[关键词]
[摘要]
目的 以微粒的体积平均粒径为评价指标,优化黄芩素微粒的制备工艺。方法 采用超临界CO2抗溶剂法制备黄芩素微粒,在单因素试验的基础上设计正交试验优选黄芩素微粒的制备工艺,并对优选的工艺组合进行了粒度分布、扫描电镜(SEM)分析、红外吸收光谱法(IR)及差示扫描量热法(DSC)的表征。结果 正交试验得到的优选工艺条件:溶液体积流量0.75 mL/min,结晶压力8 MPa,结晶温度48 ℃,黄芩素质量浓度4 mg/mL;在此工艺条件下制备得到的黄芩素微粒的大小明显小于黄芩素原料,扫描电镜显示制备出的黄芩素微粒为不规则形状;IR和DSC显示黄芩素微粒的化学结构没有发生变化,热力学性质发生了变化,并且经处理过的黄芩素的纯度变高。结论 超临界CO2抗溶剂法制备黄芩素微粒可行,为制备超细微粒提供参考依据。
[Key word]
[Abstract]
Objective The preparation technology of baicalein microparticles was optimized with volume average particle size (VAPS) of micropaticles as the evaluation index. Methods The baicalein micropartocles were prepared by supercritical CO2 antisolvent method. On the basis of single factor tests, orthogonal design was used to optimize the preparation process of baicalein microparticles. The microparticle size distribution, scanning electron microscopy (SEM) analysis, infrared spectrum (IR), and differential scanning calorimetry (DSC) were used to analyze the microparticles. Results The suitable conditions optimized by orthogonal test were set as follows: solvent flow rate 0.75 mL/min, pressure 8 MPa, temperature 48 ℃, and mass concentration of baicalein 4 mg/mL. Under the optimum conditions, the VAPS of the prepared microparticles was obviously smaller than that of the baicalein. And the shapes of baicalein in prepared microparticles were irregular under SEMA. IR and DSC analyses showed that the chemical structure of baicalein microparticles was not changed while the thermodynamic properties of baicalein might change. Meanwhile, the purity of baicalein became higher after the treatment. Conclusion Supercritical CO2 antisolvent method is feasible to prepare baicalein microparticles and provides a reference basis for preparing microparticles at the same time.
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[基金项目]
江苏省自然科学基金项目(BK2012763);大学生创新药物研发能力提高项目“国家级大学生创新创业训练计划项目”(J1030830)