熒光手性銀納米簇的制備、表征及用于手性分子的檢測(cè)研究
發(fā)布時(shí)間：2018-07-21 20:02
【摘要】：目前,很多研究者都對(duì)熒光和手性銀納米簇(AgNCs)的制備和應(yīng)用特別感興趣,并進(jìn)行了大量的研究。但AgNCs的制備方法還有待進(jìn)一步改進(jìn),同時(shí)關(guān)于AgNCs的熒光增強(qiáng)機(jī)理研究不夠充分。利用AgNCs手性特性進(jìn)行分析的研究較少,相關(guān)研究需要進(jìn)一步探索。因此本文就熒光手性AgNCs的制備、表征及手性分子的檢測(cè)進(jìn)行了深入的研究。1.本論文使用外消旋谷胱甘肽((±)GSH)作為配體,通過(guò)固相研磨的方法成功合成了既有手性又有熒光的AgNCs。將硝酸銀(AgNO3)和GSH固體混合,充分研磨后加入硼氫化鈉(NaBH4)還原。反應(yīng)完的固體混合物加入水和乙醇進(jìn)行溶解,離心分離純化后得到具有手性的AgNCs。進(jìn)一步將AgNCs溶于水,孵育24h后得到同時(shí)具有強(qiáng)烈熒光和手性的AgNCs。實(shí)驗(yàn)對(duì)AgNCs的制備溫度、配體比例、溶劑極性、溶劑pH等條件進(jìn)行了優(yōu)化。經(jīng)過(guò)實(shí)驗(yàn)優(yōu)化后的最佳制備條件為:溫度27℃、GSH和AgNO3的比例為3:1、采用水作為溶劑、pH=5.2。2.實(shí)驗(yàn)進(jìn)一步通過(guò)熒光(FL)、高分辨透射電子顯微鏡(HR-TEM)、傅里葉變換紅外光譜(FTIR)、X射線光電子能譜(XPS)、圓二色(CD)光譜和電噴霧電離質(zhì)譜(ESI-MS)對(duì)合成的AgNCs進(jìn)行表征。結(jié)果表明,實(shí)驗(yàn)中通過(guò)固相合成的方法成功制備了熒光手性AgNCs。制備的AgNCs平均粒徑為1.68nm,主要組成為Ag4(SG)4。更有趣的是,實(shí)驗(yàn)中發(fā)現(xiàn)AgNCs粉末溶于水孵育過(guò)程中,其熒光明顯增強(qiáng)且CD信號(hào)發(fā)生翻轉(zhuǎn)。3.實(shí)驗(yàn)深入研究了AgNCs聚集誘導(dǎo)熒光增強(qiáng)(AIEE)和手性變化的特性,采用基質(zhì)輔助激光解吸/電離時(shí)間飛行質(zhì)譜(MALDI-TOF-MS)、熒光(FL)及CD光譜等技術(shù)來(lái)進(jìn)行研究。結(jié)果發(fā)現(xiàn),AgNCs表面連接的GSH之間形成氫鍵引起AgNCs的交聯(lián)聚合,導(dǎo)致AIEE和手性變化的現(xiàn)象。4.將AgNCs用于D/L-青霉胺(D/LPA)、D/L-葡萄糖(D/L-Glu)和D/L-組氨酸(D/L-His)的檢測(cè)。研究表明,制備的AgNCs可以選擇性地與D構(gòu)型的青霉胺、葡萄糖和組氨酸作用,導(dǎo)致熒光信號(hào)發(fā)生變化。然而,L構(gòu)型的青霉胺、葡萄糖和組氨酸對(duì)制備的AgNCs的熒光基本無(wú)影響。同時(shí),研究結(jié)果還表明,可運(yùn)用AgNCs建立熒光傳感進(jìn)行組氨酸的定量分析,以及有望將其應(yīng)用于溫度傳感。
[Abstract]:At present, many researchers are particularly interested in the preparation and application of fluorescent and chiral silver nanoclusters (AgNCs). However, the preparation method of AgNCs needs to be further improved, and the fluorescence enhancement mechanism of AgNCs is not sufficiently studied. There are few studies on chiral properties of AgNCs, which need to be further explored. Therefore, the preparation and characterization of fluorescent chiral AgNCs and the detection of chiral molecules were studied in this paper. In this paper, the chiral and fluorescent AgNCswere synthesized by solid phase grinding using racemic glutathione (鹵) GSH) as ligand. Silver nitrate (Agno _ 3) and GSH were mixed and ground fully, then sodium borohydride (NaBH4) was added. The solid mixture was dissolved in water and ethanol and purified by centrifugation to obtain chiral AgNCs. AgNCs were further dissolved in water and incubated for 24 hours to produce both strong fluorescence and chiral AgNCs. The preparation temperature, ligand ratio, solvent polarity and solvent pH of AgNCs were optimized. The optimum preparation conditions were as follows: the ratio of GSH and Agno _ 3 was 3: 1 at 27 鈩，
本文編號(hào)：2136706
[Abstract]:At present, many researchers are particularly interested in the preparation and application of fluorescent and chiral silver nanoclusters (AgNCs). However, the preparation method of AgNCs needs to be further improved, and the fluorescence enhancement mechanism of AgNCs is not sufficiently studied. There are few studies on chiral properties of AgNCs, which need to be further explored. Therefore, the preparation and characterization of fluorescent chiral AgNCs and the detection of chiral molecules were studied in this paper. In this paper, the chiral and fluorescent AgNCswere synthesized by solid phase grinding using racemic glutathione (鹵) GSH) as ligand. Silver nitrate (Agno _ 3) and GSH were mixed and ground fully, then sodium borohydride (NaBH4) was added. The solid mixture was dissolved in water and ethanol and purified by centrifugation to obtain chiral AgNCs. AgNCs were further dissolved in water and incubated for 24 hours to produce both strong fluorescence and chiral AgNCs. The preparation temperature, ligand ratio, solvent polarity and solvent pH of AgNCs were optimized. The optimum preparation conditions were as follows: the ratio of GSH and Agno _ 3 was 3: 1 at 27 鈩，
本文編號(hào)：2136706
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