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Application Of Hydroxy Acid-derived Reagents In High Performance Liquid Chromatography-mass Spectrometry

Posted on:2013-12-04Degree:MasterType:Thesis
Country:ChinaCandidate:A J TangFull Text:PDF
GTID:2351330371991949Subject:Organic Chemistry
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After30years of development?High performance liquid chromatography (HPLC) havemade a great progress in chromatographic theory, the level of instrument development, analysisand practical application aspects and become a better separation means used in many researchareas widely, from the initial to the classic liquid chromatography, and then combines theclassical theory of liquid chromatography and gas chromatography high performance liquidchromatography, along with the application of liquid chromatography detection technologyimprovements Chromatography have become very common. Such as The field of medicine, thefield of environmental protection, the health sector, chemical industry, etc. however,the highperformance liquid chromatography as a common analysis method can not be perfect.due to theSample structure, status and physico-chemical properties or detection is not perfect, resulting in alarge number of substances in nature to the liquid chromatography separation and analysis ofdirect detection ineffective or not well detected. herefore, explorat and develop highly sensitivedetection methods has important practical significance. In recent years, In order to improve thedetection sensitivity, fluorescence detection methods developed rapidly, and is used to mark theweak fluorescence and non-fluorescent substance, labeled reagents have also developed and putinto use. At the same time, the fluorescent labeling reagent become a more emphasis on thedirection of scientific research personnel. This thesis is mainly based and total synthesis twonew fluorescent labeling reagent, through study the spectroscopic properties of the probemolecule, derivative conditions, chromatography and mass spectrometry conditions, a efficientand sensitive HPLC method established and used in appliedmeaningful sample separation.Specifically do the following tasksChapter One: Generally described the application of fluorescence in high performanceliquid chromatography, a brief introduction of the luminescence mechanism of the fluorescentsubstances, and the generality of the summary by liquid chromatography detection of fluorescentlabeling reagent.Chapter Two: The syntheses of two fluorescent probes:9-oxo-4a,9,9a,10-tetrahydroacridine-2-Carbonated,4-(1-methyl-1H-Philippines [9,10-d] imidazole-2-yl) benzoic acidhydrazide were described followed with Design, synthesis and structural characterization.Chapter Three: Labeling reagent9-oxo-4a,9,9a,10-tetrahydro acridine-2-carbonicacid as the labeling reagents, pre-column derivatization of aliphatic amines by high performanceliquid chromatography-mass spectrometry analysis to optimize good premise, in a derivedconditionderivatives of aliphatic amines were detected using high performance liquidchromatography, and this method is applied to the separation and analysis of real samples. Results showed high sensitivity, good reproducibility and simple operation, suitable for theseparation and analysis of real samples.Chapter Four: Using the detection of the9-oxo-4a,9,9a,10-tetrahydro acridine-2-carbonic acid as a fluorescent labeling reagent for aliphatic alcohols. Optimized reactionconditions, explored a suitable chromatography-mass spectrometry conditions, showed goodseparation for pre-column derivatization processed fatty alcohol compounds were separated, andfeasibility is also very good in the detection of the actual sample.Chapter Five:9-oxo-4a,9,9a,10-tetrahydro acridine-2-carbonic acid for thepre-column derivatization reagent by high performance liquid chromatography-massspectrometry method for detection of common phenolic compounds. Derivatization reactionconditions and chromatography-mass spectrometry conditions optimized establish a detectionmethod for the separation and analysis of phenolic compounds after pre-column derivatization,the detection process related to the actual samples have a very good reproducibility.
Keywords/Search Tags:derivatization reagent, derivatization reaction, fatty amines, fatty alcohols, Phenolic
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