生物检材中百草枯提取净化及检测方法的研究

发布时间：2018-06-27 20:03

本文选题：百草枯 + 生物检材　；参考：《昆明医学院》2005年硕士论文

【摘要】：[目的] 百草枯(英文名,paraquat)属灭生性除草剂,极性较强,极易溶于水,在实际检案中提取液难于浓缩,这是百草枯中毒案件分析鉴定中的一个巨大障碍。本课题采用离子对固相萃取(SPE)法提取百草枯,解决了净化及浓缩问题,建立高效液相色谱(HPLC)的定性定量分析方法,同时建立了毛细管电泳(HPCE)的定性分析方法。并进一步通过动植物中毒实验来验证所建立的提取、分离及检测方法的可行性和准确性。[方法] 植物检材直接进行离子对固相萃取,生物检材经糜蛋白酶酶解后进行萃取,用HPLC定性定量分析,同时用TLC和HPCE进行定性分析。[结果] 生物检材的回收率在81%～94%之间,标准偏差在2.98～3.95%之间,变异系数在3.6～4.4%,最低检测限1ng·ml~(-1)。[结论] 离子对固相萃取法提取百草枯的选择性强,具有提取率高、提取物干净、重现性好等优点,HPLC/DAD法定性定量结果准确、灵敏、重现性好;TLC法简单、快速易于在基层推广,HPCE法也可用于百草枯分析。本方法可用于其它各类检材中百草枯的检测,应用范围较广。本研究为百草枯农药致农作物枯死案件或致人畜中毒案件的分析鉴定提供了理论依据和快速、准确的检测方法。方法具有创新性、实用性和很高的推广应用价值。
[Abstract]:[objective] Paraquat is a kind of herbicide with strong polarity and easily soluble in water. It is difficult to concentrate the extract of paraquat in practical cases, which is a great obstacle in the analysis and identification of paraquat poisoning cases. In this paper, ion-pair solid phase extraction (SPE) was used to extract paraquat, which solved the problem of purification and concentration. The qualitative and quantitative analysis method of high performance liquid chromatography (HPLC) and capillary electrophoresis (HPCE) were established. Furthermore, the feasibility and accuracy of the established methods for extraction, separation and detection were verified by animal and plant poisoning experiments. [methods] Plant samples were extracted directly by ion pair solid phase extraction, and biological samples were extracted by chymotrypsin enzymatic hydrolysis. Qualitative analysis was performed by HPLC and TLC and HPCE at the same time. [results] the recoveries of biological samples were between 81% and 94%, the standard deviation was between 2.98% and 3.95%, the coefficient of variation was 3.66%, and the lowest detection limit was 1ng ml ~ (-1). [conclusion] Ion-pair solid-phase extraction method has the advantages of high selectivity, high extraction rate, clean extract and good reproducibility. The qualitative and quantitative results of HPLC / dad method are accurate, sensitive and reproducible. HPCE method can also be used for paraquat analysis. This method can be used for the detection of paraquat in other kinds of materials. This study provides a theoretical basis and a rapid and accurate method for the analysis and identification of paraquat pesticide-induced crop death cases or human and animal poisoning cases. The method is innovative, practical and valuable in popularization and application.
【学位授予单位】：昆明医学院
【学位级别】：硕士
【学位授予年份】：2005
【分类号】：D919

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