Synthesis Of Novel Fluorescent Amino Compound Derivatization Reagents And Their Application In HPLC Analysis

In the way of separating and analysing complex mixtures,high performance liquid chromatography(HPLC)is playing an important role.It is widely used in food detection,quality analysis,drug testing,environmental monitoring and other fields.However,the status,structure and physicochemical properties of some substances lead to poor or even undetectable results when HPLC is used for direct analysis.Therefore,considering more sensitive detection methods has important practical importance.The chemical derivatization method is one of the most widely used and efficient means at present,so the development of derivative reagents with excellent performance,low cost and high sensitivity has very important practical significance.So the development of excellent performance,low cost,high sensitivity of the derivatization reagents has a very important practical significance.This paper focuses on the design,synthesis,characterization and application of novel fluorescence derivatization reagents,from the preparation of derivatization reagents,the optimization of the pretreatment method,derivatization reaction conditions,the exploration of chromatographic separation conditions,the actual sample determination and other aspects of research work.Specific work content is as follows:Chapter one: Briefly introduced the application of HPLC and the basic content.Summarized the development of the fluorescence derivatization technology.Overview of the topic significance and main research content.Chapter two: The synthesis of fluorescent derivatization reagent 2-(9-acridone)-ethyl chloroformate(AEC-Cl)was described followed with their structural characterization.Chapter three: Using 2-(9-acridone)-ethyl chloroformate as fluorescent derivatization reagent to determine free amino acids by high performance liquid chromatography-mass spectrometry.By optimizing the derivatization conditions and chromatographic conditions,the method established was applied to the determination of trace amino acids in honey.It has the advantages of fast analysis,high efficiency,good stability and high sensitivity.Chapter four: Using 2-(9-acridone)-ethyl chloroformate as pre-column derivatization reagent to determine mycotoxins by high performance liquid chromatography-mass spectrometry.The ultrasound-assisted dispersive liquid-liquid microextraction was used as a pretreatment method.A response surface methodology was employed to optimize the main parameters affecting the derivatization and dispersive liquid-liquid microextraction efficiency.The established method was applied to the detection of four mycotoxins in grain and feed.This method has the advantages of high analytical speed,efficiency,selectivity and sensitivity,and provides a reference for the development of more sensitive labeling reagents.Chapter five: Using 2-(9-acridone)-ethyl chloroformate as pre-column derivatization reagent to determine biogenic amines by high performance liquid chromatography-mass spectrometry.Ultrasound-assisted dispersive liquid-liquid microextraction was used to eliminate matrix interference in complex samples.The experimental variables influencing the derivatization and extraction efficiency were optimized byresponse surface methodology.This method combined the advantages of dispersed-liquid microextraction and chemical derivatization method,which not only effectively improved the extraction efficiency of sample pretreatment,but also greatly improved the sensitivity and accuracy of detection,and expands the application range of dispersed-liquid microextraction and high performance liquid chromatography.