星点设计-效应面法优化荆芥穗黄酮类成分的提取工艺

目的: 优选荆芥穗黄酮类成分的提取工艺,为该药材的资源开发提供参考。方法: 选择乙醇体积分数、提取时间及乙醇用量为自变量,橙皮苷、木犀草素、芹菜素提取量的总评"归一值"为因变量,通过星点试验优选提取工艺,运用Design-Expert 8.0软件对自变量各水平进行多元线性回归和二项式拟合,利用效应面法优选提取工艺并进行预测分析。采用 HPLC测定橙皮苷、木犀草素、芹菜素含量,流动相乙腈(A)-0.4%磷酸溶液(B)梯度洗脱(0~20 min,5%~20%A;20~50 min,20%~30%;50~60 min,30%~5%A),检测波长283 nm。结果: 最佳提取工艺为加15倍量73%乙醇回流提取2次,每次2 h;橙皮苷、木犀草素、芹菜素提取量分别为3.991,1.307,0.589 mg·g^-1,总评"归一值"0.925 3,与预测值的偏差-2.14%。结论: 优选的提取工艺简单易行、准确度高,适用于荆芥穗总黄酮的工业化生产。

Optimization of Extraction Process for Flavonoids from Schizonepetae Spica by Central Composite Design-response Surface Methodology

Objective: To optimize extraction process of flavonoids from Schizonepetae Spica and provide a reference for development of this medicinal herb. Method: Ethanol concentration, the amount of ethanol and extraction time were selected as independent variables, overall desirability of extracting amounts of hesperidin, luteolin and apigenin as dependeng variable, data of overall desirabilities were fitted to a second-order polynomial equation and regressed by multiple linear, response surface methodology was used to optimize extraction technology and predictive analyze.HPLC was adopted to determine contents of hesperidin, luteolin and apigenin with mobile phase of acetonitrile-0.4% phosphoric acid solution for gradient elution and detection wavelength of 283 nm. Result: Optimal extraction technology was as following:extracted 2 times with 15-fold the amount of 73% ethanol for 2 h per time;extracting amounts of hesperidin, luteolin and apigenin were 3.991, 1.307, 0.589 mg·g^-1, respectively.Overall desirability was 0.925 3, whose deviation was -2.14% by comparing with the predictive value. Conclusion: This optimized extraction technology is convenient, accurate and suitable for industrial production of total flavonoids from Schizonepetae Spica.