微流蒸发光散射检测器的优化及其与加压毛细管电色谱联用的研究

发布时间：2019-01-01 08:29

【摘要】：加压毛细管电色谱（pressurized capillary electrochromatography,pCEC）技术源于毛细管电色谱（capillary electrochromatography, CEC），具有高柱效、高选择性、高分离度、快速分离（即“三高一快”）的特点，，且其样品和试剂消耗少、易与其他检测器在线联用。因此，在生化分析、手性分离、神经科学、蛋白质和多肽研究、医药分析等领域得到广泛应用，尤其在复杂样品分析中凸显出无可比拟的优势。目前，适用于加压毛细管电色谱的检测手段有紫外、电化学检测器、激光诱导荧光、核磁共振和质谱等，缺乏一种经济的通用型检测器。这在一定程度上制约和限制了毛细管微分离技术的广泛应用。蒸发光散射检测器（evaporative light scattering detector，ELSD）是一种通用型质量检测器，能检测挥发性低于流动相的任何样品，不受物质本身结构的限制，适用于食品安全、药物分析、中药分析等领域。因此，对ELSD进行微流微型化，并实现与加压毛细管电色谱的联用，具有非常重要的意义。基于上述背景，我们进行了蒸发光散射检测器的微流微型化研究并与毛细管色谱技术联用。本研究对初步构建的微流蒸发光散射检测器进行雾化系统和蒸发系统的优化，突破性的降低了雾化载气流速，改善了色谱峰形，扩大了仪器使用范围；考察了仪器基线本底噪声来源；构建加压毛细管电色谱-微流蒸发光散射检测器联用平台，在联用平台建立注射用血塞通（冻干）5种皂苷的检测方法，证明联用平台的稳定性和实用性。实验证明构建的pCEC-μELSD联用系统能用于药物中有效成分的含量测定。μELSD的构建为毛细管液相色谱、毛细管电色谱和毛细管电泳分离技术提供了一种全新的检测手段。
[Abstract]:Pressurized capillary electrochromatography (pressurized capillary electrochromatography,pCEC) technology is derived from the high column efficiency, high selectivity, high separation degree, rapid separation (i.e. "three high and one fast") of capillary electrochromatography (capillary electrochromatography, CEC), and less consumption of samples and reagents. Easy to use with other detectors online. Therefore, it has been widely used in the fields of biochemical analysis, chiral separation, neuroscience, protein and polypeptide research, pharmaceutical analysis and so on, especially in complex sample analysis. At present, UV, electrochemical detector, laser-induced fluorescence, nuclear magnetic resonance (NMR) and mass spectrometry are suitable for pressure capillary electrochromatography. To some extent, it restricts and limits the wide application of capillary microseparation technology. Evaporative Light scattering detector (evaporative light scattering detector,ELSD) is a universal mass detector that can detect any sample whose volatility is lower than that of the mobile phase, free from the structure of the substance itself, and suitable for food safety and drug analysis. Traditional Chinese medicine analysis and other fields. Therefore, it is of great significance to miniaturize ELSD and combine it with pressurized capillary electrochromatography. Based on the above background, we have studied the microfluidization of evaporative light scattering detector and combined with capillary chromatography. In this study, the atomization system and evaporation system were optimized for the initially constructed micro-flow evaporative light scattering detector, which greatly reduced the velocity of atomized carrier airflow, improved the chromatographic peak shape, and expanded the scope of use of the instrument. The source of background noise from the baseline of the instrument was investigated. A pressure capillary electrochromatography-microflow evaporative light scattering detector (VLS) platform was established to establish a method for the determination of five saponins in Xuesetong (freeze-dried) for injection. The stability and practicability of the platform were proved. The results show that the pCEC- 渭 ELSD system can be used for the determination of the active components in drugs. The construction of 渭 ELSD provides a new detection method for capillary liquid chromatography, capillary electrochromatography and capillary electrophoresis separation.
【学位授予单位】：上海交通大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：R927;O657

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