Fluorescent Reagent In The Pre-column Derivatization Hplc-ms Method For The Determination Of Phenols, Amines And Acids

High performance liquid chromatography (HPLC), as one of the most important modern analytical means of separation and determination, has been used in all aspects of industrial and research fields and greatly promoted the development of chemistry. However, not all compounds are suitable to be directly analyzed by HPLC simply due to lack of general-purpose detector, the limitation of the compounds'properties and the low contents of the detected component. So it is significant to develop testing methods with high sensitivity. Chemical derivatizations is one of the most effective procedures to change the properties of corresponding compounds. In this paper, we designed and synthesized three novel fluorescence labeling reagents. The optimal derivatization and chromatographic separation conditions of labeling reagents were investigated. At the same time, fluorescence and UV-Vis spectrum of labeling reagents and the suitability of the developed method for the analysis of real samples were evaluated.Chapter one:The basic theory about high performance liquid chromatography and pre-/post-column derivatizations were simply presented. Subsequently, commercial fluorescent reagent and the as-synthesized reagents of our laboratory were summarized. The process of developing interface about HPLC-MS was also presented. Lastly, the main works of the research and their practical significance were clarified.Chapter two:Designed and synthesized of three novel fluorescence labeling reagents: 2-[2-(7H-dibenzo [a,g]-carbazol)]-isopropyl-4-methylbenzenesulfonic acid; 1-(9-methyl anthracene)-3-methyl pyrazolone; 2-[12,13-dihydrogen-(7H-dibenzo[a,g]-carbazol)]-ethanolchloroformate. Then, these reagents were described and followed by their structural characterization.Chapter there:Pre-column derivatization method for the sensitive determination of phenolic compounds using 4-(1H-phenanthro[9,10-d]imidazol-2-yl)benzoic acid (PIBA) as labeling reagents followed by HPLC-MS analysis have been developed. The optimal derivatization and chromatographic separation conditions using PIBA as labeling reagent were evaluated. And the feasibility of this method has been identified by analyzing the drain water. The results showed that this method had good reproducibility and higher detection sensitivity.Chapter four:Pre-column derivatization method for the sensitive determination of aromatic amine using 4-(1-methyl-1H [9,10-d]imidazol-2-yl)benzoic acid (MPIBA) as labeling reagents followed by HPLC-MS analysis have been developed. The optimal derivatization and chromatographic separation conditions using MPIBA as labeling reagent were evaluated. And the feasibility of this method has been identified by analyzing the drain water. The results showed that this method had simple and high detection sensitivity. Chapter five:Pre-column derivatization method for the sensitive determination of aliphatic amine using 2-[12,13-dihy4rogen-(7H-dibenzo[a,g]-carbazol)]-ethanol chloroformate as labeling reagents followed by HPLC analysis have been developed. The optimal derivatization and chromatographic separation conditions using 2-[12,13-dihydrogen-(7H-dibenzo[a,g]-carbaz ol)]-ethanol chloroformate as labeling reagent were evaluated.Chapter six:Pre-column derivatization method for the sensitive determination of aromatic amine using BCETS as labeling reagents followed by HPLC-MS analysis have been developed. And the feasibility of this method has been identified by analyzing the Microula sikkimensis seed oil. The results showed that this method can be used to determination of fatty acids.