吸附胶束分散固相萃

发布时间：2018-03-27 14:09

本文选题：HPLC-UV　切入点：磁性材料　出处：《河北大学》2017年硕士论文

【摘要】：中药作为预防和治疗疾病的宝贵资源,有着上千年的历史。近年来,为了深入了解中药的功效和作用机理,越来越多的人开始对中药的活性成分进行研究。黄连是一种非常重要的中药植物,含有多种生物碱,如药根碱、小檗碱、黄连碱和巴马汀。这些活性成分具有抗病毒、消炎、抗菌、清热祛湿、解毒的功效,在中药复方中通过协同效应来发挥黄连的多种药理作用。这几种主要的生物碱常用于含黄连中药制剂的质量评价和药代动力学研究。本文构建了两种金属氧化物吸附胶束分散固相萃取体系,用于葛根芩连口服液和人体尿液中几种生物碱的检测。全文共分3章,主要内容如下:第1章:介绍了几种生物碱的作用及研究价值;概述了胶束在样品预处理应用中的研究进展,重点讨论了浊点萃取、胶束固相萃取和磁性胶束分散固相萃取。最后阐述了本文的研究背景和研究内容。第2章:利用十二烷基磺酸钠(SDS)包覆的Fe_3O_4纳米粒子吸附胶束分散固相萃取结合HPLC-UV分离和富集葛根芩连口服液中的小檗碱、黄连碱和巴马汀。本文通过共沉淀法合成了Fe_3O_4纳米粒子,通过透射电子显微镜对其进行表征。在酸性条件下,用SDS包覆在Fe_3O_4表面对其进行改性,从而形成表面包覆SDS的磁性吸附剂。一定的pH值下,带正电荷的生物碱会通过静电作用吸附在带相反电荷的磁性吸附剂上。在外加磁场作用下,磁性吸附剂与样品溶液迅速分离。本实验考察了Fe_3O_4用量、溶液pH、SDS用量、洗脱剂类型以及萃取时间对萃取效率的影响。在优化条件下,三种目标分析物的回收率为87.9%-108.1%,相对标准偏差均低于3.8%。在该方法中,磁性纳米粒子具有超顺磁性,在外加磁场作用下可迅速与样品溶液分离,省去了传统SPE淋洗、洗脱和一般分散固相萃取离心等繁琐的分离操作步骤,显著地缩短了样品预处理时间。形成的吸附胶束表面负电荷密度大,对带正电荷的生物碱的选择性好,萃取效率高。该方法将磁性纳米粒子与吸附胶束的优点相结合,环境友好、简便快速、易于操作,适用于葛根芩连口服液中三种生物碱的测定。第3章:采用金属氧化物Al_2O_3与十二烷基磺酸钠(SDS)形成吸附胶束作为分散固相微萃取(DMSPE)的吸附剂。在酸性条件下,用SDS对Al_2O_3表面进行改性形成吸附胶束。在玻璃针管中对服用葛根芩连口服液后人体尿液中的药根碱、小檗碱、黄连碱和巴马汀进行萃取,通过高压抽滤,吸附胶束与尿液分离,富集在针头式过滤器上,甲醇洗脱后氮气吹干复溶,最后采用HPLC-UV进行检测。本文对影响Al_2O_3-SDS胶束形成和影响萃取效率的因素包括Al_2O_3的用量、SDS的用量、溶液pH、洗脱条件、萃取时间和尿样稀释倍数进行了优化。在最佳条件下,对人体尿液中的四种异喹啉类生物碱进行了分析。结果表明,药根碱、黄连碱、巴马汀和小檗碱均具有良好的线性关系,R2均大于0.999。回收率为86.1%-99.2%,相对标准偏差均低于4.4%。本文首次将Al_2O_3-SDS吸附胶束分散固相微萃取应用于人体尿液中四种异喹啉类生物碱的检测。本文所建立的方法具有装置简单、操作方便、环境友好、价格低廉等优点。
[Abstract]:Chinese medicine as a valuable resource for the prevention and treatment of disease, has a history of thousands of years. In recent years, in order to understand the efficacy and mechanism of action of Chinese medicine, more and more people began to active ingredients of Chinese medicine research. Chinese medicinal plant Coptis chinensis is a kind of very important, contains many kinds of alkaloids, such as jatrorrhizine. Berberine, Huang Lianjian and Pakistan Martin. The active ingredients have antiviral, anti-inflammatory, antibacterial, dampness, detoxification, through the synergistic effect to play a variety of pharmacological effects of Rhizoma Coptidis in traditional Chinese medicine prescription. The several main alkaloids used to study quality evaluation of Chinese herbal medicine containing Coptis and pharmacokinetics. This paper constructs two the adsorption of metal oxide micelle dispersive solid phase extraction system for Gegen Qinlian oral liquid and several alkaloids in human urine detection. This thesis consists of 3 chapters, the main contents are as follows: the first chapter introduces: Function and research value of several alkaloids; summarizes the research progress of micelles in the pretreatment of the sample application, discussed the cloud point extraction, solid phase extraction and micellar magnetic micelles with dispersive solid phase extraction. Finally, the author introduces research background and research content. The second chapter: the use of twelve sodium dodecyl sulfate (SDS) micelles coated Fe_3O_4 nanoparticles adsorption the combination of berberine HPLC-UV dispersive solid phase extraction separation and enrichment of Gegen Qinlian oral liquid, Huang Lianjian and Martin. The Pakistan Fe_3O_4 nanoparticles were synthesized by co precipitation method, and characterized by transmission electron microscopy. In acidic conditions, on the surface of Fe_3O_4 modified by coating SDS, thus forming a magnetic surface SDS coated with adsorbent. A certain pH value, alkaloids with positive charge through electrostatic interaction in the magnetic adsorbent with opposite charge. Magnetic outside Field, magnetic adsorbent rapid separation and sample solution. The effects of Fe_3O_4 dosage, SDS dosage, solution pH, eluent type and the effect of extraction time on extraction efficiency. Under the optimized conditions, three kinds of target analyte recovery rate was 87.9%-108.1%, the relative standard deviations were less than 3.8%. in the method in the magnetic nanoparticles are superparamagnetic, under the applied magnetic field can be quickly separated from the sample solution, eliminating the traditional SPE eluent, elution and dispersive solid phase extraction centrifugal separation operation is complicated, significantly shorten the sample pretreatment time. The formation of micelle adsorption surface negative charge density, selectivity of the alkaloids with the positive charge of good, high extraction efficiency. The advantages of magnetic nanoparticles and adsorption of micelles combination, environment friendly, simple and rapid, easy to operate, suitable for Pueraria Qinlian oral liquid Determination of three alkaloids. The third chapter: using metal oxide Al_2O_3 and twelve sodium dodecyl sulfate (SDS) micelles formed adsorption as the dispersed solid phase microextraction (DMSPE) adsorbent. In acidic conditions, modified to form micelles adsorbed on the surface of Al_2O_3 by SDS. The glass needle in the use of jatrorrhizine, puerarin Qinlian oral liquid in human urine by berberine, Huang Lianjian and Bamatin through high pressure extraction, filtration, adsorption and separation of micelles and urine, enriched in syringe filters, methanol elution after drying with nitrogen dissolved, finally were detected by HPLC-UV. The influence on the extraction efficiency influence factors of Al_2O_3-SDS micelle formation and include the amount of Al_2O_3 SDS, dosage, solution pH, elution conditions, extraction time and urine dilution were optimized. Under the optimal conditions, four kinds of isoquinoline alkaloids in human urine were analyzed. Analysis. The results showed that jatrorrhizine, berberine and Martin Huang Lianjian, Pakistan has a good linear relationship, R2 was greater than 0.999. recovery rate was 86.1%-99.2%, the relative standard deviations were less than 4.4%. for the first time the detection of Al_2O_3-SDS micelles adsorbed dispersive solid-phase microextraction was applied to four kinds of isoquinoline alkaloids in human urine by this method. The device is simple, convenient, environmentally friendly, and low price.

【学位授予单位】：河北大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：R286.0;R446.12;O657.72

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