核—?dú)そY(jié)構(gòu)金絲桃素分子印跡磁納米球的簡(jiǎn)便制備方法研究
發(fā)布時(shí)間：2018-08-07 18:25
【摘要】：作為貫葉連翹的主要活性成份,金絲桃素具有抗菌消炎、抗抑郁、抗病毒、抗癌等一系列的藥理活性受到人們的重視。但是,貫葉連翹中金絲桃素的含量極低,導(dǎo)致從植物中提取困難,提取效率低下。分子印跡聚合物技術(shù)因其可賦予材料對(duì)特定分子的特異性識(shí)別和吸附能力成為解決金絲桃素提取問題的有效途徑之一�；诖�,我們以Fe3O4為基體,多巴胺為功能單體和交聯(lián)劑,在金絲桃素的存在下,通過多巴胺的氧化自聚形成一種具有結(jié)構(gòu)的表面分子印跡聚合物納米球(Fe3O4@PDA/Hyp)。論文首先采用FTIR、TEM、DLS、Zeta電位和BET等技術(shù)對(duì)合成的各種磁納米球(包括基體磁納米球、金絲桃素印跡和非印跡磁納米球)進(jìn)行了表征。結(jié)果表明多巴胺可以在磁球表面生成厚度介于23-29納米的聚多巴胺(PDA)薄膜,從而形成穩(wěn)定的結(jié)構(gòu)納米粒子。然后對(duì)影響金絲桃素分子印跡磁納米球(Fe3O4@PDA/Hyp)印跡效果的合成條件,包括多巴胺的濃度、丙酮的含量、模板分子和功能單體的比、反應(yīng)溫度、反應(yīng)介質(zhì)的p H、反應(yīng)物的添加順序以及是否進(jìn)行乙醇胺處理等進(jìn)行了研究。通過比較不同條件下制備的Fe3O4@PDA/Hyp納米球?qū)鸾z桃素吸附量的大小,確定了其最佳合成條件,即:在室溫條件下,首先將金絲桃素模板分子加入到基體磁珠的懸浮液中,隨后加入多巴胺單體進(jìn)行聚合。其中多巴胺的濃度為2mg/mL,丙酮與Tris-HCl的體積比為1:6,金絲桃素與多巴胺的摩爾比為1:122,溶液的pH為8.0。最后,對(duì)制備的納米球用乙醇胺進(jìn)行處理以獲得最終的Fe3O4@PDA/Hyp磁納米粒子。在此條件下制備的Fe3O4@PDA/Hyp磁納米球?qū)τ诮鸾z桃素的吸附量為18.28 mg/g。以原金絲桃和大黃素作為金絲桃素的結(jié)構(gòu)類似物,對(duì)Fe3O4@PDA/Hyp磁納米球的特異識(shí)別能力進(jìn)行研究,發(fā)現(xiàn)其對(duì)原金絲桃和大黃素的選擇因子SF分別為1.92和3.55,其對(duì)金絲桃素、原金絲桃和大黃素的印跡因子IF分別8.01、3.07和1.36,表明本工作制備的Fe3O4@PDA/Hyp磁納米球?qū)鸾z桃素模板分子具有令人滿意的識(shí)別能力和印跡效果。對(duì)該納米球吸附動(dòng)力學(xué)研究表明,其對(duì)金絲桃素分子的吸附符合Langmuir的吸附模型。實(shí)際應(yīng)用初步研究發(fā)現(xiàn),本工作制備的Fe3O4@PDA/Hyp磁納米球?qū)ω炄~連翹提取液中的金絲桃素具備較好的選擇性識(shí)別和吸附能力。該方法制備簡(jiǎn)便,制備的Fe3O4@PDA/Hyp磁納米球?qū)鸾z桃素具有較好的選擇性識(shí)別和吸附能力,有望用作金絲桃素富集和分離的吸附材料。
[Abstract]:As the main active component of Hypericum perforatum, hypericin has a series of pharmacological activities, such as anti-inflammatory, anti-depressant, anti-virus, anti-cancer and so on. However, the content of hypericin in Hypericum perforatum was very low, which led to the difficulty of extracting from plants and the low extraction efficiency. Molecularly imprinted polymer technology has become one of the effective ways to solve the problem of extraction of hypericin because of its ability of specific recognition and adsorption to specific molecules. Therefore, in the presence of hypericin, a surface molecularly imprinted polymer nanospheres (Fe3O4@PDA/Hyp) were formed by oxidation self-polymerization of dopamine with Fe3O4 as matrix, dopamine as functional monomer and crosslinking agent. The synthesized magnetic nanospheres (including matrix magnetic nanospheres, hypericin imprinted and non-imprinted magnetic nanospheres) were characterized by FTIR Tem Tem DLS Zeta potential and BET. The results show that dopamine can form polydopamine (PDA) thin films with thickness of 23-29 nanometers on the surface of magnetic spheres, thus forming stable structured nanoparticles. Then the synthetic conditions affecting the imprinting effect of hypericin molecularly imprinted magnetic nanospheres (Fe3O4@PDA/Hyp) were studied, including the concentration of dopamine, the content of acetone, the ratio of template molecule to functional monomer, the reaction temperature, The pH of the reaction medium, the addition order of reactants and the treatment of ethanolamine were studied. By comparing the amount of hypericin adsorbed by Fe3O4@PDA/Hyp nanospheres prepared under different conditions, the optimum synthesis conditions were determined: firstly, hypericin template molecule was added to the suspension of matrix magnetic beads at room temperature. Then dopamine monomer was added for polymerization. The concentration of dopamine is 2 mg / mL, the volume ratio of acetone to Tris-HCl is 1: 6, the molar ratio of hypericin to dopamine is 1: 122, the pH of solution is 8.0. Finally, the prepared nanospheres were treated with ethanolamine to obtain the final Fe3O4@PDA/Hyp magnetic nanoparticles. Under these conditions, the adsorption capacity of Fe3O4@PDA/Hyp magnetic nanospheres for hypericin was 18.28 mg / g. The specific recognition ability of Fe3O4@PDA/Hyp magnetic nanospheres was studied by using proto hypericin and emodin as structural analogues of hypericin. It was found that the selective factors SF for proto hypericin and emodin were 1.92 and 3.55, respectively. The imprinting factors of hypericin and emodin were 8.01 ~ 3.07 and 1.36, respectively, which indicated that the Fe3O4@PDA/Hyp magnetic nanospheres had satisfactory recognition ability and imprinting effect on hypericin template molecule. The adsorption kinetics of the nanospheres showed that the adsorption of hypericin was in accordance with the Langmuir adsorption model. It is found that the Fe3O4@PDA/Hyp magnetic nanospheres prepared in this work have good selective recognition and adsorption ability for hypericin in the extract of Hypericum perforatum. The prepared Fe3O4@PDA/Hyp magnetic nanospheres have good selective recognition and adsorption ability for hypericin, which is expected to be used as an adsorptive material for hypericin enrichment and separation.
【學(xué)位授予單位】：西北農(nóng)林科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O631.3;TB383.1
[Abstract]:As the main active component of Hypericum perforatum, hypericin has a series of pharmacological activities, such as anti-inflammatory, anti-depressant, anti-virus, anti-cancer and so on. However, the content of hypericin in Hypericum perforatum was very low, which led to the difficulty of extracting from plants and the low extraction efficiency. Molecularly imprinted polymer technology has become one of the effective ways to solve the problem of extraction of hypericin because of its ability of specific recognition and adsorption to specific molecules. Therefore, in the presence of hypericin, a surface molecularly imprinted polymer nanospheres (Fe3O4@PDA/Hyp) were formed by oxidation self-polymerization of dopamine with Fe3O4 as matrix, dopamine as functional monomer and crosslinking agent. The synthesized magnetic nanospheres (including matrix magnetic nanospheres, hypericin imprinted and non-imprinted magnetic nanospheres) were characterized by FTIR Tem Tem DLS Zeta potential and BET. The results show that dopamine can form polydopamine (PDA) thin films with thickness of 23-29 nanometers on the surface of magnetic spheres, thus forming stable structured nanoparticles. Then the synthetic conditions affecting the imprinting effect of hypericin molecularly imprinted magnetic nanospheres (Fe3O4@PDA/Hyp) were studied, including the concentration of dopamine, the content of acetone, the ratio of template molecule to functional monomer, the reaction temperature, The pH of the reaction medium, the addition order of reactants and the treatment of ethanolamine were studied. By comparing the amount of hypericin adsorbed by Fe3O4@PDA/Hyp nanospheres prepared under different conditions, the optimum synthesis conditions were determined: firstly, hypericin template molecule was added to the suspension of matrix magnetic beads at room temperature. Then dopamine monomer was added for polymerization. The concentration of dopamine is 2 mg / mL, the volume ratio of acetone to Tris-HCl is 1: 6, the molar ratio of hypericin to dopamine is 1: 122, the pH of solution is 8.0. Finally, the prepared nanospheres were treated with ethanolamine to obtain the final Fe3O4@PDA/Hyp magnetic nanoparticles. Under these conditions, the adsorption capacity of Fe3O4@PDA/Hyp magnetic nanospheres for hypericin was 18.28 mg / g. The specific recognition ability of Fe3O4@PDA/Hyp magnetic nanospheres was studied by using proto hypericin and emodin as structural analogues of hypericin. It was found that the selective factors SF for proto hypericin and emodin were 1.92 and 3.55, respectively. The imprinting factors of hypericin and emodin were 8.01 ~ 3.07 and 1.36, respectively, which indicated that the Fe3O4@PDA/Hyp magnetic nanospheres had satisfactory recognition ability and imprinting effect on hypericin template molecule. The adsorption kinetics of the nanospheres showed that the adsorption of hypericin was in accordance with the Langmuir adsorption model. It is found that the Fe3O4@PDA/Hyp magnetic nanospheres prepared in this work have good selective recognition and adsorption ability for hypericin in the extract of Hypericum perforatum. The prepared Fe3O4@PDA/Hyp magnetic nanospheres have good selective recognition and adsorption ability for hypericin, which is expected to be used as an adsorptive material for hypericin enrichment and separation.
【學(xué)位授予單位】：西北農(nóng)林科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O631.3;TB383.1
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