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纳米银的制备及其用于SERS法测定药物的研究

发布时间:2018-11-14 14:40
【摘要】:表面增强拉曼光谱(SERS)技术自发现以来一直备受关注,作为现代检测中一项重要的技术,能够使分析物分子的拉曼信号得到有力增强。SERS具有灵敏度高、荧光背景低、对检测样品无损等优点,因此使其在化学工业分析、生物分析以及医药检测等诸多领域都有广泛应用。纳米银粒子因具备一些非常特殊的性质,如表面效应,量子尺寸效应等,使纳米银粒子能够广泛用于表面增强拉曼光谱中,是SERS中增强效果最好的基底材料之一。纳米银粒子的制备方法一直是SERS应用研究中的热点领域。纳米银的传统制备工艺一般较为复杂、影响其成形的多种因素不易控制,从而阻碍了其在SERS中的广泛应用。本文主要围绕纳米银粒子的制备及其在表面增强拉曼光谱法测定有机小分子药物中的应用进行论述。采用了脂质体法和SDS-环己烷微乳法来制备纳米银粒子,并用得到的纳米银粒子来制备SERS活性基底,用于对乙酰氨基酚和阿司匹林的测定。 一、结合了药物制剂新剂型的发展,探索一种脂质体法来制备纳米银粒子的新方法,研究制备方法以及反应条件对纳米银粒子尺寸、形貌的影响,选择出最优的处方工艺来制备粒径均匀、性能稳定的纳米银粒子,并对其进行表征。最终确定以薄膜分散法来制备纳米银脂质体,选择乙醚为有机溶剂,大豆磷脂与胆固醇的比例3:1,硝酸银溶液的浓度确定为0.03mol·L-1,其他实验条件如下:水浴温度为40℃,柠檬酸三钠的浓度为1%,超声时间为10min。最后得到的纳米银粒子的形貌主要以类球形为主,粒径控制在20-80nm之间。 二、与传统的微乳液法制备纳米银粒子的方法相结合,选择SDS-环己烷微乳体系来制备纳米银,以十二烷基硫酸钠(SDS)为表面活性剂,以异戊醇为助表面活性剂,连续油相为环己烷,硝酸银或水合肼的水溶液为分散相,通过水合肼来还原AgNO3,来制备粒径均匀、性能稳定的纳米银粒子并对其进行表征。结果表明当体系含水量W=5,硝酸银溶液浓度为0.2mol·L-1时的微乳液体系制备得到的纳米银粒子,形貌可得为类球形的纳米粒子,平均粒径的分布范围在50-100nm之间。 三、用制得的纳米银粒子来制备SERS活性基底,并把其用于研究药物分子在SERS上的应用,并通过在不同SERS基底上的变化,来研究各纳米银粒子表征对其活性的影响。结果表明脂质体法制备的纳米银粒子当粒径在20-80nm之间,组装时间为24h~48h之间时得到的活性基底的增强强度较大。得出SERS能够用于对乙酰氨基酚和阿司匹林的检测上,并能对其进行定性分析,具有操作简便、灵敏度高等优点。
[Abstract]:Surface enhanced Raman spectroscopy (SERS) technology has attracted much attention since it was discovered. As an important technique in modern detection, it can enhance the Raman signal of analyte molecules. SERS has high sensitivity and low fluorescence background. It is widely used in many fields, such as chemical industry analysis, biological analysis and medical testing. Because of its special properties, such as surface effect and quantum size effect, silver nanoparticles can be widely used in surface-enhanced Raman spectroscopy, which is one of the most effective substrates in SERS. The preparation of silver nanoparticles has been a hot area in the application of SERS. The traditional preparation process of nano-silver is generally complex, and many factors affecting its forming are difficult to control, which hinders its wide application in SERS. In this paper, the preparation of silver nanoparticles and its application in the determination of small organic drugs by surface-enhanced Raman spectroscopy are discussed. The silver nanoparticles were prepared by liposome method and SDS- cyclohexane microemulsion method. The active substrates of SERS were prepared by using the silver nanoparticles obtained and used for the determination of acetaminophen and aspirin. First, combined with the development of new dosage forms of pharmaceutical preparations, we explored a new method of preparing silver nanoparticles by liposome, and studied the effects of preparation methods and reaction conditions on the size and morphology of silver nanoparticles. The best prescription technology was selected to prepare and characterize the silver nanoparticles with uniform particle size and stable performance. Finally, the nanometer silver liposomes were prepared by thin-film dispersion method. The ratio of soybean phospholipids to cholesterol was 3: 1, and the concentration of silver nitrate solution was determined to be 0.03mol L -1, the ratio of soybean phospholipids to cholesterol was 3: 1. Other experimental conditions are as follows: the water bath temperature is 40 鈩,

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