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Carbazole And Synthesis Of The Imidazole Fluorescent Labeling Reagent And Its High Performance Liquid Chromatography - Mass Spectrometry Applications

Posted on:2011-06-15Degree:MasterType:Thesis
Country:ChinaCandidate:X Y LiFull Text:PDF
GTID:2191360305468598Subject:Organic Chemistry
Abstract/Summary:PDF Full Text Request
High performance liquid chromatography(HPLC) is one of the most capable methods of separating complex mixture due to its powerful capacity. It has been enthusiastically and widely used in many research fields and industrial systems, such as clinical medicane, biochemistry, food hygiene, environmental monitoring and quality control. However, not all compounds are accessible to directly analysis by HPLC when the contents of the samples are less or limited by its nature, as they reduced the detection sensitivity significantly. In recent years, many researchers have used chemical derivatization in HPLC in attempt to improve detection sensitivity and separation efficiency. Although a number of different types of fluorescent tagging reagents have been developed, many reports have described various shortcomings in application. Therefore, it is highly significant to develop high sensitivity fluorescent regents to meet the actual needs of HPLC. The dominant ideology of this paper is to design a new fluorescent derivatization reagent to enhance detection sensitivity and overcome the shortcomings of existing reagents in actually analysis process. It is detailed as follows:design and syntheses of new tagging reagents, identification of spectral properties, development of new derivatization reaction, optimization of the chromatographic separation conditions, research of mass spectrometry quantitative and qualitative, analysis of real sample and so on. Specific works are as follows:Chapter one:The development and basic theory of high performance liquid chromatography and high performance liquid chromatography coupled with mass spectrometry technique were systematically reviewed. The principles and development of fluorescent derivatization were simply introduced. At last, the derivative reagents widely used in recent years were cited.Chapter two:Two novel fluorescent lableling reagents were synthesized: 2-[2-(4-dimethylamino)phenyl-l-hydrogen-philippine[9,10-d]imidazole]-acetic acid(DMAPPIA), 2-[2-(7H-dibenzo[a,g]carbazole-ethoxy)]-ethyl chloroformate (DBCEC-C1). Then, their structure and spectroscopic properties were characterized.Chapter there:Pre-column derivatization methods for the sensitive determination of aliphatic amines with 2-[2-(4-dimethylamino)-phenyl-l-hydrogen-philippine [9,10-d]imidazole]-acetic acid (DMAPPIA) as labeling reagents followed by HPLC-MS analysis have been developed. The optimization of derivatization and chromatographic separation conditions using DMAPPIA as labeling reagent were evaluated. Then, the established method has applied to analyze Rotten fish and Shrimp paste samples, the results showed that the method had great feasibility. Chapter four:Pre-column derivatization methods for the sensitive determination of aromatic amines, phenolic compounds and 20 kinds of amino acids with 2-[2-(7H-dibenzo[a,g]carbazole-ethoxy)]-ethyl chloroformate (DBCEC-C1) as labeling reagents followed by HPLC-MS analysis have been developed. The optimization of derivatization and chromatographic separation conditions using DBCEC-C1 as labeling reagent were evaluated. Then, the established method has applied to analyze the real samples, the results showed that the method had great feasibility.
Keywords/Search Tags:High performance liquid chromatography-mass spectrometry, fluorescent labeling reagents, pre-column, aliphatic amines, aromatic amines, phenolic compounds, amino acid
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