The Development Of New Type Of Derivative Reagent And The Amine Compounds In The Application Of Hplc - Ms Measurement

For the powerful separation and analytical capacities, reversed-phase highperformance liquid chromatographic method has been widely used in many fieldsof scientific research and application, such as biology, chemistry, toxicology,clinical medicine, food hygiene and environmental monitoring. It is also one of thefastest developing and the most widely used methods in analytical chemistry.However, not all compounds are accessible to be analyzed by chromatography dueto the limitation of the compounds’ properties and the low content of detectedcomponents. Therefore, developing testing methods with high sensitivity has veryimportant significance. In recent years, derivatization of analytes with fluorescentlabeling reagent has been widely adopted by many researchers. This derivatizationmethod which adopt fluorescence detection can enhance detective sensitivity in alarge extent. In this paper, one dual-sensitive probes which was sensitive not onlyto ultraviolet but also to MS ionizable potential were designed, prepared andcharacterized. The spectral properties, optimal derivatization conditions,chromatographic separation conditions and MS conditions were investigated.Pre-column derivatization methods based on reversed-phase high-performanceliquid chromatography were established and evaluated for the analysis of realsamples.Chapter One: The developing progress and basic theory about highperformance liquid chromatography and high performance liquid chromatographycoupled with mass spectrometry were simply presented. The principles ofchemical derivatization was introduced. The widely used derivatization reagentswere summarized.Chapter Two: The syntheses of4-(4-momethylbenzoic acid)-triphenylphosphonium bromide （MBATP）was described followed with their structuralcharacterization.Chapter Three: Pre-column derivatization method for the sensitivedetermination of amine compounds using MBATP as labeling reagent followed byHPLC-MS analysis has been developed. The optimal derivatization was evaluated.The proposed method showed wide linear range, excellent reproducibility, andsimple derivatization for the determination of aliphatic amines. The suitability ofthe developed method for the analysis of real sample was satisfactory.Chapter Four: Pre-column derivatization methods for the sensitivedetermination of biogenic amineswith EASC as labeling reagent followed by HPLC-MS analysis have been developed. The optimization of derivatization andchromatographic separation conditions using EASCslabeling reagent wasevaluated. Then, this method was applied to the determination of different realsamples, the results suggested that the established methods have great feasibility.Chapter Five: Based on the actual industrial production, cost savings andimproving productivity under the premise of benzyl-2--naphthyl ether synthesisconditions were optimized, and achieved satisfactory results.