氟虫腈及其代谢物VIP免费

实用文档摘要本论文从不同溶剂（正己烷、乙腈、乙酸乙酯）提取、不同的提取方式（匀浆、超声、振摇）、不同的净化方式（Flotisil硅酸镁、NH2、GCB、PSA、C18）等方面对回收率的影响得出以下主要结果。1、通过溶剂（正己烷、乙腈、乙酸乙酯）对氟虫腈及其代谢物的分析选择乙腈作为最佳提取溶液。2、考察不同提取方式（匀浆、超声、振摇）对氟虫腈及其代谢物的提取分析选择振摇样品30min为最佳提取方式。3、根据几种不同的固相萃取柱的作用不同，选择使用Flotisil（硅酸镁）萃取柱进行净化为最佳的净化方式。4、根据氮吹温度（65~70℃、70~75℃、75℃以上）回收率比较，及氟虫腈及其代谢物性质选择最佳温度为60~70℃。建立了一种快速提取、净化、使用超高效液相色谱-质谱串联联用（UPLC-MS/MS)对氟虫腈及其代谢物的新方法。用乙腈作为提取液提取，置于摇床上振摇30min，经过Flotisil（硅酸镁）净化后，使用UPLC-MS/MS仪器的MRM进行分析。回收率在70~110%之间，相对标准偏差为6.5%，小于10%。关键词：UPLC-MS/MS；氟虫腈及其代谢物；农药残留；实用文档AbstractInthispaper,fromdifferentsolvents(normalhexane,acetonitrile,ethylacetateextraction,differentextractionmethods(homogenate,ultrasound,vibrationwave),differentpurification(Flotisilmagnesiumsilicate,NH2,GCBandPSA,C18)ontherecoveryrateofthemainresultsareasfollows.1)throughtheanalysisofthesolvents(hexane,acetonitrile,ethylacetate)totheanalysisofthechoiceofacetonitrileasthebestextractionsolution.2)theextractionofdifferentextractionmethods(homogenization,ultrasound,vibration)ontheextractionandanalysisoffluorideanditsmetaboliteswereselectedasthebestextractionmethodof30min.3)accordingtothedifferentroleofseveraldifferentsolidphaseextractioncolumn,choosetouseFlotisil(magnesiumsilicate)extractioncolumnforthebestpurificationmethod.4)accordingtothenitrogenblowingtemperature(65~70degreesC,70~75degreesC,above75degrees)recoveryrate,andthenatureofthefluorineanditsmetabolitestoselectthebesttemperaturefor60~70.Anewmethodfortherapidextraction,purificationandtheuseofultraperformanceliquidchromatographytandemmassspectrometry(UPLC-MS/MS)forthedetectionoffluorideanditsmetaboliteswasestablished.Withacetonitrileasextractionliquidextraction,placedinbedshakingfor30min,afterpurificationFlotisil(magnesiumsilicate)usingUPLC-MS/MSinstrumentofMRManalysis.Recoveryratein70~110%,therelativestandarddeviationis6.5%,lessthan10%.Keywords:UPLC-MS/MS;fluorine;cyanideanditsmetabolites;pesticideresidues;实用文档目录摘要......................................................................IAbstract...................................................................II目录......................................................................III第1章绪论.................................................................11.1研究背景............................................................11.2研究目的及意义......................................................11.2.1研究目的......................................................11.2.2研究意义......................................................21.3本章小结............................................................2第2章文献综述.............................................................32.1农药残留的现状及危害................................................32.1.1农药的影响....................................................32.1.1.1对环境的影响............................................32.1.1.2对农药使用者的影响......................................32.1.1.3食物中的农药残留............................