本文選題：可調(diào)式溶劑分散液—液微萃取　切入點：福美雙　出處：《河北大學(xué)》2017年碩士論文

【摘要】：分散液—液微萃取技術(shù)以優(yōu)異的綠色化學(xué)指標和數(shù)百倍的富集倍數(shù)等優(yōu)良性能而備受青睞。它是由萃取劑、分散劑和水溶液組成的三元萃取體系。本文將從萃取劑的視角對分散液—液微萃取技術(shù)進行新的詮釋,建立了以可調(diào)式溶劑為萃取劑的分散液—液微萃取技術(shù)的新型預(yù)處理結(jié)合快速測定和分離技術(shù)用于水樣、尿樣以及油樣品中有害物質(zhì)的檢測。本文共分為4章,具體內(nèi)容如下:第1章:簡述分散液—液微萃取的概念、分散液—液微萃取中萃取劑的分類以及本文的研究目的、內(nèi)容及意義。第2章:本實驗首次將一種可調(diào)式溶劑分散液—液微萃方法與智能手機三原色法聯(lián)用測定水樣中的福美雙。顯色反應(yīng)為福美雙在堿性條件下與Cu~(2+)絡(luò)合生成黃色的疏水性螯合物。間氯苯胺作為堿性萃取劑,可溶于酸,之后通過加入堿調(diào)節(jié)溶液的pH值使疏水性的有色分析物萃取到不溶于堿溶液的有機相,整個過程不需要分散劑,幾秒內(nèi)便可完成萃取。智能手機測定過程是在一個可折疊的自制暗箱內(nèi)完成,操作簡便,經(jīng)濟快速。在最佳條件下福美雙的濃度在0.08μg/mL-1.5μg/mL范圍內(nèi)有很好的線性關(guān)系,檢出限(LOD,S/N=3)為0.023μg/mL。該方法已應(yīng)用于實際水樣分析,加標回收率在80%-119%之間。該方法成本低廉、測量方便,為野外水體中福美雙的現(xiàn)場測定提供了可能性。第3章:為了探究可調(diào)式溶劑分散液—液微萃取與毛細管電泳技術(shù)聯(lián)用的適用性,本文提出了以酸堿反應(yīng)為基礎(chǔ)的分散液—液微萃取結(jié)合瞬時等速電泳測定尿樣中的四種苯胺類化合物。該方法中以堿性溶劑間氯苯胺為萃取劑,將其溶于酸性去離子水中,之后注入堿性樣品水溶液中,酸堿反應(yīng)發(fā)生,萃取劑去質(zhì)子化形成不溶于水的小液滴萃取分析物。離心后,取出萃取劑將其溶于1:1的甲醇/緩沖溶液形成的背景電解質(zhì)中,此溶液為均相溶液,可直接大體積進毛細管電泳。在最佳的優(yōu)化條件下,提出的萃取技術(shù)得到了較好的分析性能,4種苯胺類的標準曲線分別在0.005μg/mL—1.5μg/mL、0.02μg/mL—8μg/m L、0.02μg/m L—8μg/m L、0.04μg/m L—8μg/m L范圍內(nèi)有良好的線性關(guān)系,其相關(guān)系數(shù)均大于0.999;檢出限范圍為0.97—3.22 ng/m L;日內(nèi)精密度RSD%2.16(n=6),日間精密度RSD%2.40(n=4);富集倍數(shù)為28-127。本實驗很好的解決了疏水性萃取劑與BGE溶液的兼容性問題,成功測定了實際尿樣中的苯胺類化合物,為測定ng/m L級別的苯胺類化合物提供了一種非常有潛力的手段。第4章:為了進一步擴展可調(diào)式溶劑分散液—液微萃取技術(shù)在毛細管電泳大體積直接進樣方案的發(fā)展,本研究提出了一種新型的“綠色”溶劑低共熔劑(Deep eutectic solvents,DESs)為正相萃取技術(shù),可調(diào)式溶劑分散液—液微萃取為反相萃取技術(shù),兩步萃取加熱過的植物油中的苯胺類化合物。正相萃取階段,利用氯化膽堿與乙二醇合成的親水性的DESs從實際油樣中萃取極性分析物;反相萃取階段,利用上述低共熔劑的可溶性,將富含目標分析物的DESs相釋放到一定量的堿性去離子水中,再將溶于酸的苯胺類萃取劑打入其中,形成乳濁液,萃取后,將目標分析物萃取到有機相,將有機相取出后溶于背景電解質(zhì)中,直接進毛細管電泳。在最佳的優(yōu)化條件下,兩步萃取技術(shù)得到了較好的分析性能,相關(guān)系數(shù)R20.999,兩種分析物的線性范圍分別為0.0025μg/m L—1.0μg/mL和0.01μg/m L—6μg/mL,檢出限0.97—3.22 ng/m L和重現(xiàn)性RSD%2.49,n=3。上述提到的萃取技術(shù)具有很好的靈敏度和穩(wěn)定性,為油樣中ng/mL級別的極性化合物的測定打開了新思路。
[Abstract]:The dispersion of liquid liquid micro extraction technology with excellent performance and excellent index of green chemistry and the enrichment of hundreds of times. It is favored by the extractant, three element extraction system of dispersant and water solution composition. This paper from the perspective of extractant dispersion - liquid micro extraction technology for the new interpretation a, extraction agent dispersed liquid-liquid microextraction with adjustable solvent for the new pretreatment combined with rapid determination and separation technology for the detection of urine samples, and harmful substances in the oil samples. This paper is divided into 4 chapters, the specific contents are as follows: the first chapter: introduces the concept of dispersion liquid-liquid microextraction the classification, dispersed extractant liquid-liquid microextraction in and the purpose, content and significance. The second chapter: the experiment for the first time a dispersive liquid-liquid micro extraction method and intelligent mobile phone three method combined with the determination of adjustable solvent Thiram. Color reaction for Thiram in alkaline conditions with Cu~ (2+) complex formation of hydrophobic chelate yellow. M-chloroaniline as alkaline extraction agent, acid soluble, after adding alkali by adjusting the pH value of the solution to the analyte extraction colored hydrophobic to alkali insoluble organic solution the phase, the whole process does not need dispersant, a few seconds can be completed. The extraction process is completed by the intelligent mobile phone, in a folding homemade dark box has the advantages of simple operation, rapid economic. Thiram under optimal conditions have a good linear relationship in the range of 0.08 g/mL-1.5 g/mL, the detection limit (LOD 0.023 g/mL., S/N=3) the method has been applied to the actual analysis of water samples, the recoveries were 80%-119%. The method has the advantages of low cost, convenient measurement, provides the possibility for the determination of thiram field water. The third chapter: in order to explore the adjustable solution Dispersant applicability of liquid-liquid microextraction with capillary electrophoresis coupled with the proposed determination of four aniline compounds in urine by acid-base reaction based dispersive liquid-liquid microextraction combined with transient isotachophoresis. Chloroaniline with alkaline solvent between the method for extracting agent, which is soluble in acidic deionized water, after injection of alkaline samples in aqueous solution, acid-base reaction, extraction agent to form small droplets of extraction of protonated water insoluble analyte. After centrifugation, remove the extractant dissolved in methanol / 1:1 buffer solution formed in the background electrolyte, the solution for the homogeneous solution, can be directly large volume injection by capillary electrophoresis. In the optimal condition, the extraction technology was analyzed with good performance, 4 kinds of aniline standard curve respectively in 0.005 g/mL, 1.5 g/mL, 0.02 g/mL, 8 g/m L, 0.02 g/m L 8 g/m L 0.04, g/m L 8 g/m L range has a good linear relationship, the correlation coefficient is greater than 0.999; the detection limit range of 0.97 - 3.22 ng/m L; the within day precision RSD%2.16 (n=6), inter day precision RSD%2.40 (n=4); enrichment factor is 28-127. in this experiment is a good solution to the compatibility the problem with agent BGE solution hydrophobic extraction, successful aniline compounds in urine were determined by the actual, provides a promising method for the determination of aniline compounds ng/m L level. The fourth chapter: in order to further expand the development of adjustable solvent dispersion liquid-liquid microextraction capillary electrophoresis in large volume the sample program, this study proposes a new "green" solvent of low total flux (Deep eutectic solvents, DESs) for normal phase extraction technology, adjustable solvent dispersion liquid-liquid microextraction for reversed phase extraction technology, the two step extraction heating plant Aniline compounds in oil. Positive phase extraction stage, using choline chloride and ethylene glycol synthesis of hydrophilic DESs from the actual oil extraction of polar analytes; reversed phase extraction stage, the low total soluble flux, rich target analyte DESs release to a certain amount of alkaline deionized water. The soluble aniline extraction agent acid into the emulsion formation, after extraction, the target analyte extraction into the organic phase, the organic phase after removing the dissolved in the background electrolyte, directly into the capillary electrophoresis. In the optimal condition, the two step extraction technology has been of good performance, correlation coefficient R20.999, the linear range of two analytes were 0.0025 g/m L 1 g/mL and 0.01 g/m L - 6 g/mL, the detection limit is 0.97 - 3.22 ng/m L and RSD%2.49 n=3. reproducibility, extraction technology mentioned above has good sensitivity And the stability is a new idea for the determination of ng/mL level polar compounds in oil samples.

【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】：O658.2

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相關(guān)期刊論文 前1條

1 ;Orthogonal array optimization of ionic liquid based dispersive liquid-liquid microextraction for toxic anilines in foods[J];Science China(Chemistry);2012年02期

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本文編號：1727496