【摘要】：毛細(xì)管電泳(Capillary Electrophoresis,CE)是一種已經(jīng)發(fā)展較為成熟的微分離技術(shù)。在CE中,所采用的化學(xué)發(fā)光(CL)檢測器因其背景干擾低、靈敏度高、線性范圍寬、儀器要求簡單等特點(diǎn)而常被用作CE的后期檢測手段�？v觀多種分析技術(shù),CE對于很多復(fù)雜分析是很有吸引力的。這是因?yàn)樵摷夹g(shù)具有很高的通用性,比其他分析技術(shù)便宜,所需樣品的量極小,對環(huán)境幾乎不造成污染,而且相比其他諸如震動光譜這一有利于分化過程的技術(shù),CE擁有更高的靈敏度。因此,CE-CL分析技術(shù)被廣泛用于測定復(fù)雜樣品中的多種生物分子,如血清和其他生理液。然而,與傳統(tǒng)的CL技術(shù)相比,CE-CL法因?yàn)橹荒芟蚍治鲶w系注入很小的一段樣品,同時(shí)檢測光程很短,從而導(dǎo)致毛細(xì)管電泳技術(shù)的檢測靈敏度還不是非常理想。所以,該技術(shù)難以檢測生物樣品基質(zhì)中的痕量組分。由此可見,提高毛細(xì)管電泳技術(shù)的檢測靈敏度就成為該領(lǐng)域的重要課題。鑒于此,本學(xué)位論文進(jìn)行了如下研究與創(chuàng)新:1.我們自主制作了簡易裝置用于頂空柱內(nèi)微萃取(Headspace In-tube Microextration,HS-ITME),并且闡釋了其制作方法、特點(diǎn)以及影響因素,我們將HS-ITME與CE進(jìn)行在線聯(lián)用并開展了如下五組實(shí)驗(yàn),通過實(shí)際的樣品測定實(shí)驗(yàn),我們驗(yàn)證了HS-ITME不僅可以有效提高CE的檢測靈敏度,還可以簡化樣品前處理的操作步驟,由此拓寬了毛細(xì)管電泳技術(shù)在復(fù)雜實(shí)際組分測定中的應(yīng)用。2.我們利用HS-ITME和CE進(jìn)行在線聯(lián)用來開展對溴酚類化合物的測定實(shí)驗(yàn)。在此實(shí)驗(yàn)中,我們考察并優(yōu)化了萃取條件(萃取溫度、萃取時(shí)間、鹽度、樣品的量等)和CE分離條件,后期基于優(yōu)化后的實(shí)驗(yàn)條件,我們進(jìn)一步測定了多種實(shí)際水體中的溴酚類物質(zhì),并通過一系列方法評估驗(yàn)證了HS-ITME可以使CE的檢測靈敏度大大提高。3.基于膠束毛細(xì)管電泳(MEKC)的分離機(jī)理,結(jié)合鄰苯二甲酸酯類物質(zhì)(PAEs)的結(jié)構(gòu)特性,我們采用反向遷移MEKC來分離PAEs,在此之前已開展了HS-ITME對PAEs的在線萃取,此過程考察且優(yōu)化了萃取條件和CE分離條件,后期基于得到的最佳實(shí)驗(yàn)條件,我們進(jìn)一步測定了多種自然水體和市售飲料中的PAEs,并通過一系列方法評估證明了HS-ITME使CE檢測靈敏度大大提高。4.參考3中的實(shí)驗(yàn)情況,我們繼續(xù)利用HS-ITME和反向遷移MEKC進(jìn)行在線聯(lián)用,來檢測菊酯類農(nóng)藥,同時(shí)考察并優(yōu)化了萃取條件和分離條件,后期我們將實(shí)驗(yàn)建立在最佳條件下,測定了多種水果中的菊酯類農(nóng)殘,最后通過一系列方法評估證明了HS-ITME使CE檢測靈敏度大大提高。5.基于1中的實(shí)驗(yàn)原理和結(jié)果以及離子液體(ILs)在CE方面的應(yīng)用,我們通過向CE運(yùn)行緩沖液中添加ILs來進(jìn)一步改善萃取效率,通過檢測多種酚類物質(zhì),我們考察并優(yōu)化了萃取條件(在1中條件的基礎(chǔ)上增加了ILs種類和濃度的影響)和分離條件,并在此條件下成功測定了實(shí)際水體中的多種酚類物質(zhì),最后通過方法評估證明了HS-ITME使HS-ITME的檢測靈敏度有效提高。
[Abstract]:Capillary Electrophoresis (CE) is a mature micro-separation technology. In CE, the chemiluminescence (CL) detector is often used as a post-detection method for CE because of its low background interference, high sensitivity, wide linear range and simple instrument requirements. Complex analysis is attractive because it is highly versatile, cheaper than other analytical techniques, requires very small amounts of samples, causes little pollution to the environment, and is more sensitive to CE than other techniques such as vibrational spectroscopy, which is conducive to the differentiation process. However, compared with traditional CL technique, CE-CL method can only inject a very small sample into the analytical system, and the detection optical path is very short, so the detection sensitivity of capillary electrophoresis is not very ideal. To improve the detection sensitivity of capillary electrophoresis (CE) has become an important topic in this field. In view of this, the following research and innovations have been made in this dissertation: 1. We have developed a simple headspace in-tube microextration (HS-ITME) device for headspace in-tube microextraction (HS-ITME). The manufacturing method, characteristics and influencing factors of HS-ITME and CE were explained. We combined HS-ITME with CE on-line and carried out the following five groups of experiments. Through the actual sample determination experiments, we verified that HS-ITME can not only effectively improve the detection sensitivity of CE, but also simplify the operation steps of sample pretreatment, thus broadening the capillary electrophoresis. In this experiment, we investigated and optimized the extraction conditions (extraction temperature, extraction time, salinity, sample amount, etc.) and the separation conditions of CE. In the later stage, based on the optimized experimental conditions, we studied and optimized the extraction conditions. HS-ITME can greatly improve the detection sensitivity of CE. 3. Based on the separation mechanism of micellar capillary electrophoresis (MEKC) and the structural characteristics of phthalate esters (PAEs), we used reverse migration MEKC to separate PAEs. The on-line extraction of PAEs by HS-ITME has been carried out before. The extraction conditions and CE separation conditions have been investigated and optimized. Based on the best experimental conditions, PAEs in various natural waters and commercial drinks have been further determined. The sensitivity of CE detection has been greatly improved by HS-ITME through a series of evaluation methods. Referring to the experiment in 3, we continue to use HS-ITME and reverse migration MEKC for on-line detection of pyrethroid pesticides, while investigating and optimizing the extraction conditions and separation conditions. Later we will establish the experiment under the best conditions to determine pyrethroid residues in a variety of fruits, and finally through a series of methods to evaluate and prove HS. Based on the experimental principle and results in 1 and the application of ionic liquids (ILs) in CE, we further improved the extraction efficiency by adding ILs to the running buffer of CE. By detecting a variety of phenolic substances, we investigated and optimized the extraction conditions (adding ILs on the basis of 1 condition). The results show that HS-ITME can effectively improve the detection sensitivity of HS-ITME.
【學(xué)位授予單位】：青島科技大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O658

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