正交试验法优选大黄中蒽醌类成分提取工艺

目的优化大黄中蒽醌类成分提取工艺。方法 HPLC法测定大黄药材中8个结合型蒽醌、5个游离型蒽醌共计13个原型蒽醌及总蒽醌质量分数,选用L_9(3~4)正交表,以乙醇体积分数、乙醇用量、提取时间和提取次数为考察因素,分别以总蒽醌、5个游离型蒽醌、8个结合型蒽醌提取率为考察指标,优化大黄总蒽醌、游离型蒽醌、结合型蒽醌提取工艺参数,并对优化的工艺进行放大验证试验。结果总蒽醌和游离型蒽醌最佳提取工艺为5倍量75%乙醇,回流提取5次,每次30 min,采用该工艺原型蒽醌类成分和总蒽醌提取率均在90%左右,游离型蒽醌提取率超过160%;结合型蒽醌最佳提取工艺为5倍量95%乙醇,回流提取3次,每次60 min,采用该工艺原型蒽醌类成分提取率接近90%,结合型蒽醌提取率超过80%。结论优化的工艺简单、稳定、可行,重复性好,可分别用于大黄中总蒽醌和游离型蒽醌、结合型蒽醌的提取。

Optimization of extract process of anthraquinones from Rhei Radix et Rhizoma by orthogonal test

Objective To optimize the extract process of anthraquinones from the Rhei Radix et Rhizoma (RRR). Methods The contents of eight bound anthraquinones (BAs) and five free anthraquinones (FAs), a total of 13 original anthraquinones, and total anthraquinones (TAs) in RRR were determined by HPLC. L₉(3⁴) orthogonal table was used, with ethanol concentration, solvent ratio, extract time, and number of extract as factors and extract quantity of TAs, five FAs, and eight BAs as the investigation index, respectively, the extract processes of TAs, FAs, and BAs from RRR were optimized. The optimized processes were verified by magnification test. Results The optimum extract process of TAs and FAs was as follows:five times of 75% ethanol, extracting five times by reflux, 30 min for each time. Using this process, the extraction rate for both original anthraquinones and TAs was about 90%, and FAs extraction rate was over 160%. The optimum extract process of BAs was as follows:five times of 95% ethanol, extracting three times by reflux, 60 min for each time. Using this process, original anthraquinones extraction rate was close to 90%, and the one of BAs was over 80%. Conclusion The optimized process is simple, stable, feasible, and repeatable, and can be used for the extraction of TAs, FAs, and BAs from RRR, respectively.