School of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou 450002, Henan, China.
Collaborative Innovation Center of Food Production and Safety, Zhengzhou 450002, Henan, China.
Molecules. 2019 Apr 2;24(7):1284. doi: 10.3390/molecules24071284.
We aimed to purify polyphenols from distiller's grain extract using macroporous resins and to identify its polyphenolic components. The influence of operational parameters on purification efficiency was investigated. The polyphenolic composition was analyzed by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) and then quantified by UPLC-MS using authenticated standards. The results showed that the optimal purifying conditions were D101 resin with a dosage of 3 g, four hours adsorption, three hours desorption time, and 60% ethanol as the eluent, producing the highest purification rate of 51%. The purified distiller's grain extract exhibited stronger antioxidant activity than the unpurified extracts, which was assessed using DPPH and ABTS methods (IC DPPH = 34.03 and 16.21 μg/mL, respectively; IC ABTS = 20.31 and 5.73 μg/mL, respectively). UPLC-MS results indicated that (-)-epicatechin is the major compound found in distiller's grain extract which was quantified as 562.7 μg/g extract, followed by ferulic acid (518.2 μg/g), -hydroxybenzoic acid (417.7 μg/g), caffeic acid (217.1 μg/g), syringic acid (158.0 μg/g) and quercetin (147.8 μg/g). Two compounds, vanillic acid (66.5 μg/g) and gallic acid (41.4 μg/g), were found in lower concentrations. The findings of this study suggest that purification of polyphenolic compounds from distiller's grain by macroporous resins is feasible, providing a new and effective method for the secondary use of distiller's grain resources.
本研究旨在利用大孔树脂从酒糟提取物中纯化多酚,并鉴定其多酚成分。考察了操作参数对纯化效率的影响。采用超高效液相色谱-串联质谱法(UPLC-MS/MS)分析多酚组成,并采用经认证的标准品通过 UPLC-MS 进行定量。结果表明,最佳纯化条件为 D101 树脂用量 3 g、吸附 4 h、解吸 3 h、60%乙醇为洗脱剂,可获得最高的纯化率 51%。与未纯化的提取物相比,纯化后的酒糟提取物表现出更强的抗氧化活性,这是通过 DPPH 和 ABTS 法评估的(IC DPPH = 34.03 和 16.21 μg/mL;IC ABTS = 20.31 和 5.73 μg/mL)。UPLC-MS 结果表明,(-)-表儿茶素是酒糟提取物中的主要化合物,其含量为 562.7 μg/g 提取物,其次是阿魏酸(518.2 μg/g)、-羟基苯甲酸(417.7 μg/g)、咖啡酸(217.1 μg/g)、丁香酸(158.0 μg/g)和槲皮素(147.8 μg/g)。两种化合物香草酸(66.5 μg/g)和没食子酸(41.4 μg/g)的含量较低。本研究结果表明,大孔树脂纯化酒糟中多酚化合物是可行的,为酒糟资源的二次利用提供了一种新的有效方法。