壳聚糖/凹凸棒复合辅料固化薄荷挥发油的工艺优化及粉体性能评价

Process Optimization and Powder Performance Evaluation of Chitosan/Attapulgite Compound Excipients for Curing Peppermint Volatile Oil

目的 以壳聚糖(chitosan,CS)和凹凸棒(attapulgite,ATP)为原料,制备适宜于固化薄荷挥发油的复合辅料。方法 以3%冰醋酸为分散介质分散CS和ATP,薄荷挥发油为模型药物,薄荷挥发油保留率为考察指标,复合辅料改性比例、搅拌时间及搅拌温度为考察因素,通过响应面法优选CS/ATP复合辅料固化薄荷挥发油的最佳工艺参数,并对该工艺条件下复合辅料的粉体性能及固化挥发油后的湿、热稳定性进行测试,同时进行扫描电子显微镜、傅里叶变换红外光谱、X射线衍射表征分析。结果 复合辅料CS/ATP固化薄荷挥发油的最佳工艺参数:CS与ATP比例为1∶9,搅拌时间为16 h,搅拌温度为55℃。在CS/ATP复合辅料制备工艺优选条件下,50℃放置3 d后,薄荷挥发油的保留率为78.02%,较同等条件下未用CS/ATP固化的薄荷挥发油保留率提高了90.45%;CS/ATP复合辅料粉体性能测试表明,复合辅料阻湿性较好,复合后流动性良好。结论 CS/ATP复合辅料制备工艺简单,可操作性强,在固化薄荷挥发油方面有潜在的应用价值。

OBJECTIVE To prepare a compound excipient suitable for curing peppermint oil using chitosan(CS) and attapulgite(ATP) as raw materials.METHODS CS and ATP were dispersed with 3% glacial acetic acid as dispersion medium,peppermint oil was used as a model drug,the retention rate of peppermint oil was the inspection index,the modification ratio of the composite excipients,the stirring time and the stirring temperature were the investigation factors,the best process parameters of CS/ATP composite excipients for curing peppermint oil was optimized by response surface methodology,and the powder properties of the composite excipients and the moisture and thermal stability after curing the volatile oil under the process conditions were tested,and scanning electron microscope,Fourier transform infrared spectroscopy,X-ray diffraction characterization analysis was performed at the same time.RESULTS The best process parameters for the composite excipient CS/ATP to solidify the volatile oil of mint were:the ratio of CS to ATP was 1∶9,the stirring time was 16 h,and the stirring temperature was 55 ℃.Under the optimal conditions for the preparation of CS/ATP composite excipients,it was placed at 50 ℃after 3 d,the retention rate of the oil of peppermint was 78.02%,which was 90.45% higher than the retention rate of the oil of peppermint which was not cured with CS/ATP under the same conditions.The powder performance test of CS/ATP composite excipients showed that the composite excipients had better moisture barrier properties and good liquidity.CONCLUSION The preparation process of CS/ATP composite excipients is simple and has strong operability.It has potential application value in curing peppermint oil.