荆芥内酯纳米粒冻干粉末的制备工艺及质量研究

Preparation technology and quality assay of schizonepetolide polylactic-co-glycolic acid nanoparticles lyophilized powder

目的制备荆芥内酯聚乳酸乙醇酸纳米粒冻干粉末,并探讨其工艺与质量评价标准。方法以外观、色泽、再分散性为指标,优选支架剂的种类和浓度及冻干工艺;并对该冻干粉末的外观、再分散性、pH值、纳米粒的形态、粒径分布、多分散系数、质量分数、包封率及载药量等质量评价指标进行考察。结果10%甘露醇作为支架剂可以较好地防止纳米粒的聚集,优化的冻干工艺为-45℃预冻10 h,升温至-25℃维持5 h,再升温至-5℃维持2 h,再升温至10℃维持2 h,最后升温至30℃维持6 h。冻干粉末的外观和分散性良好,平均pH值为6.25,纳米粒平均粒径为80.2 nm,多分散系数为0.024 8,包封率为52.17%,载药量为28.73%。结论荆芥内酯纳米粒冻干粉末制备工艺简便、重复性好;所选用的质量评价方法适用于该冻干粉末,可有效反映其性质。

Objective To study the preparation technology and quality assay of schizonepetolide poly- lactic-co-glycolic acid nanoparticles （SCH-PLGA-NP） lyophilized powder. Methods The parameters of lyophilizing process were optimized. In addition, the types, concentration, and lyophilizing technology of supporting agent were tested by shape, color, and re-dispersion as indexes. And the quality assay of SCH- PLGA-NP lyophilized powder, such as shape, re-dispersion, pH value, morphology, diameter, re-dispersion, content, encapsulation efficiency, and drug loading of SCH-PLGA-NP lyophilized powder was investigated. Results The supporting agent of 10% manicol could prevent nanoparticles from aggregating very well. The optimal lyophilizing process was as follow： pre-cooled at -45 ℃ for 10 h, primary drying at - 25 ℃ for 5 h, secondary drying at -5 ℃ for 2 h, the third drying at 10 ℃ for 2 h, and the finally drying at 30 ℃ for 6 h. The shape and re-dispersion of SCH-PLGA-NP lyophilized powder were good. The pH value was 6.25, mean diameter and re-dispersion of SCH-PLGA-NP were 80. 2 nm and 0. 024 8, respectively, the encapsulation efficiency and drug loading of SCH-PLGA-NP lyophilized powder were 52.17 % and 28.73%, respectively. Conclusion This best preparation process is reasonable after repetition. The quality assay method above mentioned is simple and suitable to lyophilized powder with good repeatability, which could indicate its advantage.