【作者】 涂貌贞；

【导师】 谢增鸿；

【作者基本信息】 福州大学 ， 分析化学， 2006， 硕士

【摘要】 第一部分为综述,介绍了有机磷农药残留检测的研究现状,综述了化学发光法近几年在农药残留等多个领域的研究应用。第二部分,利用化学发光-流动注射技术对甲胺磷、敌百虫、乐果、三唑磷几种有机磷农药的化学发光行为进行了研究。建立了这几种农药的化学发光检测体系,并应用于蔬菜中的农药残留量检测,初步探讨了体系发光反应机理。基于NaH₂PO₄-NaOH碱性条件下,甲胺磷增强铁氰化钾和鲁米诺体系的化学发光,建立了流动注射化学发光（FI-CL）检测甲胺磷的方法。测定甲胺磷的线性范围为1.0×10^-8-1.0×10^-5g/mL,检测限（S/N=3）为3.3×10^-9g/mL,相对标准偏差RSD为2.0%(1.0×10^-6g/mL的甲胺磷,n=11)。方法简单、快速、灵敏,已成功用于白菜中甲胺磷的测定,回收率为93.0%-94.4%,探讨了体系发光反应机理。基于碱性介质中敌百虫增强鲁米诺-H₂O₂体系发光,建立了测定敌百虫的流动注射化学发光分析方法,测定线性范围为1.0×10^-8-1.0×10^–5g/mL,检测限（S/N=3）为3.2×10^-9g/mL,相对标准偏差RSD为1.10%(1.0×10^-7g/mL的敌百虫,n=11)。对白菜样品进行加标回收率测定,回收率在88.5%-92.6%之间,探讨了体系发光反应机理。碱性介质中,乐果极大增强鲁米诺-H₂O₂体系的化学发光反应,基于此建立了测定乐果的流动注射化学发光分析方法。测定线性范围为5.0×10^-8-1.0×10^-5g/mL,检测限（S/N=3）为1.5×10^-8g/mL,相对标准偏差RSD为1.9% (1.0×10^-7g/mL的乐果,n=11)。成功地用于白菜样中的乐果的残留量测定,回收率为108.0-119.3%,探讨了体系发光反应机理。基于碱性介质中三唑磷增强鲁米诺-H2O2体系发光的研究,建立了测定三唑磷的流动注射化学发光分析方法。测定线性范围为1.0×10^-8-1.0×10^-5g/mL。检测限（S/N=3）为6.7×10^-9g/mL,相对标准偏差RSD为2.4%(1.0×10^-7g/mL的三唑磷,n=11)。对白菜样品进行加标回收率测定,回收率为78.0-108.6%,探讨了体系发光反应机理。更多还原

【Abstract】 This thesis includes two parts. Part one（Chapter one） is review. Part two（Chapter two to Chapter five） is research reports.In the first part, the present state of organophosphorous pesticides residues research and basic Knowledge of chemiluminescence （CL） were introduced. And the present applications of the CL method in organophosphorous pesticide residues and other fields were also reviewed in this part.In part two, the flow injection CL assay of some organophosphorous pesticides （methamidophos,trichlorphon,dimethoate,triazophos） were investigated.Methods for the determination of these organophosphorous pesticides were proposed,and were applied to the vvegetable samples determination.The CL reaction mechanisms were also discussed.In chapter two,a method for the determination of methamidophos based on the enhancement of chemiluminescence（CL） of luminol-potassium ferricyanide in basic medium by flow injection CL analysis has been established. The calibration graph is linear for1.0×10^-8-1.0×10^-5g/mL with a detection limit （S/N=3） of 5.3×10^-9g/mL,the relative standard RSD is 2.0%for 1.0×10^-6g/mLmethamidophos（n=11）.The method was simple, fast,sensitive and cheap,and was applied successfully to the determination of methamidophos in vegetables,recovery is between 93.0%-94.4%. The system’s reaction mechanism was also discussed.In chapter three, based on the chemiluminescence（CL） enhancement of luminol-H2O2 in basic medium,a flow-injection CL method for the determination of trichlorphon has been proposed. The calibration graph is linear for 1.0×10^-8-1.0×10^-5g/mL,the detection limit （S/N=3） is 3.2×10^-9g/mL, the relative standard RSD is 1.10% for 1.0×10^-7g/mL trichlorphon（n=11）. The method was applied to the determination of trichlorphon in vegetable ,recovery is between 88.5%-92.6%. The system’s reaction mechanism was also discussed.In chapter four,based on the chemiluminescence（CL） can be greatly enhanced by adding dimethoate in the basic medium,a a flow-injection CL method for the analysis更多还原