甲基-β-环糊精与芘包合物的制备与表征

Preparation and characterization of the inclusioncompound of pyrene with methyl -β- cyclodextrin

摘要:

以甲基-β-环糊精与芘为原料，通过饱和溶液法制备得到甲基-β-环糊精与芘的包合物(INC)，并利用紫外光谱（UV）、红外光谱（IR）、热重-差热分析（TG-DSC）、扫描电镜（SEM)以及X射线粉末衍射（XRD）等对其结构与性能进行了表征。对不同温度下INC的紫外光谱和红外光谱进行了考察。结果表明：当制备温度为25 ℃时，INC包得率最高（为39%），在240 nm处对应吸光度最大（为1.62）；IR检测到受包合物形成的影响，包合物INC中芘的特征峰强度变低、峰形变宽或发生位移；TG-DSC表明，芘占据甲基-β-环糊精的空腔生成了包合物，并通SEM、XRD显示，包合物出现一组新的特征衍射峰2θ=11.73°、 18.04°、20.56°；甲基-β-环糊精与芘可形成稳定的包合物，当温度为25 ℃时，甲基-β-环糊精（MCD）使芘在水中的质量浓度增加到7.36 mg/L，为15℃时2倍。

Abstract:

To study the characterization of the inclusion compound of pyrene with methyl-β-cyclodextrin，which is formed by two ingredients(pyrene and methyl-β-cyclodextrin) and prepared with saturated solution method, the inclusion compound was prepared at difference conditions and studied by using ultraviolet spectroscopy(UV),infrared spectroscopy(IR),thermal gravimetric analysis(TG),differential thermal analysis(DSC), scanning electron microscope(SEM),X-ray diffraction(XRD) and other methods. According to the results, the inclusion efficiency of saturated aqueous solution method is higher (39%) at 25 ℃ conditions, At 240nm, the corresponding absorbance was the largest (1.62).With IR method, characteristic peak intensity of pyrene becomes lower and peak shape widens or displaces. With TG, DSC methods, pyrene occupies methyl-β-cyclodextrin cavity and the inclusion compound is formed ,and with XRD method, the inclusion compound shows a new set of characteristic diffraction peaks at 11.73 °, 18.04 °, 20.56 °. Conclusion shows that pyrene and methyl-β-cyclodextrin could form a stable inclusion compound when the temperature is 25℃. MCD increases the mass concentration of pyrene in water to 7.36 mg/L, which twice time of 15℃.