本文選題：毛細(xì)管電泳 + 毛細(xì)管電動(dòng)分級(jí)提取　； 參考：《福州大學(xué)》2014年博士論文

【摘要】：復(fù)雜樣品的分離分析是近年分析科學(xué)領(lǐng)域的重要研究熱點(diǎn)及難點(diǎn)之一。本論文在傳統(tǒng)毛細(xì)管電泳的理論基礎(chǔ)上建立一種全新的毛細(xì)管電泳技術(shù)——毛細(xì)管電動(dòng)分級(jí)分離技術(shù)(CEkF),并將其與高分辨質(zhì)譜技術(shù)聯(lián)用,對(duì)幾個(gè)典型的復(fù)雜樣品進(jìn)行分析鑒定。論文共分為七章,主要內(nèi)容如下：第一章,介紹了復(fù)雜樣品的定義及特征、毛細(xì)管電泳與高分辨質(zhì)譜聯(lián)用技術(shù)的特點(diǎn)及優(yōu)勢(shì),并對(duì)本論文建立的毛細(xì)管電動(dòng)分級(jí)分離技術(shù)的理論基礎(chǔ)和方案設(shè)計(jì)進(jìn)行詳述。第二章,選取14個(gè)代表性模型化合物,采用CEkF技術(shù),根據(jù)模型化合物的信號(hào)強(qiáng)度隨基質(zhì)pH變化的規(guī)律建立半經(jīng)驗(yàn)?zāi)Ｐ?推導(dǎo)pKa的計(jì)算公式。該模型無(wú)需復(fù)雜的分離,實(shí)現(xiàn)了多種目標(biāo)物pKa的同時(shí)測(cè)定以及結(jié)構(gòu)的推測(cè)。第三章,在pKa測(cè)定模型的基礎(chǔ)上,將建立的CEkF技術(shù)與傅里葉變換離子回旋共振(Fourier transform ion cyclotron resonance, FTICR)質(zhì)譜準(zhǔn)在線聯(lián)用對(duì)葡萄酒中主要代謝物進(jìn)行分析。實(shí)現(xiàn)了對(duì)葡萄酒重要標(biāo)志性成分的鑒定,并證明了在極酸性條件下,CEkF技術(shù)對(duì)葡萄酒中的含硫化合物具有極高的選擇性。第四章,利用CEkF技術(shù)對(duì)含硫化合物的高選擇性,以及FTICR/MS的超高分辨率,實(shí)現(xiàn)對(duì)復(fù)雜樣品二級(jí)有機(jī)氣溶膠中水溶性有機(jī)化合物——有機(jī)磺酸酯的分析鑒定。在極酸性條件下,鑒定出生物燃燒質(zhì)樣品中有機(jī)磺酸酯以及硝基有機(jī)磺酸酯500余種。第五章,將制備型CEkF技術(shù)與超高分辨的FTICR/MS以及高場(chǎng)核磁共振(Nuclear magnetic resonance, NMR)技術(shù)準(zhǔn)在線聯(lián)用,實(shí)現(xiàn)了天然有機(jī)質(zhì)代表物——Suwannee River黃腐酸(Suwannee River fulvic acid, SRFA)的分子層面的表征。這是電泳技術(shù)首次與NMR聯(lián)用用于復(fù)雜樣品的研究。第六章,采用CE-ESI/MS檢測(cè)聯(lián)用技術(shù),以電動(dòng)進(jìn)樣的場(chǎng)放大(Field amplified sample stacking, FASS)技術(shù)作為在線富集方法,實(shí)現(xiàn)了藻類樣品中微囊藻毒素異構(gòu)體的同時(shí)分離檢測(cè)以及尿液中β2-激動(dòng)劑的快速、靈敏的分離檢測(cè)。第七章,采用高效液相色譜-三重四級(jí)桿串聯(lián)質(zhì)譜技術(shù)對(duì)失憶性貝毒——軟骨藻酸的穩(wěn)定性進(jìn)行考察。并在最佳色譜條件下,成功實(shí)現(xiàn)了海水樣品及貝類樣品中軟骨藻酸的檢測(cè)。
[Abstract]:The separation and analysis of complex samples is one of the hot and difficult points in the field of analytical science in recent years. Based on the theory of traditional capillary electrophoresis (CE), a new capillary electrokinetic separation technique, CEkFN, was established in this paper, and it was combined with high resolution mass spectrometry (HRMS) to analyze and identify several typical complex samples. The paper is divided into seven chapters. The main contents are as follows: in Chapter 1, the definition and characteristics of complex samples, the characteristics and advantages of capillary electrophoresis and high resolution mass spectrometry are introduced. The theoretical basis and scheme design of the capillary electrokinetic separation technology established in this paper are described in detail. In the second chapter, 14 representative model compounds are selected and CEKF technique is used to establish semi-empirical model according to the change of signal intensity of model compounds with pH of matrix, and the calculation formula of PKA is deduced. The model can simultaneously determine PKA and conjecture the structure without complicated separation. In chapter 3, on the basis of PKA determination model, the main metabolites in wine were analyzed by using the established CEKF technique and Fourier transform ion cyclotron resonance Fourier transform ion cyclotron resonance, FTICR mass spectrometry. It is proved that CEKF has a high selectivity to sulfur compounds in wine under extremely acidic conditions. In chapter 4, the high selectivity of sulfur compounds by CEkF technique and the ultra-high resolution of FTICR / MS are used to analyze and identify the water-soluble organic compounds-organic sulfonic acid esters in secondary organic aerosols of complex samples. More than 500 kinds of organic sulfonic esters and nitroorganic sulfonic esters were identified in the biocombustible samples under extremely acidic conditions. In chapter 5, the synthetic CEKF technique is combined with ultrahigh resolution FTICR / MS and high field nuclear magnetic resonance (NMRs) to characterize the molecular level of natural organic matter, Suwannee River fulvic acid suwannee fulvic acid. This is the first time that electrophoretic technique is combined with NMR to study complex samples. In chapter 6, the simultaneous separation and detection of microcystin isomers in algae samples and the rapid detection of 尾 _ 2-agonist in urine were achieved by using the CE-ESI / MS technique and the field amplification amplified sample stacking, FASS technique of electric injection as the on-line enrichment method. Sensitive separation and detection. In chapter 7, the stability of amnesic shellfish-alginic acid was investigated by high performance liquid chromatography-quadruplex tandem mass spectrometry. Under the optimum chromatographic conditions, the determination of alginic acid in seawater and shellfish samples was successfully realized.
【學(xué)位授予單位】：福州大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2014
【分類號(hào)】：R917;O657.63

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