目的:制备阿魏酸/钾/β-环糊精金属有机骨架包合物(FA/K/β-CD/MOF),并优化其制备工艺。方法:利用溶剂热法制备K/β-CD/MOF,以其为包合材料、FA为主药,采用研磨法制备FA/K/β-CD/MOF。以主药-包合材料摩尔比、研磨时间、滴加时间、包合温度为考察因素,以包合率为评价指标,通过正交设计优化处方工艺。采用红外光谱和差示扫描量热法对所制FA/K/β-CD/MOF进行鉴定,并测定其包合率和溶解度。结果:最优处方工艺为主药-包合材料摩尔比3∶1、滴加时间60 min、包合温度40℃、包合时间60 min;所制得的FA/K/β-CD/MOF已经构成一种新的物相,其平均包合率为(18.0±1.6)%,RSD为0.9%(n=6),其溶解度是FA的15倍(9.582 mg/ml vs.0.647 mg/ml)。结论:成功制得FA/K/β-CD/MOF,且处方工艺合理、可行。
OBJECTIVE: To prepare Ferulic acid/K/β-CD/metal organic framework (FA/K/fl-CD/MOF) inclusion, and to optimize its preparation technology. METHODS: K/β-CD/MOF was synthesized by solvotbermal method as inclusion material. Using FA as main component, FA/K/β-CD/MOF was prepared by grinding method. The preparation technology was optimized by orthogonal test using mole ratio of main component-inclusion material, grinding time, dropping time and inclusion temperature as factors, inclusion rate as index. Prepared FA/K/β-CD/MOF was indentified by IR spectrum and DSC, and inclusion rate and dissolution rate were determined. RESULTS: Optimized preparation technology was as follows as mole ratio of main main component to inclusion material 3 : 1, dropping time 60 rain, inclusion temperature 40 ℃, inclusion time 60 min. Prepared FA/K/β-CD-MOF had already formed a new kind of phase, and its average inclusion rate was (18.0 ± 1.6)% (RSD=0.9%, n=6); its solubility was 15 times as much as FA (9.582 mg/ml vs. 0.647 mg/ml). CONCLUSIONS: FA/K/β-CD/MOF is prepared successfully; and the preparation technology is reasonable and feasible.