罗丹明类衍生试剂原位衍生联合液相色谱质谱分析方法的开发

发布时间：2018-10-25 17:25

【摘要】：超高效液相色谱质谱(UHPLC-MS)作为一种新型检测技术,发展速度迅速,具有强大的分离分析能力而被运用于各个领域,比如生命分析、药物分析、食品卫生及环境化学等。该方法具有发展速度快、应用广泛等特点,良好的分离特性使之受到了诸多领域的关注。UHPLC-MS技术不仅运用范围广泛,且具有选择性好、灵敏度高、分离度高等特点,可以根据碎裂离子和图谱推断分析物的相对分子质量和物质结构。一般样品的检测量都比较小,或者需要检测的组分的含量很低,并且很多化合物不适合色谱分析的直接检测,没有良好的紫外或荧光吸收,然而需要得到较高的检测灵敏度。因此,化学衍生化作为改善以上问题的有效技术手段往往被引入。超声辅助分散液液微萃取(UA-DLLME)不仅高效快速且具有强大的富集、净化能力而受到了广泛关注并作为前处理技术而被运用。UA-DLLME具有萃取率高、简单、快速等优势而被广泛运用于分析物的富集、净化过程。本论文开发了一种新型高效的超声辅助-原位衍生-分散液液微萃取的样品前处理技术,联合超高液相色谱质谱(UHPLC-MS)检测分析,用于生物样本的检测工作。一种新型的用于生物样品分析物衍生标记的罗丹明类试剂4′-甲酰氯罗丹明,成功被用于神经递质和食品中氨基酸和生物胺的含量检测。本文具体工作如下:第一章:简述了UHPLC-MS在分析化学工作中的应用进展。第二章:介绍了化学衍生化增敏技术与液液微萃取技术,及UA-DLLME技术联合衍生前处理技术研究。第三章:采用超声辅助-原位衍生-分散液液微萃取的样品前处理技术成功应用于帕金森病模型大鼠脑微透析液中多种神经递质快速检测。第四章:利用衍生试剂4′-甲酰氯罗丹明,首次对大鼠尿液中的神经递质进行衍生标记,结果表明本论文所建立方法能够很好的运用到生物样本的检测分析。第五章:以4′-甲酰氯罗丹明作为质谱增敏试剂,对食品中的氨基酸和生物胺进行衍生标记,结果表明本论文所建立的实验方法和新合成的衍生试剂能够成功运用不同食品氨基酸和生物胺含量测定。
[Abstract]:As a new detection technology, ultra-high performance liquid chromatography-mass spectrometry (UHPLC-MS) has been widely used in many fields, such as life analysis, drug analysis, food hygiene and environmental chemistry. This method has the characteristics of rapid development, wide application and good separation characteristics. UHPLC-MS technology is not only widely used, but also has good selectivity, high sensitivity, high separation degree and so on. The molecular weight and structure of the analyte can be inferred from the fragmentation ions and spectra. Generally, the detection of samples is relatively small, or the content of the components to be detected is very low, and many compounds are not suitable for the direct detection of chromatographic analysis, there is no good UV or fluorescence absorption, but high detection sensitivity is needed. Therefore, chemical derivation is often introduced as an effective technical means to improve the above problems. Ultrasound-assisted dispersible liquid microextraction (UA-DLLME) is not only highly efficient and rapid, but also has a strong enrichment, purification ability and has been widely concerned and used as a pretreatment technology. UA-DLLME has a high extraction rate and is simple. Rapid and other advantages are widely used in the enrichment and purification process of analytes. In this paper, a new and high efficient ultrasonic assisted in situ derivation-dispersion liquid microextraction sample pretreatment technique was developed, which was combined with ultra-high liquid chromatography-mass spectrometry (UHPLC-MS) for the detection of biological samples. A new type of Rhodamine reagent 4-formyl chloride rhodamine was successfully used for the determination of amino acids and biogenic amines in neurotransmitters and foods. The main work of this paper is as follows: chapter 1: the application of UHPLC-MS in analytical chemistry is reviewed. Chapter 2: the research of chemical derivatization sensitizing technology, liquid-liquid microextraction technology and UA-DLLME combined derivatization pretreatment technology are introduced. Chapter 3: the ultrasonic assisted in situ derivation-dispersion liquid microextraction technique was successfully applied to the rapid detection of multiple neurotransmitters in the cerebral microdialysis solution of Parkinson's disease model rats. Chapter 4: the method was used to label the neurotransmitters in rat urine for the first time. The results showed that the method established in this paper could be applied to the detection and analysis of biological samples for the first time. Chapter 5: amino acids and biogenic amines in food were labeled with 4-formyl chloride rhodamine as the sensitizing reagent by mass spectrometry. The results show that the experimental method and the newly synthesized derivative reagent can be used successfully to determine the amino acids and biogenic amines in different foods.
【学位授予单位】：曲阜师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.63;TS207.3

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