【摘要】：表面增強拉曼光譜(SERS)技術(shù)自發(fā)現(xiàn)以來一直備受關(guān)注,作為現(xiàn)代檢測中一項重要的技術(shù),能夠使分析物分子的拉曼信號得到有力增強。SERS具有靈敏度高、熒光背景低、對檢測樣品無損等優(yōu)點,因此使其在化學(xué)工業(yè)分析、生物分析以及醫(yī)藥檢測等諸多領(lǐng)域都有廣泛應(yīng)用。納米銀粒子因具備一些非常特殊的性質(zhì),如表面效應(yīng),量子尺寸效應(yīng)等,使納米銀粒子能夠廣泛用于表面增強拉曼光譜中,是SERS中增強效果最好的基底材料之一。納米銀粒子的制備方法一直是SERS應(yīng)用研究中的熱點領(lǐng)域。納米銀的傳統(tǒng)制備工藝一般較為復(fù)雜、影響其成形的多種因素不易控制,從而阻礙了其在SERS中的廣泛應(yīng)用。本文主要圍繞納米銀粒子的制備及其在表面增強拉曼光譜法測定有機小分子藥物中的應(yīng)用進行論述。采用了脂質(zhì)體法和SDS-環(huán)己烷微乳法來制備納米銀粒子,并用得到的納米銀粒子來制備SERS活性基底,用于對乙酰氨基酚和阿司匹林的測定。 一、結(jié)合了藥物制劑新劑型的發(fā)展,探索一種脂質(zhì)體法來制備納米銀粒子的新方法,研究制備方法以及反應(yīng)條件對納米銀粒子尺寸、形貌的影響,選擇出最優(yōu)的處方工藝來制備粒徑均勻、性能穩(wěn)定的納米銀粒子,并對其進行表征。最終確定以薄膜分散法來制備納米銀脂質(zhì)體,選擇乙醚為有機溶劑,大豆磷脂與膽固醇的比例3：1,硝酸銀溶液的濃度確定為0.03mol·L-1,其他實驗條件如下：水浴溫度為40℃,檸檬酸三鈉的濃度為1%,超聲時間為10min。最后得到的納米銀粒子的形貌主要以類球形為主,粒徑控制在20-80nm之間。 二、與傳統(tǒng)的微乳液法制備納米銀粒子的方法相結(jié)合,選擇SDS-環(huán)己烷微乳體系來制備納米銀,以十二烷基硫酸鈉(SDS)為表面活性劑,以異戊醇為助表面活性劑,連續(xù)油相為環(huán)己烷,硝酸銀或水合肼的水溶液為分散相,通過水合肼來還原AgNO3,來制備粒徑均勻、性能穩(wěn)定的納米銀粒子并對其進行表征。結(jié)果表明當(dāng)體系含水量W=5,硝酸銀溶液濃度為0.2mol·L-1時的微乳液體系制備得到的納米銀粒子,形貌可得為類球形的納米粒子,平均粒徑的分布范圍在50-100nm之間。 三、用制得的納米銀粒子來制備SERS活性基底,并把其用于研究藥物分子在SERS上的應(yīng)用,并通過在不同SERS基底上的變化,來研究各納米銀粒子表征對其活性的影響。結(jié)果表明脂質(zhì)體法制備的納米銀粒子當(dāng)粒徑在20-80nm之間,組裝時間為24h～48h之間時得到的活性基底的增強強度較大。得出SERS能夠用于對乙酰氨基酚和阿司匹林的檢測上,并能對其進行定性分析,具有操作簡便、靈敏度高等優(yōu)點。
[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，

本文編號：2331456