本文選題：環(huán)境雌激素 + 鹽析輔助液液萃取　； 參考：《河北大學(xué)》2017年碩士論文

【摘要】：環(huán)境雌激素為內(nèi)分泌干擾物的一類,是指能夠模擬或干擾生物體內(nèi)分泌功能的物質(zhì),可通過食物鏈在生物體內(nèi)富集,也可通過環(huán)境暴露(水)與生物體接觸,從而影響生物體的各個系統(tǒng),破壞機(jī)體內(nèi)環(huán)境的穩(wěn)定,危害生物體的健康。因此,對各類水體中環(huán)境雌激素的監(jiān)測具有十分重要的意義。本文建立了兩種新型樣品預(yù)處理方法對水中的環(huán)境雌激素進(jìn)行監(jiān)測。全文共分為3章,其基本內(nèi)容如下:第一章:簡要概述了樣品預(yù)處理的方法。其中重點(diǎn)闡述了分散液液微萃取及環(huán)境雌激素的萃取方法,以及本文的選題背景和研究內(nèi)容。第二章:建立了逆流鹽析均勻液液萃取-分散液液微萃取結(jié)合高效液相色譜(HPLC-UV)測定水中的環(huán)境雌激素。本實(shí)驗(yàn)考察了逆流鹽析均勻液液萃取方法的萃取劑種類及體積、流速、水樣的pH和分散液液微萃取方法的萃取劑種類及體積和離子強(qiáng)度對萃取效率的影響,并對該方法進(jìn)行了系統(tǒng)評估。最佳萃取條件為:2 mL乙腈;流速0.4 mL/min;50μL四氯化碳;10%離子強(qiáng)度。己烯雌酚和辛基酚的線性關(guān)系良好(R20.9991),LOD在0.09-0.203 ng/mL之間,該方法的加標(biāo)回收率在81.4-105.9%之間,相對標(biāo)準(zhǔn)偏差為1.0-7.6%。所建立的方法已成功應(yīng)用于河水、井水、瓶裝水和校園飲用水的檢測,該方法操作簡單、成本低、分相速度快,對分析物的測定有較好的重現(xiàn)性和高的回收率。第三章:建立了泡騰輔助分散液液微萃取結(jié)合高效液相色譜(HPLC/UV)測定環(huán)境水中的雌激素。該方法以碳酸鈉與磷酸二氫鈉產(chǎn)生的二氧化碳為分散驅(qū)動力,使萃取劑快速均勻地分散在水樣中,實(shí)現(xiàn)整個萃取過程。本實(shí)驗(yàn)考察了泡騰劑的組成及總量、加入泡騰劑的方式、萃取劑種類及體積和水樣的pH對萃取效率的影響,并對該方法進(jìn)行了系統(tǒng)評估。最優(yōu)的萃取條件為:0.35 g的碳酸鈉和磷酸二氫鈉作為泡騰劑置于試管底部,60μL四氯化碳用作萃取劑,水樣的pH對萃取效率無影響。在最佳的萃取條件下,兩種物質(zhì)均呈現(xiàn)良好的線性關(guān)系,線性范圍為5-200 ng/m L,加標(biāo)回收率在81.5-102.8%,相對標(biāo)準(zhǔn)偏差為0.90-4.4%。本文所建立的方法已成功應(yīng)用于海水、井水和飲用水樣品的檢測,在萃取過程中無需使用有機(jī)溶劑作分散劑,整個過程僅需幾十秒鐘即可達(dá)到好的萃取效率。因此,該方法具有操作簡單、快速、低成本、綠色環(huán)保等特點(diǎn)。
[Abstract]:Environmental estrogens, a class of endocrine disruptors, are substances capable of mimicking or disrupting the endocrine function of organisms, which can be enriched in organisms through the food chain or in contact with organisms through environmental exposure (water), Thus affecting the various systems of the organism, destroying the stability of the environment, endangering the health of the organism. Therefore, the monitoring of environmental estrogens in various water bodies is of great significance. In this paper, two new sample pretreatment methods were established to monitor environmental estrogens in water. The whole paper is divided into three chapters. The basic contents are as follows: chapter 1: the methods of sample pretreatment are summarized briefly. The methods of microextraction and environmental estrogens extraction, as well as the background and research contents of this paper are emphasized. Chapter 2: the determination of environmental estrogens in water by countercurrent salting-out homogeneous liquid-liquid extraction dispersible liquid microextraction and high performance liquid chromatography (HPLC-UV) has been established. The effects of extractant type and volume, flow rate, pH of water sample and extractant type and volume and ionic strength of dispersion liquid microextraction method on extraction efficiency were investigated. The method is systematically evaluated. The optimum extraction conditions were as follows: 1: 2 mL acetonitrile, flow rate 0.4 mL / min ~ (-1) 50 渭 L carbon tetrachloride 10% ionic strength. The linear relationship between diethylstilbestrol and octyl phenol was good. The relative standard deviation was 1.0-7.6% and the recoveries of the method were between 81.4-105.9% and 0.09-0.203 ng/mL. The established method has been successfully applied to the detection of river water, well water, bottled water and campus drinking water. The method is simple in operation, low in cost, fast in phase separation, and has good reproducibility and high recovery rate for the determination of analytes. Chapter 3: a method for the determination of estrogens in environmental water by effervescent assisted dispersible liquid microextraction combined with high performance liquid chromatography (HPLC / UV) was established. In this method, the carbon dioxide produced by sodium carbonate and sodium dihydrogen phosphate is used as the driving force, and the extractant is dispersed in the water sample quickly and uniformly, and the whole extraction process is realized. The effects of the composition and total amount of effervescent agent, the way of adding effervescent agent, the type and volume of extractant and the pH of water sample on the extraction efficiency were investigated, and the method was systematically evaluated. The optimal extraction conditions were as follows: sodium carbonate and sodium dihydrogen phosphate were used as effervescent agents at the bottom of the tube and 60 渭 L carbon tetrachloride was placed at the bottom of the test tube as the extractant. The pH of the water sample had no effect on the extraction efficiency. Under the optimum extraction conditions, the linear range was 5-200 ng/m / L, the recovery rate was 81.5-102.8, and the relative standard deviation was 0.90-4.4%. The method established in this paper has been successfully applied to the detection of seawater, well water and drinking water samples. No organic solvent is used as dispersant in the extraction process, and the extraction efficiency can be achieved in only a few tens of seconds. Therefore, the method has the advantages of simple operation, fast operation, low cost and green environmental protection.
【學(xué)位授予單位】：河北大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：X832;O658.2

【參考文獻(xiàn)】

相關(guān)期刊論文 前1條

1 張紅醫(yī);張志軍;王子川;梁玉環(huán);;鹽加速沉降-分散液液微萃取-毛細(xì)管區(qū)帶電泳測定水中芳香胺類化合物[J];分析化學(xué);2013年12期

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本文編號：1913621