本文選題：HPLC-UV　切入點(diǎn)：磁性材料　出處：《河北大學(xué)》2017年碩士論文

【摘要】：中藥作為預(yù)防和治療疾病的寶貴資源,有著上千年的歷史。近年來(lái),為了深入了解中藥的功效和作用機(jī)理,越來(lái)越多的人開(kāi)始對(duì)中藥的活性成分進(jìn)行研究。黃連是一種非常重要的中藥植物,含有多種生物堿,如藥根堿、小檗堿、黃連堿和巴馬汀。這些活性成分具有抗病毒、消炎、抗菌、清熱祛濕、解毒的功效,在中藥復(fù)方中通過(guò)協(xié)同效應(yīng)來(lái)發(fā)揮黃連的多種藥理作用。這幾種主要的生物堿常用于含黃連中藥制劑的質(zhì)量評(píng)價(jià)和藥代動(dòng)力學(xué)研究。本文構(gòu)建了兩種金屬氧化物吸附膠束分散固相萃取體系,用于葛根芩連口服液和人體尿液中幾種生物堿的檢測(cè)。全文共分3章,主要內(nèi)容如下:第1章:介紹了幾種生物堿的作用及研究?jī)r(jià)值;概述了膠束在樣品預(yù)處理應(yīng)用中的研究進(jìn)展,重點(diǎn)討論了濁點(diǎn)萃取、膠束固相萃取和磁性膠束分散固相萃取。最后闡述了本文的研究背景和研究?jī)?nèi)容。第2章:利用十二烷基磺酸鈉(SDS)包覆的Fe_3O_4納米粒子吸附膠束分散固相萃取結(jié)合HPLC-UV分離和富集葛根芩連口服液中的小檗堿、黃連堿和巴馬汀。本文通過(guò)共沉淀法合成了Fe_3O_4納米粒子,通過(guò)透射電子顯微鏡對(duì)其進(jìn)行表征。在酸性條件下,用SDS包覆在Fe_3O_4表面對(duì)其進(jìn)行改性,從而形成表面包覆SDS的磁性吸附劑。一定的pH值下,帶正電荷的生物堿會(huì)通過(guò)靜電作用吸附在帶相反電荷的磁性吸附劑上。在外加磁場(chǎng)作用下,磁性吸附劑與樣品溶液迅速分離。本實(shí)驗(yàn)考察了Fe_3O_4用量、溶液pH、SDS用量、洗脫劑類型以及萃取時(shí)間對(duì)萃取效率的影響。在優(yōu)化條件下,三種目標(biāo)分析物的回收率為87.9%-108.1%,相對(duì)標(biāo)準(zhǔn)偏差均低于3.8%。在該方法中,磁性納米粒子具有超順磁性,在外加磁場(chǎng)作用下可迅速與樣品溶液分離,省去了傳統(tǒng)SPE淋洗、洗脫和一般分散固相萃取離心等繁瑣的分離操作步驟,顯著地縮短了樣品預(yù)處理時(shí)間。形成的吸附膠束表面負(fù)電荷密度大,對(duì)帶正電荷的生物堿的選擇性好,萃取效率高。該方法將磁性納米粒子與吸附膠束的優(yōu)點(diǎn)相結(jié)合,環(huán)境友好、簡(jiǎn)便快速、易于操作,適用于葛根芩連口服液中三種生物堿的測(cè)定。第3章:采用金屬氧化物Al_2O_3與十二烷基磺酸鈉(SDS)形成吸附膠束作為分散固相微萃取(DMSPE)的吸附劑。在酸性條件下,用SDS對(duì)Al_2O_3表面進(jìn)行改性形成吸附膠束。在玻璃針管中對(duì)服用葛根芩連口服液后人體尿液中的藥根堿、小檗堿、黃連堿和巴馬汀進(jìn)行萃取,通過(guò)高壓抽濾,吸附膠束與尿液分離,富集在針頭式過(guò)濾器上,甲醇洗脫后氮?dú)獯蹈蓮?fù)溶,最后采用HPLC-UV進(jìn)行檢測(cè)。本文對(duì)影響Al_2O_3-SDS膠束形成和影響萃取效率的因素包括Al_2O_3的用量、SDS的用量、溶液pH、洗脫條件、萃取時(shí)間和尿樣稀釋倍數(shù)進(jìn)行了優(yōu)化。在最佳條件下,對(duì)人體尿液中的四種異喹啉類生物堿進(jìn)行了分析。結(jié)果表明,藥根堿、黃連堿、巴馬汀和小檗堿均具有良好的線性關(guān)系,R2均大于0.999�；厥章蕿�86.1%-99.2%,相對(duì)標(biāo)準(zhǔn)偏差均低于4.4%。本文首次將Al_2O_3-SDS吸附膠束分散固相微萃取應(yīng)用于人體尿液中四種異喹啉類生物堿的檢測(cè)。本文所建立的方法具有裝置簡(jiǎn)單、操作方便、環(huán)境友好、價(jià)格低廉等優(yōu)點(diǎn)。
[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.

【學(xué)位授予單位】：河北大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：R286.0;R446.12;O657.72

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