL)建议。丙酯草醚为我国开发的具有自主知识产权的新型除草剂,此前国内外没有丙酯草醚的残留数据和残留分析方法,本文开发了液相色谱紫外法检测油菜和土壤中丙酯草醚残留量的方法,方法操作简单,准确度和精密度满足农药残留测定要求,系统研究了丙酯草醚在油菜和土壤中的残留降解规律,提出了丙酯草醚防治油菜杂草的合理使用准则和丙酯草醚在油菜籽中的MRL建议。此外,本文还对甲基二磺隆、氟虫腈,嘧霉胺和氟喹唑在小麦、稻米和梨及土壤中的残留分析方法分别作了研究和改进。甲基二磺隆残留采用液相色谱法检测,降低了分析成本；实现了对嘧霉胺和氟喹唑残留的同时提取净化,简化了前处理过程,验证试验表明上述农药的残留分析方法均符合农药残留测定要求。在此基础上,研究了上述农药在农作物和土壤中的残留降解规律,得出了几种农药降解的动力学方程和半衰期,提出了它们在农作物上的合理使用准则及MRL建议。
The hazards of pesticide residues to human health and environment have caught many attentions through out of the world. To evaluate the risk of pesticide residues, the analytical method for determine residues of metribuzin, pyribambenz-propyl, mesosulfuron-methyl, fluquinconazole, pyrimethanil and fipronil in crops and soils were developed, and their residue dynamics in crops and soil environment were studied in this paper. The molecularly imprinted polymer (MIP) of metribuzin was prepared by in-situ polymerization. The retention behavior of metribuzin and its structural analogs were determined on both the MIP and blank columns. The results showed that the MIP had high affinity and selectivity for metribuzin. This monolithic polymer was used for on-line preconcentration and detection of metribuzin residue in soil samples. The dynamics and final state of residues of metribuzin in corn and soil were studied. The guideline for safety application of metribuzin and the maximum residue limit (MRL) of metribuzin in corn grain were proposed based on the research results. Pyribambenz-propyl was a new herbicide with China's independent intellectual property rights. There was no related residue data and residue analysis method of pyribambenz-propyl in the world before. The HPLC-UV detection which was used to determine pyribambenz-propyl residues in rapes and soil was developed. The method was easy to operate, and its accuracy and precision met the requirements of pesticide residue determination. Systematic study on pyribambenz-propyl residue degradation in rapes and soil was carried out. The guideline for safety application of pyribambenz-propyl and the MRL of pyribambenz-propyl in rapeseeds were proposed. Moreover, this paper studied and improved the analysis methods for determination of residues of mesosulfuron-methyl, fluquinconazole, pyrimethanil and fipronil. Mesosulfuron-methyl residue was detectded by HPLC, and the cost of the determination was reduced. The residues of fluquinconazole and pyrimethanil were extracted with one procedure, and the sample pretreatment had been simplified and optimized The data of these methods validation indicated that they could meet the requirements of pesticide residue determination. The residues dynamics of these pesticides in crops and soils were studied. Their dynamic equations and half lives were obtained. Suggestions about safety application of these pesticides and the MRL of these pesticides in crops were put forward based on the results.
The hazards of pesticide residues to human health and environment have caught many attentions through out of the world. To evaluate the risk of pesticide residues, the analytical method for determine residues of metribuzin, pyribambenz-propyl, mesosulfuron-methyl, fluquinconazole, pyrimethanil and fipronil in crops and soils were developed, and their residue dynamics in crops and soil environment were studied in this paper. The molecularly imprinted polymer (MIP) of metribuzin was prepared by in-situ polymerization. The retention behavior of metribuzin and its structural analogs were determined on both the MIP and blank columns. The results showed that the MIP had high affinity and selectivity for metribuzin. This monolithic polymer was used for on-line preconcentration and detection of metribuzin residue in soil samples. The dynamics and final state of residues of metribuzin in corn and soil were studied. The guideline for safety application of metribuzin and the maximum residue limit (MRL) of metribuzin in corn grain were proposed based on the research results. Pyribambenz-propyl was a new herbicide with China's independent intellectual property rights. There was no related residue data and residue analysis method of pyribambenz-propyl in the world before. The HPLC-UV detection which was used to determine pyribambenz-propyl residues in rapes and soil was developed. The method was easy to operate, and its accuracy and precision met the requirements of pesticide residue determination. Systematic study on pyribambenz-propyl residue degradation in rapes and soil was carried out. The guideline for safety application of pyribambenz-propyl and the MRL of pyribambenz-propyl in rapeseeds were proposed. Moreover, this paper studied and improved the analysis methods for determination of residues of mesosulfuron-methyl, fluquinconazole, pyrimethanil and fipronil. Mesosulfuron-methyl residue was detectded by HPLC, and the cost of the determination was reduced. The residues of fluquinconazole and pyrimethanil were extracted with one procedure, and the sample pretreatment had been simplified and optimized The data of these methods validation indicated that they could meet the requirements of pesticide residue determination. The residues dynamics of these pesticides in crops and soils were studied. Their dynamic equations and half lives were obtained. Suggestions about safety application of these pesticides and the MRL of these pesticides in crops were put forward based on the results.
引文
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