鱼腥草挥发油羟丙基-β环糊精包合物的制备

Preparation of hydroxypropyl-β cyclodextrin inclusion compound of volatile oil from Houttuyniae Herba

目的制备鱼腥草挥发油羟丙基-β环糊精包合物。方法 GC法测定挥发油含有量(以甲基正壬酮为对照品),计算包合率和载药量。分别采用搅拌法、研磨法和超声法制备包合物。以挥发油与羟丙基-β环糊精比例、包合温度、搅拌速度、包合时间为影响因素,包合率和载药量为评价指标,正交试验优化制备工艺。TLC法、红外光谱法、差示扫描量热法进行表征。再通过高温、高湿、强光照试验考察包合物稳定性。结果搅拌法所得包合物的产率、包合率、载药量均最高。最佳条件为挥发油与羟丙基-β环糊精比例1∶25,包合温度50℃,搅拌速度420 r/min,包合时间80 min,包合率77.35%,载药量4.48%。所得包合物为白色粉末,质地疏松,溶解度显著增加,体外累计释放度达80.05%。其在高温(60℃)、强光照(3 000 lx)下稳定性良好,而在相对湿度大于75%时潮解结块,包合率和载药量明显降低,但复水性良好。结论鱼腥草挥发油羟丙基-β环糊精包合物不是简单的混合物,有可能生成了新物相,在储藏时应保持干燥密封。

AIM To prepare the hydroxypropyl-13 cyclodextrin inclusion compound of volatile oil from Hout- tuyniae Herba. METHODS In the content determination of volatile oil by GC, 2-undecanone was taken as a ref- erence substance, and inclusion rate and drug loading were calculated. After the determination of optimal method for preparing the inclusion compound among techniques of mixing, grinding and ultrasonic methods, the preparation process was optimized by orthogonal test with ratio of volatile oil to hydroxypropyl-β eyclodextrin, inclusion temper- ature, mixing speed and inclusion time as influencing factors, and inclusion rate and drug loading as evaluation in- dices. The characterization was performed by TLC, infrared spectroscopy and differential scanning calorimetry. Then high temperature, high humidity and strong light tests were applied to investigating the inclusion compound stability. RESULTS Mixing method brought forth the maximal yield, inclusion rate and drug loading for the in- clusion compound. And under the optimal conditions of 1 ： 25 for ratio of volatile oil to hydroxypropylq3 cyelodex- trin, 50 ~C for inclusion temperature, 420 r/min for mixing speed, and 80 min for inclusion time, the inclusion rate and drug loading were identified to be 77.35% and 4. 48% , respectively. The obtained inclusion compound was found to be white powder with loose texture and significantly increased solubility, the in vitro accumulative re- lease rate reached 80. 85~/6. Deliquescence and agglomeration, as well as obviously decreased inclusion rate and drug loading, were observed at a relative humidity of more than 75% , despite the good stability at high temperature （60 ℃ ） and strong light （3 000 Ix）, and yet the rehydration character was good. CONCLUSION It is possible that the hydroxypropyl-~ cyclodextrin inclusion compound of volatile oil from Houttuyniae Herba generates a new phase rather than a simple mixture, which should be kept dry and sealed at the time of storage.