本文選題：毛細(xì)管電泳柱上富集 + pH調(diào)制堆積�。� 參考：《河北大學(xué)》2016年碩士論文

【摘要】：高效毛細(xì)管電泳技術(shù)具有分析速度快、分離效率高等優(yōu)點(diǎn),為了進(jìn)一步提高毛細(xì)管電泳方法的靈敏度,基于毛細(xì)管柱的柱上富集方法一直是毛細(xì)管電泳研究的熱點(diǎn)之一,本文建立了型態(tài)可調(diào)陽(yáng)離子有機(jī)物的兩種毛細(xì)管電泳柱上富集的新機(jī)制,旨在提高其在毛細(xì)管電泳檢測(cè)中的靈敏度,同時(shí)尋求一種簡(jiǎn)單快速、綠色環(huán)保的毛細(xì)管電泳柱上富集檢測(cè)方法。本文共分3章,其主要內(nèi)容如下:第1章:緒論。介紹了高效毛細(xì)管電泳分離的基本原理及分離的突出特點(diǎn),詳細(xì)綜述了近年來(lái)高效毛細(xì)管電泳柱上富集的方法及其研究進(jìn)展,在文獻(xiàn)調(diào)研的基礎(chǔ)上發(fā)現(xiàn)各個(gè)富集方法的優(yōu)劣之處,對(duì)型態(tài)可調(diào)陽(yáng)離子有機(jī)物毛細(xì)管電泳柱上富集的研究提供了思路和方法。第2章:本章建立了pH調(diào)制堆積技術(shù)檢測(cè)型態(tài)可調(diào)陽(yáng)離子有機(jī)物的新機(jī)制。該機(jī)制通過(guò)樣品區(qū)帶pH的變化,調(diào)節(jié)樣品區(qū)帶的電導(dǎo)率和型態(tài)可調(diào)陽(yáng)離子有機(jī)物的帶電狀態(tài),從而改變分析物遷移速率實(shí)現(xiàn)其柱上富集,該機(jī)制具有操作簡(jiǎn)單、快速,綠色環(huán)保等特點(diǎn)。在本工作中,以選擇苯胺類(lèi)和維生素B類(lèi)物質(zhì)作為型態(tài)可調(diào)陽(yáng)離子有機(jī)物分析模型分子,進(jìn)行了pH調(diào)制新機(jī)制的分析與檢測(cè):通過(guò)酸引入pH調(diào)制堆積對(duì)環(huán)境水樣中的聯(lián)苯胺和鄰-甲基苯胺進(jìn)行了富集分離,加標(biāo)回收率在94.3-101.7%之間;通過(guò)堿引入pH調(diào)制堆積對(duì)人體尿樣中的維生素B1和煙酰胺進(jìn)行了富集分離,加標(biāo)率在83.4-106.3%之間。第3章:本章建立了水凝膠半封閉毛細(xì)管柱抑制電滲流-瞬時(shí)等速電泳檢測(cè)型態(tài)可調(diào)陽(yáng)離子有機(jī)物的新機(jī)制。本文用水凝膠將毛細(xì)管柱的一端進(jìn)行封閉,減弱了毛細(xì)管柱中液體的整體流動(dòng),抑制了電滲流。與高酸度條件下抑制電滲流的方法相比,水凝膠半封閉毛細(xì)管柱電滲流抑制法更容易在較高pH條件下,實(shí)現(xiàn)瞬時(shí)等速電泳柱上富集。與傳統(tǒng)的毛細(xì)管柱壁改性修飾抑制電滲流法相比,水凝膠半封閉法達(dá)到電滲流抑制目的的實(shí)驗(yàn)操作更為簡(jiǎn)單。首先,選取二甲亞砜(DMSO)為中性標(biāo)記物,以毛細(xì)管區(qū)帶電泳為分離模式,對(duì)比了不同pH值下電泳分離過(guò)程中在毛細(xì)管柱陽(yáng)極端使用或不使用水凝膠時(shí),DMSO的出峰時(shí)間的變化,從而對(duì)半封閉毛細(xì)管抑制電泳中的電滲流方法的可靠性進(jìn)行了驗(yàn)證。然后,以三聚氰胺作為型態(tài)可調(diào)陽(yáng)離子有機(jī)物的分析物模型,電泳時(shí)使用水凝膠半封閉毛細(xì)管柱,在較高pH值下(pH5.6)通過(guò)瞬時(shí)等速電泳富集法檢測(cè)了牛奶中的三聚氰胺。三聚氰胺在0.01-10 mg/L范圍內(nèi)峰面積與濃度具有良好的線性,實(shí)際牛奶樣品的加標(biāo)回收率在89.1-113.8%之間。
[Abstract]:High performance capillary electrophoresis (HPCE) has the advantages of fast analysis and high separation efficiency. In order to further improve the sensitivity of capillary electrophoresis, capillary column enrichment method has always been one of the hotspots in capillary electrophoresis. In this paper, two capillary electrophoresis columns with adjustable Yang separated organic compounds were enriched. The new mechanism is designed to improve its sensitivity in capillary electrophoresis detection and to seek a simple, fast, green and environmentally friendly capillary electrophoresis column enrichment detection method. This paper is divided into 3 chapters. The main contents are as follows: first chapter: introduction. The basic principle of high performance capillary electrophoresis separation and the outstanding characteristics of separation are introduced. The method and progress in the enrichment of high performance capillary electrophoresis (HPCE) on the column of high performance capillary electrophoresis (HPCE) have been found on the basis of literature research, and the advantages and disadvantages of the enrichment methods are found. The second chapter: this chapter has established the adjustable cation of pH modulation Accumulation Technology in this chapter. A new mechanism of organic matter. Through the change of pH in the sample area, the mechanism regulates the electrical conductivity of the sample zone and the electrified state of the cationic organic matter, thus changing the migration rate of the analyte to the enrichment of the column. This mechanism has the characteristics of simple operation, rapid and green environmental protection. In this work, the selection of aniline and vitamin B is selected. As a model molecule of adjustable cationic organic matter analysis model, a new mechanism of pH modulation was analyzed and detected. Through the introduction of acid into pH modulation accumulation, the concentration and separation of benzidine and O methylaniline in environmental water samples were enriched and the recovery rate was between 94.3-101.7%; pH modulation accumulation was introduced to the dimension of human urine by the alkali introduction. The concentration and separation of raw B1 and nicotinamide were concentrated and separated and the standard rate was between 83.4-106.3%. The third chapter: a new mechanism of adjustable cation organics was established by the hydrogel semi closed capillary column restraining the electroosmotic percolation transient isokinetic electrophoresis. The end of the capillary column was closed by the hydrogel, and the liquid whole in the capillary column was weakened. Compared with the method of suppressing the electroosmotic seepage under high acidity, the hydrogel semi closed capillary column electroosmotic seepage suppression method is more likely to be enriched in the instantaneous isokinetic electrophoresis column under the higher pH condition. Compared with the traditional capillary wall modified modified electroosmotic flow method, the hydrogel semi closed method achieves the electroosmotic flow suppression. The experimental operation of the purpose is more simple. First, two methyl sulfoxide (DMSO) is selected as neutral marker, and capillary zone electrophoresis is used as the separation mode. The variation of the peak time of the DMSO in the capillary positive or non use of hydrogels at the capillary column sun at different pH values is compared. The reliability of the electroosmotic method was verified. Then, using melamine as an analytical model of the adjustable cationic organic matter, a hydrogel semi closed capillary column was used for electrophoresis to detect melamine in milk at a high pH value (pH5.6) by instantaneous isokinetic electrophoresis enrichment. The peak of melamine in the range of 0.01-10 mg/L was detected. The area and concentration had good linearity, and the recovery rate of the actual milk samples was between 89.1-113.8%.
【學(xué)位授予單位】：河北大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類(lèi)號(hào)】：O658.9

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