Zhang Shuting, Li Lingxi, Cui Yan, Luo Lanxin, Li Yuanyuan, Zhou Peiyu, Sun Baoshan
School of Pharmacy, Shenyang Pharmaceutical University, 110016 Shenyang, China; Department of Pharmacy, Jiamusi University, 154007 Jiamusi, China.
School of Pharmacy, Shenyang Pharmaceutical University, 110016 Shenyang, China; School of Functional Food and Wine, Shenyang Pharmaceutical University, 110016 Shenyang, China.
Food Chem. 2017 Mar 15;219:399-407. doi: 10.1016/j.foodchem.2016.09.170. Epub 2016 Sep 28.
Separation of plant proanthocyanidins remains a major challenge for scientists due to the structural diversity and complexity. In this work, a new and effective method was developed for preparative separation of grape seed proanthocyanidins (GSPs) according to degree of polymerization (DP) by high-speed counter-current chromatography (HSCCC). Under the optimized HSCCC conditions, GSPs could be separated into seven distinct fractions (F1-F7) with mean degree of polymerization in increasing order, from 1.44 to 6.95. High yields for these fractions (53.7, 12.2, 29.5, 30.2, 11.2, 50.8 and 169.8mg, respectively) were achieved by only one-step HSCCC of 400mg of GSPs. Further, seventeen individual proanthocyanidins, most of which are commercially not available, were efficiently isolated by re-chromatography on HSCCC or prep-HPLC; each of the isolated compounds presented high yields (7.1-78.9mg) and high purity (70.0-95.7%). The positive correlation was observed between DP and antioxidant activity of proanthocyanidins.
由于结构的多样性和复杂性，植物原花青素的分离仍然是科学家面临的一项重大挑战。在这项工作中，开发了一种新的有效方法，通过高速逆流色谱法（HSCCC）根据聚合度（DP）对葡萄籽原花青素（GSPs）进行制备分离。在优化的HSCCC条件下，GSPs可被分离成七个不同的组分（F1 - F7），平均聚合度按升序排列，从1.44到6.95。通过对400mg GSPs进行仅一步的HSCCC，这些组分分别获得了高产率（分别为53.7、12.2、29.5、30.2、11.2、50.8和169.8mg）。此外，通过在HSCCC或制备型高效液相色谱（prep - HPLC）上重新色谱分离，有效地分离出了十七种单独的原花青素，其中大多数在商业上无法获得；每种分离出的化合物都具有高产率（7.1 - 78.9mg）和高纯度（70.0 - 95.7%）。观察到原花青素的DP与抗氧化活性之间存在正相关。
