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氣泡預(yù)處理技術(shù)的研究及其應(yīng)用

發(fā)布時(shí)間:2018-06-14 20:16

  本文選題:氣泡預(yù)處理技術(shù) + 分離富集。 參考:《東華理工大學(xué)》2017年碩士論文


【摘要】:進(jìn)行痕量待測(cè)物的檢測(cè)時(shí),一般需要對(duì)樣品進(jìn)行預(yù)濃縮(富集)和去除溶質(zhì)干擾(分離)的處理,通常會(huì)經(jīng)過分離,提取,冷凍干燥,重結(jié)晶,超濾等多重預(yù)處理程序[1-4]。因此,發(fā)展一個(gè)更加簡(jiǎn)單、快速、環(huán)保的分離富集方法是非常必要的。本文提出了一種對(duì)水態(tài)復(fù)雜基體樣品快速分離富集的樣品前處理技術(shù)-氣泡預(yù)處理技術(shù)。它可以實(shí)現(xiàn)對(duì)水態(tài)復(fù)雜基體樣品中有機(jī)組分的分離富集,具有操作簡(jiǎn)便、成本廉價(jià)、環(huán)境友好等優(yōu)點(diǎn)。本文研究了氣泡預(yù)處理技術(shù)的工作原理,闡述了其技術(shù)特點(diǎn),探討其與常用分析儀器(質(zhì)譜,色譜,光譜等)的適用性,并將其運(yùn)用于人尿代謝組學(xué)、違禁藥物檢測(cè)、臨床診斷等方面。本文主要研究?jī)?nèi)容包括:1.對(duì)氣泡預(yù)處理技術(shù)的操作方式、參數(shù)設(shè)置、工作原理及特點(diǎn)進(jìn)行研究。2.氣泡預(yù)處理技術(shù)-質(zhì)譜法在復(fù)雜樣品分析中的應(yīng)用。1)建立氣泡預(yù)處理技術(shù)-電噴霧電離質(zhì)譜法對(duì)各類有機(jī)物的分離富集實(shí)驗(yàn),研究17種化合物在一定濃度下的富集倍數(shù)R,R范圍在10~100,而無機(jī)分析物的濃度基本不變;2)建立氣泡預(yù)處理技術(shù)-萃取電噴霧電離質(zhì)譜法對(duì)實(shí)際樣品花露水中揮發(fā)性組分進(jìn)行小體積在線分析,檢測(cè)到揮發(fā)性組分特征信號(hào)4倍增加;3)建立氣泡預(yù)處理技術(shù)-傅里葉變換離子回旋共振質(zhì)譜法對(duì)人尿代謝物的鑒定,通過數(shù)據(jù)庫檢索和串聯(lián)質(zhì)譜分析綜合確定出133個(gè)尿液代謝物;4)對(duì)尿中違禁藥品興奮劑類物質(zhì)的檢測(cè),提高質(zhì)譜對(duì)克倫特羅和沙丁胺醇的檢測(cè)靈敏度;5)通過主成分分析(PCA)方法區(qū)分健康人和腎病病人的尿樣,為腎病患者的提前診斷帶來福音。3.氣泡預(yù)處理技術(shù)-高效液相色譜法對(duì)環(huán)境水樣中土霉素的測(cè)定。土霉素富集倍數(shù)達(dá)到36倍,加標(biāo)回收率分別為97.71%,102.81%,105.26%。能滿足環(huán)境水樣中土霉素的測(cè)定需求。為環(huán)境水樣中抗生素含量測(cè)定提供技術(shù)支持。4.氣泡預(yù)處理技術(shù)-氣相色譜質(zhì)譜聯(lián)用法對(duì)花露水的測(cè)定。有效提高分離富集效果,檢測(cè)到組分信號(hào)強(qiáng)度提高的同時(shí)數(shù)量也增加三倍,為香水領(lǐng)域中的香水鑒別和香水評(píng)價(jià)提供技術(shù)支持。5.氣泡預(yù)處理技術(shù)-熒光光譜法在高濃度鹽下對(duì)奎寧的熒光分析。在有高濃度鹽干擾情況下奎寧的熒光信號(hào)仍然得到10倍增強(qiáng),具有重要的應(yīng)用前景。
[Abstract]:In the detection of trace samples, it is generally necessary to preconcentrate (enrich) and remove solute interference (separation) from the sample, which is usually subjected to multiple pretreatment procedures such as separation, extraction, freeze-drying, recrystallization, ultrafiltration and so on [1-4]. Therefore, it is necessary to develop a simpler, faster and environmentally friendly method of separation and enrichment. In this paper, a sample pretreatment technique, bubble pretreatment, is proposed for rapid separation and enrichment of complex aqueous matrix samples. It can be used to separate and enrich the components in complex aqueous matrix samples. It has the advantages of simple operation, low cost and environmental friendliness. In this paper, the working principle of bubble pretreatment technology is studied, and its technical characteristics are expounded. The applicability of bubble pretreatment technology to common analytical instruments (mass spectrometry, chromatography, spectrum, etc.) is discussed, and it is applied to the detection of human urine metabolomics and illegal drugs. Clinical diagnosis. The main contents of this paper include: 1. The operation mode, parameter setting, working principle and characteristics of bubble pretreatment technology are studied. The Application of Bubble Pretreatment Technology-Mass Spectrometry in complex sample Analysis. The enrichment ratio of 17 compounds at a certain concentration is in the range of 10 ~ 100, while the concentration of inorganic analytes is almost unchanged.) A bubble pretreatment technique, extraction electrospray ionization mass spectrometry, was established for volatile components in dew water of practical samples. Small volume online analysis, It was found that the characteristic signal of volatile components was increased by 4 times. (3) the identification of human urinary metabolites by Fourier transform ion cyclotron resonance mass spectrometry was established. 133 urinary metabolites were identified by database retrieval and tandem mass spectrometry (MS) for the detection of proscribed drugs and stimulant substances in urine. To improve the sensitivity of mass spectrometry for clenbuterol and salbutamol) to distinguish urine samples from healthy subjects and nephrotic patients by principal component analysis (PCA), and to bring evangel.3for the early diagnosis of nephropathy patients. Determination of oxytetracycline in environmental water by high performance liquid chromatography. The enrichment times of oxytetracycline were 36 times and the recoveries were 97.71% and 102.81% respectively. It can meet the requirement of determination of oxytetracycline in environmental water. To provide technical support for the determination of antibiotics in environmental water samples. Determination of Dew Water by Gas Chromatography-Mass Spectrometry with Bubble Pretreatment technique. The separation and enrichment effect was improved effectively, and the signal intensity of components was increased by three times, which provided technical support for perfume identification and perfume evaluation in the field of perfume. Fluorescence analysis of quinine under high salt concentration by bubble pretreatment-fluorescence spectrometry. The fluorescence signal of quinine can still be enhanced 10 times under the condition of high concentration salt interference, so it has an important application prospect.
【學(xué)位授予單位】:東華理工大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:O652

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