本文選題：毛細(xì)管電泳 + 分散液液微萃取��； 參考：《煙臺(tái)大學(xué)》2016年碩士論文

【摘要】：環(huán)境水體中污染物含量較低,且基質(zhì)復(fù)雜、干擾物質(zhì)較多,因而,在檢測(cè)污染物之前需要對(duì)實(shí)際樣品進(jìn)行預(yù)處理,以達(dá)到對(duì)待測(cè)物濃縮凈化的目的。液液萃取和固相萃取是兩種較為經(jīng)典的傳統(tǒng)樣品前處理技術(shù),然而,這種傳統(tǒng)的樣品前處理技術(shù)需要消耗大量的有機(jī)試劑,過程復(fù)雜,耗時(shí)較長,對(duì)環(huán)境和人體造成危害。分散液液微萃取(DLLME)和分散固相萃取(dSPE)是在傳統(tǒng)的液液萃取和固相萃取的基礎(chǔ)上發(fā)展而來的新型樣品前處理技術(shù),以其簡單、快速、高效等優(yōu)勢(shì)得到了快速的發(fā)展,廣泛應(yīng)用于各種樣品的檢測(cè),受到廣大分析工作者的關(guān)注。毛細(xì)管電泳(CE)是一種相對(duì)成熟的分離檢測(cè)技術(shù),具有分析速度快、樣品用量少、自動(dòng)化程度高的優(yōu)點(diǎn),在環(huán)境、醫(yī)藥、食品等各個(gè)領(lǐng)域有著廣泛的應(yīng)用。在本文中,采用新型的樣品前處理技術(shù)與毛細(xì)管電泳結(jié)合檢測(cè)環(huán)境水樣中的污染物,并探究了毛細(xì)管電泳的在線富集技術(shù)用于檢測(cè)酚類雌激素。本文主要包括以下內(nèi)容:第1章,緒論,著重介紹了分散液液微萃取和分散固相萃取兩種新型的樣品前處理技術(shù)。介紹了毛細(xì)管電泳技術(shù)的原理、分離模式、在線富集技術(shù)等。闡述了論文研究的依據(jù)及主要內(nèi)容。第2章,采用分散固相萃取的前處理技術(shù)結(jié)合毛細(xì)管電泳檢測(cè)環(huán)境水樣中的有機(jī)汞。首次采用自主合成的巰基功能化材料作為分散固相萃取的吸附劑,并使用含有鹽酸的L-半胱氨酸溶液作為洗脫劑進(jìn)行洗脫。對(duì)合成的材料進(jìn)行掃描電鏡表征,對(duì)影響萃取效果的前處理?xiàng)l件進(jìn)行了優(yōu)化,包括溶液pH,吸附劑的用量,洗脫劑的體積以及洗脫溶液中鹽酸的濃度。在最優(yōu)的條件下,我們得到甲基汞和苯基汞的線性范圍是2-200μg/L,乙基汞的線性范圍是4-200μg/L,分析物的檢出限和定量限為0.24-1.07μg/L和0.79-3.57μg/L,富集倍數(shù)為109-184。此方法成功應(yīng)用于自來水和湖水中有機(jī)汞的分析,回收率為62.3%-107.2%,RSDs為3.5 10.1%,結(jié)果滿意。第3章,采用分散液液微萃取的樣品前處理技術(shù)結(jié)合膠束電動(dòng)色譜(MEKC)檢測(cè)環(huán)境水樣中的己烷雌酚、雙酚A、己烯雌酚和雙烯雌酚四種雌激素。實(shí)驗(yàn)考察了毛細(xì)管電泳條件和分散液液微萃取的前處理?xiàng)l件。在最優(yōu)的條件下,我們得到四種分析物的富集因子為241-467,檢出限分別為0.3-0.6μg/L。將方法DLLME-MEKC成功應(yīng)用于海水、湖水、自來水三種的真實(shí)水樣中雌激素的檢測(cè),回收率在70.4 108.1%之間,RSDs為2.1 9.7%,結(jié)果令人滿意。第4章,在膠束電動(dòng)色譜的模式下,采用壓力輔助電動(dòng)進(jìn)樣的進(jìn)樣方式在線富集四種酚類雌激素,對(duì)影響富集效果的進(jìn)樣電壓、進(jìn)樣時(shí)間等進(jìn)行考察,并與傳統(tǒng)的壓力進(jìn)樣進(jìn)行比較。在最優(yōu)的條件下,四種分析物在壓力輔助電動(dòng)進(jìn)樣時(shí)得到的檢出限為0.0071-0.017 mg/L,富集倍數(shù)為11-15。
[Abstract]:The content of pollutants in environmental water is relatively low, the matrix is complex, and there are many interfering substances. Therefore, it is necessary to pretreat the actual samples before detecting the pollutants in order to achieve the purpose of concentrating and purifying the test materials. Liquid-liquid extraction and solid-phase extraction are two classical traditional sample pretreatment techniques. However, this traditional sample pretreatment technology needs a large number of organic reagents, the process is complex and time-consuming, which is harmful to the environment and human body. Dispersible liquid microextraction (DLLME) and dispersed solid phase extraction (dSPE) are new sample pretreatment techniques developed on the basis of traditional liquid-liquid extraction and solid-phase extraction. Widely used in the detection of various samples, the majority of analysts pay attention to. Capillary electrophoresis (CE) is a relatively mature separation and detection technology with the advantages of fast analysis, less sample consumption and high automation. CE has been widely used in many fields, such as environment, medicine, food and so on. In this paper, a new sample pretreatment technique combined with capillary electrophoresis was used to detect pollutants in environmental water samples, and the on-line enrichment technique of capillary electrophoresis was explored for the detection of phenolic estrogens. The main contents of this paper are as follows: chapter 1, introduction, focusing on two new sample pretreatment techniques: dispersible liquid microextraction and dispersible solid phase extraction. The principle, separation mode and on-line enrichment of capillary electrophoresis were introduced. The basis and main contents of this paper are expounded. In chapter 2, organic mercury in environmental water samples was determined by dispersive solid phase extraction (DSPE) combined with capillary electrophoresis (CE). For the first time, the self-synthesized thiol functionalized material was used as the adsorbent for dispersive solid-phase extraction, and the L-cysteine solution containing hydrochloric acid was used as the eluent for elution. Scanning electron microscope (SEM) was used to characterize the synthesized materials. The pretreatment conditions affecting the extraction effect were optimized, including the pH of the solution, the amount of adsorbent, the volume of eluent and the concentration of hydrochloric acid in the elution solution. Under the optimal conditions, the linear range of methylmercury and phenyl mercury is 2-200 渭 g / L, the linear range of ethyl mercury is 4-200 渭 g / L, the detection and quantification limits of the analyte are 0.24-1.07 渭 g / L and 0.79-3.57 渭 g / L, and the enrichment multiple is 109-184. The method has been successfully applied to the analysis of organic mercury in tap water and lake water. The recovery rate is 62.3- 107.2 and the RSDs is 3.5 ~ 10.1.The results are satisfactory. In chapter 3, the sample pretreatment technique of dispersive liquid microextraction and micellar electrokinetic chromatography (MEKC) were used to detect four kinds of estrogens in environmental water samples, such as hexanoestrin, bisphenol A, diethylstilbestrol and dienoestriol. The conditions of capillary electrophoresis and the pretreatment of dispersive liquid microextraction were investigated. Under the optimal conditions, the enrichment factors of the four analytes were 241-467, and the detection limits were 0.3-0.6 渭 g / L. DLLME-MEKC was successfully applied to the determination of estrogen in seawater, lake water and tap water. The recovery rate was between 70.4 and 108.1% and the RSDs was 2.1%. The results were satisfactory. In chapter 4, in the mode of micellar electrokinetic chromatography, four phenolic estrogens were enriched online by pressure-assisted electrokinetic sampling, and the sampling voltage and injection time which affected the enrichment effect were investigated. And compared with the traditional pressure injection. Under the optimum conditions, the detection limit of the four analytes was 0.0071-0.017 mg / L and the enrichment factor was 11-15 when the pressure assisted electric injection was carried out.
【學(xué)位授予單位】：煙臺(tái)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：X832;O658.9
，

本文編號(hào)：2115269