沙棘叶中鞣花酸的提取和纯化工艺研究

Study on the Extraction and Purification Process of Ellagic Acid from Sea Buckthorn Leaves

中文关键词:沙棘叶  鞣花酸  提取工艺  含量测定  大孔吸附树脂

keywords:seabuckthorn leaves  ellagic acid  extraction process  content determination  macroporous adsorption resin

中文摘要:目的：优化沙棘叶中活性成分鞣花酸提取工艺，并基于大孔吸附树脂建立鞣花酸的纯化方法，以提升鞣花酸的纯度。方法：采用高效液相色谱法，以沙棘叶中鞣花酸含量为评价指标，以提取方法、提取溶剂、提取时间、料液比为考察因素，通过单因素试验优化沙棘叶中鞣花酸的提取工艺。以大孔吸附树脂对沙棘叶中鞣花酸的吸附-解吸性能为评价指标，从大孔吸附树脂的3个型号（D101、AB-8、SP700）中筛选最佳型号，并对纯化条件（上样流速、除杂体积与洗脱体积）进行优化。结果：沙棘叶中鞣花酸最佳提取工艺为采用95%乙醇（含2 mol·L–1 HCl）为提取溶剂，料液比为1∶10，加热回流提取75 min。基于最佳工艺提取获得的沙棘叶中鞣花酸的含量比常规溶剂（95%乙醇）提取提高了约6倍。最佳大孔吸附树脂的型号为AB-8，最佳纯化条件为上样流速0.5 mL·min–1，采用30%乙醇4 BV除杂，75%乙醇（含0.1%甲酸）6 BV洗脱，在最佳纯化工艺条件下，鞣花酸的纯度为7.7%。结论：优化后的提取、纯化工艺稳定可行，可一定程度上提高沙棘叶中鞣花酸的纯度，为沙棘叶资源的高值化综合利用提供了参考。

Abstract:Objective: To optimize the extraction process of ellagic acid from sea buckthorn leaves and establish a purification method based on macroporous adsorption resin in order to improve the purity of ellagic acid. Methods: High-performance liquid chromatography (HPLC) was employed, and the content of ellagic acid in sea buckthorn leaves was used as the evaluation index. The extraction process was optimized through single-factor experiments by investigating extraction method, extraction solvent, extraction time, and solid–liquid ratio. The adsorption–desorption performance of macroporous adsorption resins toward ellagic acid was used as the evaluation criterion to screen the optimal resin type from three macroporous resins (D101, AB-8, and SP700). In addition, the purification conditions, including sample loading flow rate, impurity removal volume, and elution volume, were further optimized. Results: The optimal extraction conditions for ellagic acid from sea buckthorn leaves were as follows: 95 % ethanol containing 2 mol·L?1 HCl as the extraction solvent, a solid–liquid ratio of 1:10, and heat reflux extraction for 75 min. Under the optimized conditions, the extraction yield of ellagic acid was approximately six times higher than that obtained using the conventional solvent (95 % ethanol). Among the tested macroporous adsorption resins, AB-8 exhibited the best purification performance. The optimal purification conditions were determined as follows: sample loading at a flow rate of 0.5 mL·min-1, impurity removal with 4 bed volumes (BV) of 30 % ethanol, and elution with 6 BV of 75 % ethanol containing 0.1 % formic acid. The purity of ellagic acid obtained by the established purification process was 7.7 %. Conclusion: The optimized extraction and purification processes were stable and feasible, and could improve the purity of ellagic acid from sea buckthorn leaves to a certain extent, providing a reference for the high-value utilization of sea buckthorn leaf resources.