發(fā)布時(shí)間：2018-04-23 22:33

  本文選題：毛細(xì)管電泳 + 在線雙富集方法��； 參考：《南方醫(yī)科大學(xué)》2017年碩士論文

【摘要】：目前,由藥物殘留和藥物濫用造成的社會危害越來越明顯,因此對微量藥物組分殘留量的檢測引起了廣泛重視。而傳統(tǒng)方法在藥物檢測的過程中都會遇到被測組分濃度低、基質(zhì)復(fù)雜、存在大量干擾物等問題,因此為了對微量超微量組分準(zhǔn)確分析定量,迫切需要建立簡單快速、靈敏的方法。毛細(xì)管電泳技術(shù)是目前分離學(xué)科中最活躍的方法之一,具有操作簡單、高效、高速、樣品預(yù)處理簡單、樣品需要量小等特點(diǎn)。但因毛細(xì)管內(nèi)徑小,檢測窗口光程短,而導(dǎo)致的靈敏度小,成為其檢測復(fù)雜基質(zhì)中痕量物質(zhì)最大的限制。可通過改造儀器以提高其靈敏度,例如更換不同的檢測器,但價(jià)格昂貴,進(jìn)一步發(fā)展的潛力較小。所以,目前靈敏度問題主要通過樣品在線富集方法來解決。在線富集是指通過改變體系的條件,使毛細(xì)管內(nèi)樣品區(qū)帶壓縮,從而使樣品濃度變大,靈敏度增強(qiáng)的一種方法。每種在線富集方法都有一定的適用范圍和前提條件,為了進(jìn)一步降低檢測限,針對分析分析物的物理化學(xué)性質(zhì)及基質(zhì)的復(fù)雜性,通常需要幾種在線富集方法的聯(lián)用。因此,毛細(xì)管電泳在線富集聯(lián)用方法的發(fā)展成為分析工作者研究的重點(diǎn)。本論文在前人工作的基礎(chǔ)上,對毛細(xì)管在線富集方法在藥物殘留中的應(yīng)用進(jìn)行了研究,主要開展了如下創(chuàng)新性的工作:1.將有機(jī)溶劑膠束堆積和場放大樣品堆積富集技術(shù)聯(lián)用,建立了磺胺甲惡唑和甲氧芐啶的分離富集體系。甲氧芐啶和磺胺甲惡唑具有疏水性,在樣品基質(zhì)中加入十二烷基磺酸鈉可形成膠束。引入樣品后再引入一段有機(jī)溶劑,膠束在有機(jī)溶劑的誘導(dǎo)下更易于解聚,完成有機(jī)溶劑膠束富集。利用磺胺甲惡唑和甲氧芐啶在酸性溶液中的電荷性質(zhì)使其在有機(jī)溶劑低電導(dǎo)率區(qū)和緩沖溶液高電導(dǎo)率區(qū)帶邊界完成場強(qiáng)放大樣品堆積。建立了生物樣品中甲氧芐啶和磺胺甲惡唑的殘留檢測新方法,并實(shí)際應(yīng)用于6種動物源性食品(純牛奶、高鈣奶、純羊奶、奶粉、蜂蜜、雞蛋)。2.建立了 β-CD輔助在線毛細(xì)管雙富集體系,在毛細(xì)管電泳中先后實(shí)現(xiàn)了場放大樣品堆積和有機(jī)溶劑膠束解聚兩步富集,并以興奮劑阿替洛爾和美托洛爾為模型驗(yàn)證了方法的可行性。在樣品基質(zhì)中加入少量的β-CD,可降低十二烷基磺酸鈉膠束的表面活性,從而降低膠束的臨界膠束濃度(CMC),更有利于膠束解聚。該方法簡單、快速、重現(xiàn)性好,并已應(yīng)用于人尿液中阿替洛爾和美托洛爾的殘留檢測。
[Abstract]:At present, the social harm caused by drug residue and drug abuse is becoming more and more obvious. Therefore, the detection of trace residues in microdrugs has attracted wide attention. The traditional methods will meet the problems of low concentration, complex matrix and large number of dry disturbances in the process of drug testing. It is urgent to establish a simple, rapid and sensitive method for accurate analysis and quantitative analysis. Capillary electrophoresis (CE) is one of the most active methods in the field of separation. It has the characteristics of simple operation, high efficiency, high speed, simple sample preprocessing and small sample requirement. However, the sensitivity of the detection window is small because of small capillary diameter, and the sensitivity is small. It can detect the greatest limit of trace substance in complex matrix. It can improve its sensitivity by changing the instrument, such as the replacement of different detectors, but the price is expensive and the potential for further development is small. So, the problem of sensitivity is mainly solved by the method of sample on-line enrichment. The sample area in the tube is compressed, which makes the sample concentration larger and the sensitivity enhanced. Each on-line enrichment method has a certain range of application and precondition. In order to further reduce the detection limit, several on-line enrichment methods are usually needed to analyze the physical and chemical properties of the analyte and the complexity of the matrix. On the basis of predecessors' work, this paper studies the application of capillary on-line enrichment in drug residue. The main work is as follows: 1. the accumulation of organic solvent micelles and accumulation of field magnification samples are carried out. The separation and enrichment system of sulfamethoxazole and trimethoprim was established by technology. The hydrophobicity of trimethoprim and sulfamethoxazole was hydrophobic, and the sodium alkyl sulfonate was added to the sample matrix to form micelles. The sample was introduced into an organic solvent and the micelles were more easily depolymerization under the induction of organic solvents and completed the organic solvent micelles. Enrichment. Using the charge properties of sulfamethoxazole and trimethoprim in the acidic solution to complete the accumulation of field strength samples in the low conductivity area of organic solvents and the high conductivity zone of the buffer solution, a new method for the detection of trimethoprim and sulfamethoxazole in biological samples was established and applied to the 6 species of animal origin food. The product (pure milk, high calcium milk, pure goat milk, milk powder, honey, egg).2. has established a beta -CD assisted on-line capillary double rich group. In capillary electrophoresis, the accumulation of field amplification samples and the two steps of organic solvent micelle depolymerization have been realized, and the feasibility of the method is verified by the model of atenolol and metoprolol. The addition of a small amount of beta -CD can reduce the surface activity of the sodium alkyl sulfonate micelle and reduce the critical micelle concentration (CMC) of the micelles, which is more conducive to the depolymerization of the micelles. This method is simple, rapid and reproducible, and has been applied to the determination of atenolol and metoprolol in human urine.

【學(xué)位授予單位】：南方醫(yī)科大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O658.9;R927

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