大孔树脂纯化宽叶缬草中缬草素工艺优化

以宽叶缬草中的缬草素提取物为原料，对选取的 5 种大孔吸附树脂进行静态吸附试验，确定 D101 树脂为最优吸附树脂。通过 D101 树脂吸附缬草素的上样量试验与动态洗脱试验，确定上样溶液中缬草素质量浓度为10.0mg/mL，上样体积为 20.0mL，洗脱体积为 4BV。采用三元二次通用组合试验，考察上样流速、洗脱流速和洗脱液甲醇体积分数对柱层析纯化缬草素效果的影响，建立大孔树脂柱层析纯化缬草素的数学模型，经回归与方差分析，对模型进行局部寻优得出最佳工艺条件为：上样流速 2.5BV/h、洗脱流速 1.7BV/h，甲醇体积分数 75%，纯化后缬草素理论得率为72.40%，验证值为(72.12 ± 0.1)%。

Purification of Valtrate from Valeriana officinalis L.var. latifolia Miq by Optimized Macroporous Resin Adsorption

The purpose of the present study was to evaluate the use of macroporous resin adsorption for purifying crude valtrate extract from Valeriana officinalis L.var. latifolia Miq. Five macroporous resins were tested for their static adsorption/desorption performance towards Valeriana officinalis L.var. latifolia Miq valtrate, and D101 resin was the selected adsorbent. The optimal values of sample concentration and sample loading amount were determined to be 10.0 mg/mL and 20 mL/13 g resin, respectively, and an amount of desorption solvent (aqueous methanol solution) of 4 BV was found enough to recover adsorbed valtrate. A quadratic general rotary unitized design involving 20 experiments of 3 variables at 5 levels combined with multiple regression analysis leading to a quadratic regression model was employed to deal with the effects of sample flow rate, desorption flow rate and methanol concentration in aqueous solution on valtrate recovery. The optimal values of the process conditions were found to be: sample flow rate 2.5 BV/h, desorption flow rate 1.7 BV/h and methanol concentration in aqueous solution 75%. Under the optimized conditions, the theoretical and experimental values of valtrate recovery from crude extract from Valeriana officinalis L.var. latifolia Miq were 72.40% and (72.12± 0.1)%, respectively.