Xiao Jun-Song, Liu Liang, Wu Hua, Xie Bi-Jun, Yang Er-Ning, Sun Zhi-Da
College of Food Science and Technology, Huazhong Agricultural University, Wuhan, PR China.
J Agric Food Chem. 2008 Mar 26;56(6):2096-101. doi: 10.1021/jf072679x. Epub 2008 Feb 26.
Research in the field of procyanidins is always hindered by the lack of procyanidin standards, and the preparation of procyanidins, especially in large scale, remains difficult and time-consuming. Commercial sources of procyanidin standards are scarce. In this study, a rapid preparation method of procyanidins by using low-pressure column chromatography was developed. Procyanidins in Granny Smith apples were extracted with boiled water and purified on an ADS-17 macroporous resin column to obtain a Granny Smith apple procyanidin extract (GSE). GSE was fractionated according to its degree of polymerization on a Toyopearl TSK HW-40s column. Procyanidins B2 (epicatechin-(4beta-8)-epicatechin) and C1 (epicatechin-(4beta-8)-epicatechin-(4beta-8)-epicatechin) were prepared without HPLC separation. Oligomeric procyanidins from Granny Smith apples were also identified by liquid chromatography-electrospray ionization-mass spectrometry.
原花青素领域的研究一直受到原花青素标准品缺乏的阻碍，而且原花青素的制备，尤其是大规模制备，仍然困难且耗时。商业来源的原花青素标准品稀缺。在本研究中，开发了一种使用低压柱色谱法快速制备原花青素的方法。用沸水提取澳洲青苹中的原花青素，并在ADS - 17大孔树脂柱上进行纯化，以获得澳洲青苹原花青素提取物（GSE）。GSE在Toyopearl TSK HW - 40s柱上根据其聚合度进行分级分离。无需高效液相色谱分离即可制备原花青素B2（表儿茶素 - (4β - 8) - 表儿茶素）和C1（表儿茶素 - (4β - 8) - 表儿茶素 - (4β - 8) - 表儿茶素）。还通过液相色谱 - 电喷雾电离 - 质谱法鉴定了澳洲青苹中的低聚原花青素。
