| HPLC is a kind of high efficient separation and analysis technique. This technique can achieve rapid separation of different components in the complex matrix and qualitative and quantitative analysis. It has become one of the fastest growing, the most affected and the most widely used modern analytical methods, which has been widely used in analytical chemistry, biochemistry, clinical medicine, pharmaceutical chemistry, food hygiene, and environmental monitoring, etc. For HPLC-MS technique, HPLC is used as separation method and MS is used as the detection method. Chromatography has strong separation ability for the complex matrix samples, and MS can achieve the high selective and sensitive analysis, what’s more MS can provide relative molecular mass and structural information of analytes. However, for some compounds, the sensitivity of HPLC determination is limited. For example, when the analyte has no ultraviolet absorption or fluorescence and the ionization efficiency is very low, chemical derivatization method could be introduced to solve this problem. Dispersive liquid-liquid microextraction(DLLME) is a novel and efficient sample pretreatment technology. DLLME has many advantages such as simple, low consumption, high recovery and high enrichment factor(EFs) and the extraction procedure is very fast. Currently, DLLME has been widely used in the determination of various organic and inorganic compounds in many different matrixes. In this article, a novel hyphenated method based on dispersive liquid-liquid microextraction(DLLME) coupled to precolumn derivatization has been established for the efficiently determination of environmental estrogens and brassinolide by HPLC fluorescence detection(HPLC-FLD). The hyphenated method is verified for the feasibility of detection. A novel derivatization reagent 4′-carboxyl-rosamine has been synthesized and applied to the high sensitive detection of panoxadiol. The idiographic work is as follows:Chapter One: High performance liquid chromatography and mass spectrometry are briefly introduced in the application of modern organic analysis.Chapter Two: The introduction of the chemical derivatization sensitization and dispersive liquid-liquid microextraction pretreatment technology and their research progress.Chapter Three: The novel derivatization and dispersive liquid-liquid microextraction pretreatment hyphenated technique is applied in the high sensitive determination of environmental estrogens and brassinolide, and successfully used in the real sample analysis with high sensitivity, selectivity and speed. The established derivatization and dispersive liquid-liquid microextraction hyphenated technique is verified to be extensive applicable.Chapter Four: A novel derivatization reagent 4′-carboxyl-rosamine is synthesized and purified by the semipreparative high performance liquid chromatography.Chapter Five: 4′-Carboxyl-rosamine is used as MS sensitization reagent for the determination of panoxadiol. And ultrasonic assisted dispersive liquid-liquid microextraction technology is applied for the sample pretreatment. The method is successfully used for the sensitive determination of panoxadiol in varieties of ginseng herbs and makeup. The established method in this article has extensive applicability. The synthesized derivatization reagent also has vast application prospects. |
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