本文選題：開管毛細(xì)管電色譜　切入點(diǎn)：多巴胺　出處：《蘭州大學(xué)》2017年碩士論文

【摘要】：手性是自然界的本質(zhì)屬性之一,手性化合物的分離一直是分離領(lǐng)域的一個(gè)研究熱點(diǎn)和難點(diǎn)。近年來,聚多巴胺(Polydopamine,PDA)由于具有獨(dú)特的物理粘附性、親水性、穩(wěn)定性及良好的生物相容性,已在分離科學(xué)領(lǐng)域特別是毛細(xì)管電泳中的應(yīng)用引起了研究者的廣泛關(guān)注。鑒于此,本學(xué)位論文在前人工作的基礎(chǔ)上,圍繞以新型聚多巴胺類物質(zhì)為開管毛細(xì)管電色譜(Open Tubular Capillary Electrochromatography,OT-CEC)柱的涂層材料在手性分離中的應(yīng)用,開展了以下創(chuàng)新性研究工作:1.在室溫下,首次原位制備了β-環(huán)糊精和聚多巴胺復(fù)合材料(β-CD/PDA)涂層的開管毛細(xì)管柱,并以其為OT-CEC分離通道,實(shí)現(xiàn)了七對(duì)手性化合物的分離。2.在室溫下,首次以CuSO_4/H_2O_2作為引發(fā)劑將聚左旋多巴胺(poly-(L-DOPA))通過物理沉積和吸附的方式成功地修飾在毛細(xì)管內(nèi)壁上,制備了新型涂層毛細(xì)管柱。利用該涂層毛細(xì)管實(shí)現(xiàn)了十對(duì)手性化合物的分離。3.首次制備了L-組氨酸@聚左旋多巴胺(L-His/poly-(L-DOPA))涂層的開管毛細(xì)管柱,并考察了此柱對(duì)手性化合物的分離能力。本論文共分為四章:第一章簡要介紹了近年來不同涂層技術(shù)在開管毛細(xì)管電色譜手性分離中的應(yīng)用。第二章在室溫下,首次通過聚多巴胺的粘附性質(zhì)原位快速制備了β-CD/PDA涂層毛細(xì)管。利用掃描電子顯微鏡(SEM)、傅立葉紅外光譜(FT-IR)、流動(dòng)電勢(SPs)、電滲流等對(duì)涂層毛細(xì)管進(jìn)行了表征,表明β-CD/PDA被成功地修飾在毛細(xì)管內(nèi)壁上。詳細(xì)考察了背景電解質(zhì)的種類、濃度和pH、有機(jī)添加劑、β-CD和多巴胺的用量以及聚合時(shí)間等對(duì)手性分離的影響。結(jié)果表明,當(dāng)以β-CD和多巴胺的用量均為5.0 mg/mL、聚合時(shí)間為1.0 h時(shí)獲得的涂層毛細(xì)管為分離通道時(shí),可實(shí)現(xiàn)對(duì)特布他林、卡維地洛、維拉帕米、腎上腺素、去甲腎上腺素、異丙腎上腺素和色氨酸等對(duì)映異構(gòu)體的分離。第三章在室溫下,首次以CuSO_4(5 mM)/H_2O_2(19.6 mM)作為引發(fā)劑,原位快速制備了聚左旋多巴(poly-(L-DOPA))涂層毛細(xì)管,并將其作為分離通道用于對(duì)映異構(gòu)體的分離。CuSO_4/H_2O_2可催化產(chǎn)生活性氧,從而加快左旋多巴的聚合和沉積。我們先用離線實(shí)驗(yàn)驗(yàn)證了用此方法制備poly-(L-DOPA)涂層毛細(xì)管的可行性,并用SEM、FI-IR、流動(dòng)電勢和電滲流對(duì)涂層毛細(xì)管進(jìn)行了表征。進(jìn)而,以三種手性胺類藥物、三種胺類神經(jīng)遞質(zhì)、四種氨基酸對(duì)映體為模型分析物,詳細(xì)地考察了實(shí)驗(yàn)條件包括聚合時(shí)間等對(duì)涂層毛細(xì)管分離性能的影響。此涂層柱具有良好的穩(wěn)定性和重現(xiàn)性,可連續(xù)使用250次而不引起分離效率的改變。第四章在第三章工作的基礎(chǔ)上,首先原位制備了poly-(L-DOPA)涂覆的開口毛細(xì)管,再進(jìn)一步將L-組氨酸修飾在毛細(xì)管內(nèi)壁上,并考察了該涂層柱在手性分離中的應(yīng)用。結(jié)果表明,L-組氨酸與poly-(L-DOPA)作為手性選擇劑的協(xié)同作用,導(dǎo)致L-His/poly-(L-DOPA)涂層毛細(xì)管柱對(duì)色氨酸和卡維地洛對(duì)映體具有良好的手性分離效果。
[Abstract]:Chirality is one of the essential properties of nature. The separation of chiral compounds has been a hot and difficult point in the field of separation. In recent years, polydopamine polydopamine (PDAA) has been hydrophilic due to its unique physical adhesion. Stability and good biocompatibility have attracted wide attention in the field of separation science, especially in capillary electrophoresis. Based on the application of a novel polydopamine coating material used in chiral separation on Open Tubular Capillary ElectrochromatographyCcolumn, the following innovative research work was carried out at room temperature. The open tube capillary column of 尾 -cyclodextrin and polydopamine composite (尾 -CD / PDA) coating was prepared in situ for the first time and used as the OT-CEC separation channel to achieve the separation of seven chiral compounds at room temperature. Poly (L-DOPA) was successfully modified on the inner wall of capillary by physical deposition and adsorption with CuSO_4/H_2O_2 as initiator for the first time. A novel coated capillary column was prepared. The separation of ten chiral compounds was achieved by using the coated capillary column. For the first time, an open-tube capillary column with Lhistidine @ poly-L-histidine @ poly-L-DOPAP coating was prepared. The separation ability of chiral compounds on this column was also investigated. This thesis is divided into four chapters: chapter 1 briefly introduces the application of different coating techniques in chiral separation by capillary electrochromatography at room temperature in recent years, the second chapter is about the separation of chiral compounds by capillary electrochromatography at room temperature. The 尾 -CD-P / PDA coated capillary tubes were prepared by the adhesion properties of polydopamine for the first time. The coated capillaries were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), flow potential (FEP) and electroosmotic flow (EOF). The results showed that 尾 -CD / P PDA was successfully modified on the inner wall of capillary tube. The effects of background electrolytes, concentration and pH, organic additives, amounts of 尾 -CD and dopamine, and polymerization time on chiral separation were investigated in detail. When the amount of 尾 -CD and dopamine were 5.0 mg / mL and the coated capillary tubes obtained at 1.0 h were used as separation channels, p-terbutaline, carvedilol, verapamil, epinephrine and norepinephrine could be achieved. Separation of enantiomers such as isoproterenol and tryptophan. In chapter 3, CuSO_4(5 mM)/H_2O_2(19.6 mm was used as initiator for the first time in situ to prepare poly-L-DOPA-coated capillary tubes. It is used as a separation channel for separation of enantiomers. CuSOs 4 / H _ 2O _ 2 can catalyze the production of reactive oxygen species, thus accelerating the polymerization and deposition of levodopa. The coated capillary was characterized by SEMFI-IRI, flow potential and electroosmotic flow. Further, three chiral amines, three amine neurotransmitters and four amino acid enantiomers were used as model analytes. The effects of experimental conditions, including polymerization time, on the capillary separation performance of the coating were investigated in detail. The coating column has good stability and reproducibility. In chapter 4, on the basis of the work in chapter 3, the poly-L-DOPA-coated open capillary tube was prepared in situ, and the L-histidine was further modified on the inner wall of the capillary. The application of the coated column in chiral separation was also investigated. The results showed that the synergistic effect of L-histidine and poly-L-DOPA as chiral selector resulted in a good chiral separation of tryptophan and carvedilol on L-His-p-poly-L-DOPA-coated capillary column.
【學(xué)位授予單位】：蘭州大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O652.6

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