牡丹籽粕中黄酮类化合物的提取工艺优化及膜法分离纯化

Optimization of Extraction Process and Purification of Flavonoids from Peony Seed Meal by Membrane Method

本研究采用微滤-纳滤二级膜分离的方法对牡丹籽粕中的黄酮类化合物进行分离提纯。通过单因素实验研究料液比、提取温度、乙醇体积分数和提取时间对总黄酮提取量的影响,在单因素的基础上采用响应面法对提取工艺进行优化及验证。选用聚偏二氟乙烯(PVDF)、聚醚砜(PES)、聚四氟乙烯(PTFE)、聚丙烯(PP)、混合纤维素(MCE)、聚丙烯腈(PAN)、水系醋酸纤维(CA)和聚酰胺(PA)8种材料微滤膜对牡丹籽粕黄酮类化合物(PSMF)提取液进行初级分离。纳滤膜为实验室自制的有机硅/PA复合膜。结果表明,PSMF最佳的提取条件为料液比1:15 g/mL,提取温度50℃,乙醇体积分数为70%,提取时间为30 min,PSMF提取量为(240.28±2.25)μg/mL。将粗提液稀释10倍用于比较8种不同微滤膜对于PSMF粗提液的过滤效果,发现PA膜具有较好的分离效果,复合膜对PSMF存在较好的纯化效果,且分离后黄酮水溶性提升至90%以上。经过800℃煅烧之后,原料液的残余质量为1.43%,PA膜分离液的残余质量为0.76%,BTESE/PA复合膜降至0.26%,杂质更少纯度较高。对比其分离前后的抗氧化活性,分离后的·OH、DPPH·清除率以及还原力有所提升,O_(2)^(−)·清除率由79.94%下降至64.82%。本研究对牡丹籽粕中的活性成分进行分析,PSMF是一种新型的植物黄酮资源,组成丰富,具有一定的研究空间。

In this study,the flavonoids in peony seed meal were separated and purified by microfiltration-nanofiltration secondary membrane separation method.The effects of material-liquid ratio,extraction temperature,ethanol volume fraction and extraction time on the extraction amount of total flavonoids were investigated by single-factor experiments,and the extraction process was optimized and validated by response surface methodology on the basis of single factors.Eight types of microfiltration membranes,including polyvinylidene fluoride(PVDF),polyethersulfone(PES),polytetrafluoroethylene(PTFE),polypropylene(PP),mixed cellulose(MCE),polyacrylonitrile(PAN),aqueous acetate(CA)and polyamide(PA),were selected for the primary separation of PSMF extracts.The nanofiltration membranes were homemade organosilicon/PA composite membranes in the laboratory.The results showed that the optimum extraction conditions for PSMF were 1:15 g/mL,50℃,70%ethanol volume fraction,30 min,(240.28±2.25)μg/mL of PSMF extraction amount.The PA membrane had a better separation effect,and the composite membrane had a better purification effect on PSMF,and the water solubility of flavonoids was increased to more than 90%after separation.After calcination at 800℃,the residual mass of the raw material solution was 1.43%and that of the PA membrane separation was 0.76%,and the BTESE/PA composite membrane was reduced to 0.26%,with fewer impurities and higher purity.Comparing its antioxidant activity before and after separation,the·OH,DPPH·scavenging rate and reducing power were improved after separation,and the O_(2)^(−)·scavenging rate decreased from 79.94%to 64.82%.In this study,the active components in peony seed meal were analyzed.PSMF would be a novel phytoflavonoid resource with rich composition and certain research space.