乳香超微粉的制备工艺及理化性质研究

Preparation technology and physico-chemical characteristics of Olibanum ultramicro powders

目的优选乳香超微粉制备工艺,研究微粉化对乳香粉体理化性质与体外溶出等特性的影响。方法以超微粉收率为评价指标,单因素实验考察原粉末粒度、冷冻时间、辅药比及粉碎时间对乳香超微粉碎的影响;对比分析考察微粉化对粉体学性质(休止角、松密度、振实密度、压缩度)、有效成分的量(挥发油、乙酸辛酯及11-羰基-β-乙酰乳香酸)与溶出情况等的影响。结果优选得到乳香超微粉工艺为粉碎至细粉,冷冻4 h,辅药比1∶5、超微粉碎15 min。随粉碎度增加,乳香粉体休止角增大,松密度与振实密度减小,压缩度有增加的趋势,说明流动性降低;乳香挥发油中有效成分乙酸辛酯的量呈先增后降的趋势。溶出实验表明经优化工艺制备得到的超微粉中乙酸辛酯的量最高,11-羰基-β-乙酰乳香酸的累积溶出率明显比普通粉大。结论优选的乳香超微粉工艺可行,适度微粉化有利于乳香有效成分的提取与溶出。

Objective To optimize the technology and evaluate the influence of micronization on Olibanum physic-chemical characteristics and dissolution. Methods The single factor test was employed to investigate the effect of the size and freezing time of common powder particle, the ratio of excipients, and grinding time on the yield of ultramicro powder; Additionally a comparative research between ultramicro powder and common powder was designed, including micromeritic properties （angle of repose, bulk density, tap density, and squeezing degree）, effective components concentration [volatile oil, octyl acetate and 3-acetyl-11-keto-β- boswellic acid （AKBA）], and cumulative dissolution rate. Results The optimal technology of ultramicro powder was as follows： the medicinal material was ground into fine powder, followed by 4 h freezing at -20℃ and 15 min superfine grinding with excipient and fine powder in ratio of 1 ： 5; As the degree of smashing enhanced, the angle of repose of powders increased, bulk density and tap density decreased, and compressibility had a tendency of increase as flowability declined; The concentration of octyl acetate had an increased tendency and then decreased. While the concentration of octyl acetate in ultrafine powder prepared by optimal technology was the highest, the cumulative dissolution rate of AKBA in the ultramicro powder was higher than that in common powder. Conclusion The application of optimal superfine pulverizing technique to Olibanum is feasible, and appropriate degree of micronization is helpful for the extraction and dissolution of effective components in Olibanum.