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摘要【目的】用超高效液相色谱-串联质谱法(UPLC-MS/MS)研究田水和土壤中吡唑醚菌酯的最终残留和动态消解。【方法】稻田水样用CH2Cl2萃取浓缩，UPLC-MS/MS检测；土样用乙腈超声提取，PSA净化，UPLC-MS/MS检测；外标法定量。【结果】0.0~1.0mg/L浓度范围内吡唑醚菌酯线性关系良好；加标量为0.01~1.0mg/L时，田水和土壤中的平均加标回收率分别为94.2%~106.9%和78.4%~87.1%，相对标准偏差(RSD)为2.82%~6.53%和1.17%~3.55%；仪器检测限为0.1ug/L；常量（100g a.i./ha）与高量（150g a.i./ha）用药时，福建和南京稻田土壤最终残留均小于0.01~0.08 mg/kg；消解动态曲线均符合一级动力学方程，该农药在田水和土壤中的残留量随时间而逐渐降低。【结论】本研究提出了快速高效分析吡唑醚菌酯残留和消解的方法，为指导吡唑醚菌酯在农业生产中的安全合理使用和减少环境污染提供了科学的依据。25483
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关键词 吡唑醚菌酯 高效液相色谱-质谱 稻田水 土壤 残留 动态消解
毕业论文设计说明书外文摘要
Title Final residue and dissipation dynamics of pyraclostrobin in paddy water and soil by UPLC-MS
Abstract
【Objective】 The final residues and dynamic degradation of pyraclostrobin in paddy water and soil was researched by UPLC-MS/MS.【Method】The paddy water was extracted by dichloromethane and then concentrated before UPLC-MS/MS detection; The soil was extracted with acetonitrile by ultrasonic-assisted method, purified by primary secondary amine (PSA),and then detected by UPLC-MS/MS, with external standard method for quantitative.【Results】 The linearity of pyraclostrobin in the concentration of 0.01~1.0 mg/L was acceptable; within the range of 0.01-1.0 mg/L, the average recovery of field water and soil were 94.2%~106.9% and 78.4%-87.1%,respectively.The relative standard deviation (RSD) were 2.82%-6.53% and 1.17%~ 3.55%.The detection limit of the instrument was 0.1ug/L.In constant (100g a.i./ha) and high (150 g a.i./ha) medication, final residues of pyraclostrobin in paddy soils of Fujian and Nanjing both were less than 0.08 mg/kg; degradation dynamics curve conforms to the first-order kinetic equation and the pesticide residual in paddy water and soil decreased with the time prolongation. 【Conclusion】The research provides a fast and efficient analysis of residues and dynamic degradation of pyraclostrobin, and could de regarded as the guidance of safety and reasonable use of pyraclostrobin in agricultural production and provides the scientific basis for reducing the pollution to the environment.
Keywords pyraclostrobin; LC–MS/MS; paddy water; soil; residues; dissipation
目 录
1 绪论 1
1.1 吡唑醚菌酯 1
1.1.1 吡唑醚菌酯杀菌机理 1
1.1.2 吡唑醚菌酯的基本理化性质 1
1.2 高效液相色谱串联质谱法LC–MS/MS 2
1.2.1 高效液相色谱分析 2
1.2.2 质谱分析 3
1.2.3 液相色谱-质谱联用技术 4
1. 3 吡唑醚菌酯的残留分析 4
1.3.1 吡唑醚菌酯的残留分析研究现状 4
1.3.2 液质串联分析吡唑醚菌酯 5
2 实验过程 5
2.1 实验材料与方法 5
2.1.1 仪器与试剂 5
2.1.2 仪器条件 5
2.2 田间试验 6
2.2.1 试验地点 6