目的:制备阿司匹林磷脂复合物(ASP-PC)并进行表征。方法:以ASP与PC的复合率为指标,采用单因素试验筛选ASP-PC的制备方法、PC种类、溶剂种类、反应时间、反应温度、溶剂体积和药脂比,并进行验证。采用紫外分光光度法、热重分析法、X射线衍射法和傅里叶红外光谱分析对所制ASP-PC进行表征。结果:采用磁力搅拌-冷凝回流法,药物-大豆磷脂比为1∶3(mol/mol),溶剂为四氢呋喃(50 m L),58℃下反应3 h,所制ASP-PC的平均复合率为83.52%(RSD=1.16%,n=3)。与ASP、ASP和PC的物理混合物比较,紫外光谱显示ASP-PC没有出现新的吸收峰;热重分析、X射线衍射分析和傅里叶红外光谱分析显示ASP-PC中的ASP与PC发生了相互作用,且ASP-PC在0~300℃范围内质量变化较小。结论:成功制得ASP-PC,其中ASP与PC复合成功,但仍有微量ASP以晶体形式存在。
OBJECTIVE: To prepare aspirin phospholipid complex (ASP-PC) and conduct the characterization. METHODS: Using the combination rate of ASP and PC as index, single factor test was used to screen the preparation method of ASP-PC, PC type, solvent type, reaction time, reaction temperature, solvent volume and drug-lipid ratio. The verification test was conducted. UV spectrophotometry, Therrnogravimetric analysis, X-ray diffraction and Fourier transform infrared spectroscopy were used for the characterization of ASP-PC. RESULTS: Magnetic stirring-condensing reflux method was adopted, drug-soybean phospholipids ratio was 1 : 3 (mol/mol), solvent was tetrahydrofuran, reacting for 3 h under 58℃. The average combination rate of prepared ASP-PC was 83.52% (RSD=1.16%, n=3). Compared with ASP, physical mixture of ASP and PC, UV spectrum showed that ASP-PC had no new absorption peak. Thermogravimetric analysis, X-ray diffraction and Fourier transform infrared spectroscopy showed the ASP and PC in ASP-PC were interacted; and ASP-PC changed little in quality within 0-300 ℃. CONCLUSIONS: ASP-PC can be successfully prepared, in which, ASP and PC were combined successfully; while there are still trace amounts of ASP in the form of crystals.