Synthesis Of Carbazole And Phenanthroimidazole Derivative Reagents And Their Analysis And Application In HPL

Since the 20 th century,especially since the 1970 s,high performance liquid chromatographic technology(HPLC)has developed rapidly in the separation and analysis of complex mixtures,and has gradually become an important branch of analytical chemistry.The technology is widely used in the environmental safety detection,biochemistry,drug analysis,food detection and other fields,and is closely related to human clothing,food,housing and transportation.However,due to the non-luminescent properties of some compounds and the limitation of low content in the tested samples,not all samples can be directly analyzed by liquid chromatography.Therefore,it is very important to improve the detection specificity and sensitivity of HPLC.At present,chemical derivatization is still one of the most widely used and efficient methods.The combination of high performance liquid chromatography and chemical derivatization method can effectively solve the limitation of detection.This work focuses on the design,synthesis and characterization of two new fluorescence derivatization reagents,at the same time,their applications for the determination of some low content of compounds with HPLC were investigated with satisfactory results.The details are as follows:Chapter one: The research progress and basic theory of high performance liquid chromatography,at the same time,the combination technology of chemical derivatization and mass spectrometry is briefly described.In addition,the chemicals needed in the experiment and the research paper ideas were presented.Chapter two: This chapter describes the design,synthesis and characterization of new fluorescent labeling reagents of 4-(9-carbazole)-benzoyl imidazole(CPIM),and 4-(n-phenylphenanthimidazole)-phenylmethyl chloroformate(PPIBC-Cl).Chapter three: The novel fluorescence derivatization reagent of 4-(9-carbazole)-benzoylimidazole(CPIM)was used for the analysis of aliphatic amine by HPLC.The sample was extracted by self-made air purging-microsyringe extraction method(GP-MSE)to improve the extraction efficiency of food packaging materials.After optimization of derivatization conditions and chromatographic conditions,the established method has been successfully applied to the determination of trace aliphatic amines in food packaging materials with satisfactory results.Chapter four: A new fluorescent derivatization reagent of 4-(9-carbazole)-benzoylimidazole(CPIM)was prepared for the analysis of fatty alcohols by high performance liquid chromatography.In order to improve the detection sensitivity,the response surface analysis method was used to optimize the factors affecting the derivatization process such as temperature,time,DMAP dosage and so on.The proposed method has been successfully applied to the detection of trace fatty alcohols in detergent products.Chapter five: The novel fluorescent derivatization reagent of4-(N-phenylphenanthimidazole)-phenylmethyl chloroformate(PPIBC-Cl)was used for the determination of biogenic amines by HPLC.The liquid-liquid extraction method was used to extract biogenic amines from hyaluronic acid fermentation broth and fermented yogurt.After the optimization of derivatization conditions and chromatographic conditions,the proposed method was applied to the determination of biogenic amines in hyaluronic acid fermentation broth and fermented yogurt.This established method has advantages of simple operation,high analytical efficiency,good linearity,high sensitivity and low detection limits,at the same time,it also provides important reference for the development of more efficient fluorescence derivatization reagents.Chapter six: A novel fluorescent derivatization reagent of4-(N-phenylphenanthimidazole)-phenylmethyl chloroformate(PPIBC-Cl)was used for the determination of small molecular aliphatic amines by high performance liquid chromatography.Response surface analysis method was used to optimize the derivatization conditions,and the analytical method was successfully applied to the determination of aliphatic amines in seafood.