气泡预处理技术的研究及其应用

发布时间：2018-06-14 20:16

本文选题：气泡预处理技术 + 分离富集　；参考：《东华理工大学》2017年硕士论文

【摘要】：进行痕量待测物的检测时,一般需要对样品进行预浓缩(富集)和去除溶质干扰(分离)的处理,通常会经过分离,提取,冷冻干燥,重结晶,超滤等多重预处理程序[1-4]。因此,发展一个更加简单、快速、环保的分离富集方法是非常必要的。本文提出了一种对水态复杂基体样品快速分离富集的样品前处理技术-气泡预处理技术。它可以实现对水态复杂基体样品中有机组分的分离富集,具有操作简便、成本廉价、环境友好等优点。本文研究了气泡预处理技术的工作原理,阐述了其技术特点,探讨其与常用分析仪器(质谱,色谱,光谱等)的适用性,并将其运用于人尿代谢组学、违禁药物检测、临床诊断等方面。本文主要研究内容包括:1.对气泡预处理技术的操作方式、参数设置、工作原理及特点进行研究。2.气泡预处理技术-质谱法在复杂样品分析中的应用。1)建立气泡预处理技术-电喷雾电离质谱法对各类有机物的分离富集实验,研究17种化合物在一定浓度下的富集倍数R,R范围在10~100,而无机分析物的浓度基本不变;2)建立气泡预处理技术-萃取电喷雾电离质谱法对实际样品花露水中挥发性组分进行小体积在线分析,检测到挥发性组分特征信号4倍增加;3)建立气泡预处理技术-傅里叶变换离子回旋共振质谱法对人尿代谢物的鉴定,通过数据库检索和串联质谱分析综合确定出133个尿液代谢物;4)对尿中违禁药品兴奋剂类物质的检测,提高质谱对克伦特罗和沙丁胺醇的检测灵敏度;5)通过主成分分析(PCA)方法区分健康人和肾病病人的尿样,为肾病患者的提前诊断带来福音。3.气泡预处理技术-高效液相色谱法对环境水样中土霉素的测定。土霉素富集倍数达到36倍,加标回收率分别为97.71%,102.81%,105.26%。能满足环境水样中土霉素的测定需求。为环境水样中抗生素含量测定提供技术支持。4.气泡预处理技术-气相色谱质谱联用法对花露水的测定。有效提高分离富集效果,检测到组分信号强度提高的同时数量也增加三倍,为香水领域中的香水鉴别和香水评价提供技术支持。5.气泡预处理技术-荧光光谱法在高浓度盐下对奎宁的荧光分析。在有高浓度盐干扰情况下奎宁的荧光信号仍然得到10倍增强,具有重要的应用前景。
[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.
【学位授予单位】：东华理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O652

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