School Pharmaceutical Engineering, Shenyang Pharmaceutical University, Wenhua Road 103, Shenyang 110016, PR China.
Ultrason Sonochem. 2014 Mar;21(2):461-6. doi: 10.1016/j.ultsonch.2013.09.009. Epub 2013 Sep 18.
The objective of this study is to develop a process consisting of ultrasonic-assisted extraction, silica-gel column chromatography and crystallization to optimize pilot scale recovery of schisandrin B (SAB) from Schisandra chinensis seeds. The effects of five independent variables including liquid-solid ratio, ethanol concentration, ultrasonic power, extraction time, and temperature on the SAB yield were evaluated with fractional factorial design (FFD). The FFD results showed that the ethanol concentration was the only significant factor for the yield of SAB. Then, with the liquid-solid ratio 5 (mL/g) and ultrasonic power 600 W, the other three parameters were further optimized by means of response surface methodology (RSM). The RSM results revealed that the optimal conditions consisted of 95% ethanol, 60 °C and 70 min. The average experimental SAB yield under the optimum conditions was found to be 5.80 mg/g, which was consistent with the predicted value of 5.83 mg/g. Subsequently, a silica gel chromatographic process was used to prepare the SAB-enriched extract with petroleum ether/acetone (95:5, v/v) as eluents. After final crystallization, 1.46 g of SAB with the purity of 99.4% and the overall recovery of 57.1% was obtained from 400 g seeds powder. This method provides an efficient and low-cost way for SAB purification for pharmaceutical industrial applications.
本研究旨在开发一种工艺，包括超声辅助提取、硅胶柱色谱和结晶，以优化五味子种子中五味子醇甲（SAB）的中试规模回收。采用部分因子设计（FFD）评估了五个独立变量（液固比、乙醇浓度、超声功率、提取时间和温度）对 SAB 产率的影响。FFD 结果表明，乙醇浓度是影响 SAB 产率的唯一显著因素。然后，在液固比为 5（mL/g）和超声功率为 600 W 的条件下，通过响应面法（RSM）进一步优化了其余三个参数。RSM 结果表明，最佳条件为 95%乙醇、60°C 和 70 min。在最佳条件下，平均实验 SAB 产率为 5.80mg/g，与预测值 5.83mg/g 一致。随后，采用硅胶色谱法，以石油醚/丙酮（95:5，v/v）为洗脱剂，制备 SAB 富集提取物。最后结晶后，从 400g 种子粉中得到 1.46g 纯度为 99.4%、总收率为 57.1%的 SAB。该方法为医药工业应用中 SAB 的纯化提供了一种高效、低成本的方法。
