响应面法优化黑木耳酸性多糖硫酸酯化制备工艺

Study on the Optimization of Acid Auricularia Auricular Polysaccharides Sulfate Esterification Process by Response Surface Methodology

前期研究发现,硫酸酯化黑木耳酸性多糖具有较好的生物活性,运用响应面法对黑木耳酸性多糖的最佳硫酸酯化工艺条件进行优化研究。研究了氯磺酸与N,N-二甲基甲酰胺的体积比、酯化试剂的体积含量、反应温度、反应时间、转速5个因素对黑木耳多糖硫酸酯化取代度的影响。利用最陡爬坡试验逼近因素的最大响应区域,采用Box-Behnken设计法对各因素的水平组合进行优化,获得黑木耳酸性多糖硫酸酯化优化条件:氯磺酸∶N,N-二甲基甲酰胺为1∶3.49、酯化试剂比例为33%、反应温度50℃、反应时间112.84 min、转速为200 r/min,在此优化条件下硫酸酯化黑木耳酸性多糖的取代度可达0.490 5。

Previous studies have found that＇sulfate esterification Auricularia auricular acidic-polysaccharides has good biological activity. Re- sponse surface methodology was adopted to optimize sulfuric acid esterification process conditions for Auricularia auricular polysaccharides. Effects of the volume ratio of chlorosulfonic acid and N, N- dimethyl formamide, the volume ratio of esterification reagent, the reaction tempera- ture, the reaction time, rotational speed on degree of substitution of the ulfatex acid esterification for polysaccharide of Aurieularia auricular were studied. The path of steepest ascent was used to define optimal response region for these three factors. Optimal level combinations of factors were obtained through Box-Behnken design. The optimal sulfuric acid esterification process conditions for polysaceharide of Aurieularia auricular were as follows ： the volume ratio of chlorosulfonic acid and N, N dimethyl formamide is 1： 3.49, the volume ratio of the esterifieation reagent is 33%, the reaction temperature is 50 ℃, the reaction time is 112.84 min, rotational speed is 200 r/min. Under optimal sulfuric acid esterification con- ditions, the DS of polysaccharide reached 0.490 5.