發(fā)布時間：2019-01-01 08:29

【摘要】：加壓毛細(xì)管電色譜（pressurized capillary electrochromatography,pCEC）技術(shù)源于毛細(xì)管電色譜（capillary electrochromatography, CEC），具有高柱效、高選擇性、高分離度、快速分離（即“三高一快”）的特點，，且其樣品和試劑消耗少、易與其他檢測器在線聯(lián)用。因此，在生化分析、手性分離、神經(jīng)科學(xué)、蛋白質(zhì)和多肽研究、醫(yī)藥分析等領(lǐng)域得到廣泛應(yīng)用，尤其在復(fù)雜樣品分析中凸顯出無可比擬的優(yōu)勢。目前，適用于加壓毛細(xì)管電色譜的檢測手段有紫外、電化學(xué)檢測器、激光誘導(dǎo)熒光、核磁共振和質(zhì)譜等，缺乏一種經(jīng)濟的通用型檢測器。這在一定程度上制約和限制了毛細(xì)管微分離技術(shù)的廣泛應(yīng)用。蒸發(fā)光散射檢測器（evaporative light scattering detector，ELSD）是一種通用型質(zhì)量檢測器，能檢測揮發(fā)性低于流動相的任何樣品，不受物質(zhì)本身結(jié)構(gòu)的限制，適用于食品安全、藥物分析、中藥分析等領(lǐng)域。因此，對ELSD進(jìn)行微流微型化，并實現(xiàn)與加壓毛細(xì)管電色譜的聯(lián)用，具有非常重要的意義�；谏鲜霰尘�，我們進(jìn)行了蒸發(fā)光散射檢測器的微流微型化研究并與毛細(xì)管色譜技術(shù)聯(lián)用。本研究對初步構(gòu)建的微流蒸發(fā)光散射檢測器進(jìn)行霧化系統(tǒng)和蒸發(fā)系統(tǒng)的優(yōu)化，突破性的降低了霧化載氣流速，改善了色譜峰形，擴大了儀器使用范圍；考察了儀器基線本底噪聲來源；構(gòu)建加壓毛細(xì)管電色譜-微流蒸發(fā)光散射檢測器聯(lián)用平臺，在聯(lián)用平臺建立注射用血塞通（凍干）5種皂苷的檢測方法，證明聯(lián)用平臺的穩(wěn)定性和實用性。實驗證明構(gòu)建的pCEC-μELSD聯(lián)用系統(tǒng)能用于藥物中有效成分的含量測定。μELSD的構(gòu)建為毛細(xì)管液相色譜、毛細(xì)管電色譜和毛細(xì)管電泳分離技術(shù)提供了一種全新的檢測手段。
[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.
【學(xué)位授予單位】：上海交通大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2014
【分類號】：R927;O657

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