本文選題：逆流鹽析均勻液液萃取　切入點：分散液-液微萃取　出處：《河北大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：隨著科學(xué)技術(shù)的發(fā)展,利用分析儀器對樣品的檢測技術(shù)也在不斷發(fā)展和進(jìn)步。而樣品預(yù)處理是樣品進(jìn)行測定過程中的重要步驟之一。傳統(tǒng)的樣品萃取技術(shù)存在操作費時費力、需要使用大量的毒性有機溶劑和樣品等缺點,因此,發(fā)展省時、高效、減少有機溶劑的耗用量的樣品前處理技術(shù)一直是分析化學(xué)研究的熱點領(lǐng)域之一。目前,出現(xiàn)了多種新型預(yù)處理技術(shù),如固相微萃取和液相微萃取,克服了傳統(tǒng)方法中存在的問題。2006年,Assadi等人首次報道了一種新型樣品預(yù)處理技術(shù),即分散液-液微萃取(Dispersive Liquid-Liquid Microextraction,DLLME)。該技術(shù)以其操作簡單、快速、耗費少、富集倍數(shù)高且對環(huán)境友好等優(yōu)點,備受人們關(guān)注和歡迎,廣泛應(yīng)用于痕量分析樣品測定領(lǐng)域。本文建立了3種新型樣品預(yù)處理方法對環(huán)境樣品分析物的測定。全文共包括四章,具體內(nèi)容如下:第一章:緒論。對樣品預(yù)處理方法進(jìn)行了總結(jié)。重點介紹了分散液-液微萃取的研究現(xiàn)狀、應(yīng)用及發(fā)展趨勢,同時闡述了本文的研究背景、選題思想和研究內(nèi)容。第二章:本文提出了一種基于逆流鹽析均勻液液萃取-分散液液微萃取結(jié)合智能手機比色法測定土壤中苯酚含量的方法。該方法中,首先,目標(biāo)分析物經(jīng)過衍生反應(yīng)后,形成橙紅色疏水性化合物,與乙腈和萃取劑1,1,2,2-四氯乙烷混合均勻轉(zhuǎn)移至裝填有NaCl固體小柱的窄管中,利用逆流鹽析液液萃取使乙腈相和水相分離,將目標(biāo)分析物萃取到有機相(包含乙腈和作為下一步分散液液微萃取的萃取劑)中;隨后把上述乙腈相作為第二步分散液-液微萃取中的分散劑,對分析物進(jìn)一步萃取;最后,利用智能手機比色法在一個可折疊自制的拍攝暗箱內(nèi)完成對待測樣品的測定。在優(yōu)化的實驗條件下,苯酚的濃度在9-400μg/L范圍內(nèi)有良好的線性關(guān)系,檢出限(LOD,S/N=3)為2.7μg/L。該方法的加標(biāo)回收率在85%-104%之間,方法操作簡單、消耗少、分相快,并成功用于土壤中苯酚含量的測定。第三章:本文提出了一種基于固體預(yù)分散輔助分散液-液微萃取結(jié)合HPLC-UV分離和富集水中多環(huán)芳烴的方法。該方法中,先將萃取劑加入到適當(dāng)量固體方糖上,此過程萃取劑完成了預(yù)分散,之后將固體加入樣品溶液中,手動搖晃,使固體完全溶解,同時萃取劑分散到水樣中,形成乳濁的溶液。經(jīng)離心,完成對分析物的萃取,經(jīng)氮氣吹干復(fù)溶,最后采用HPLC-UV進(jìn)行分離檢測。此分散法不需要加入毫升級別的有機溶劑,僅憑借易溶、表面多孔的、可食用固體方糖即可完成對萃取劑的分散,該方法對環(huán)境友好、簡便快速、易于操作,并成功用于水樣中多環(huán)芳烴的測定。第四章:建立了一種基于懸浮固化可調(diào)節(jié)萃取劑原位分散液-液微萃取結(jié)合HPLC-UV測定蒽醌類藥物的方法。該方法中以中鏈脂肪酸為萃取劑,將其溶于堿性溶液,之后注入酸性樣品水溶液中調(diào)節(jié)萃取劑在溶液中存在狀態(tài),轉(zhuǎn)換為疏水形式,完成對目標(biāo)分析物的萃取過程。該方法是一種快速、簡單、對環(huán)境友好的樣品預(yù)處理技術(shù)。本實驗考察了質(zhì)子酸類型和用量、萃取劑用量、離子強度、離心時間對萃取效率的影響,并對該方法進(jìn)行了系統(tǒng)評估。在優(yōu)化的實驗條件下,兩種蒽醌類化合物在5-400 ng/mL濃度范圍內(nèi)有良好的線性關(guān)系,其相關(guān)系數(shù)均大于0.999,對實際樣品進(jìn)行了加標(biāo)回收率實驗,回收率在82%-110%范圍內(nèi),準(zhǔn)確度和精密度均得到了滿意的結(jié)果。該萃取過程中并未使用有機分散溶劑,萃取時間短、操作簡單、成本低、綠色環(huán)保。因此,該新型分散液-液微萃取在樣品預(yù)處理中具有巨大潛質(zhì)。
[Abstract]:With the development of science and technology, the use of analytical instruments on the sample detection technology is also in constant development and progress. The sample pretreatment is one of the most important steps in the process of determination of the samples. The existence of the traditional sample extraction technique is time-consuming, requires the use of large amounts of toxic organic solvents and samples and other shortcomings, therefore, the development of time, high efficiency, reduce consumption of samples of organic solvent pretreatment technology has been one of the hot spots in the field of analytical chemistry research. At present, there are many new pretreatment technology, such as solid phase microextraction and liquid phase microextraction, to overcome the existing problems in the traditional method of.2006, Assadi et al reported for the first time a new sample processing technology, namely dispersive liquid-liquid microextraction (Dispersive Liquid-Liquid, Microextraction, DLLME). The operation is simple, rapid, less cost, high number of times and enrichment of environmental protection Good attention and welcome, widely used in trace analysis determination of field samples. This paper established 3 new sample pretreatment methods for determination of analytes in environmental samples. The thesis consists of four chapters, the specific contents are as follows: the first chapter: introduction. The sample pretreatment methods are summarized. The key is introduced the research status of DLLME, application and development trend, and expounds the research background of this paper, research ideas and research content. The second chapter: This paper presents a method based on uniform salting out countercurrent liquid-liquid extraction and dispersive liquid liquid for determination of phenol in soil colorimetric micro extraction combined with intelligent mobile phone. In this method, firstly, analysis after derivatization reaction after the goal, the formation of orange red hydrophobic compounds, and acetonitrile and extraction agent 1,1,2,2- four chlorine ethane mixed evenly transferred to the narrow tube filled with solid column in NaCl, Salting out by countercurrent liquid-liquid extraction to acetonitrile and aqueous phase separation, the target analytes extracted into organic phase (extractant containing acetonitrile and as the next step of dispersed liquid-liquid microextraction); then the acetonitrile phase as the second step of DLLME in dispersing agent for further analyte extraction; finally, the use of intelligent mobile phone colorimetry in a folding homemade shooting box determination completed within the sample to be measured. Under the optimized experimental conditions, the phenol concentration has a good linear relationship in the range of 9-400 g/L, the detection limit (LOD, S/N=3) and the recovery is 2.7 ~ g/L. of the method the rate between 85%-104% method has advantages of simple operation, less consumption, fast phase, and was successfully used to determine the content of phenol in soil. The third chapter: This paper proposes a method based on solid dispersion assisted dispersive liquid-liquid microextraction combined with HPLC-UV separation and enrichment of PAHs in water Aromatics method. In this method, the extraction agent is added to the appropriate amount of solid sugar, the extractant completed pre dispersion after the solid is added to the sample solution, manual shaking, the solid is completely dissolved, at the same time solvent dispersed into water. The solution to form emulsion. After centrifugation, complete the extraction of the analyte, dried by nitrogen and dissolved, and finally HPLC-UV was separated and detected. The organic solvent dispersion method doesn't need to add the ml level, only by virtue of soluble, porous surface, solid dispersion can be completed on the edible sugar extraction agent, this method is simple and rapid, environmentally friendly, easy to operate, and for the determination of polycyclic aromatic hydrocarbons in water samples. The fourth chapter: the establishment of a suspension based on curing adjustable extractant in situ dispersive liquid-liquid microextraction combined with HPLC-UV method for the determination of anthraquinone drugs. This method in medium chain fatty acid for extraction The agent, which is dissolved in the alkaline solution after injection, extraction agent regulating state in the solution of acid water solution samples, converted to hydrophobic form of target analyte extraction process. This method is a rapid, simple, the sample pretreatment technology of friendly environment. The effects of acid type and the amount of proton, amount of solvent, ionic strength, the influence of centrifugal time on extraction efficiency, and the method of the evaluation system. Under the optimized experimental conditions, two kinds of anthraquinone compounds have a good linear relationship in the concentration range of 5-400 ng/mL, the correlation coefficient is greater than 0.999, the actual samples the recovery test, the recovery rate is in the range of 82%-110%, the accuracy and precision of the results are satisfactory. The extraction process does not use organic solvent dispersion, short extraction time, simple operation, low cost, green environmental protection Therefore, the new dispersing liquid liquid microextraction has great potential in the sample pretreatment.

【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

【參考文獻(xiàn)】

相關(guān)期刊論文 前2條

1 李明杰;張紅醫(yī);劉曉哲;崔春艷;石志紅;;分散液-液微萃取萃取劑分散策略的新進(jìn)展[J];分析化學(xué);2015年08期

2 楊傳孝;孫向英;劉斌;連惠婷;;數(shù)碼成像比色法測定水樣中的總磷[J];分析化學(xué);2007年06期

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本文編號：1608891