半制备型高效液相色谱法分离刺葡萄花色苷单体-食品科学.pdfVIP

※成分分析 食品科学 2016, Vol.37, No.18 71 半制备型高效液相色谱法分离刺葡萄花色苷单体 1 1,* 2 王维茜 ，邓洁红 ，刘永红 （1.湖南农业大学食品科技学院，湖南 长沙 410128 ；2.湖南生物机电职业技术学院，湖南 长沙 410127 ） 摘  要：经大孔吸附树脂HP-20纯化刺葡萄花色苷的粗提物后，以半制备型高效液相色谱法分离得到高纯度的刺葡 萄花色苷单体。以XCharge C18柱（20 mm ×250 mm ，10 μm）制备柱，考察梯度洗脱条件、流动相流速、进样量 对刺葡萄花色苷分离的影响，确定了最佳制备条件为甲醇-3% 甲酸溶液流动相梯度洗脱、流速15 mL/min、进样量 1.2 mL，实现了2 种主要花色苷单体的分离及制备。经超高效液相色谱- 四极杆飞行时间质谱鉴定，2 种花色苷单体 分别是锦葵素-3,5-O-双葡萄糖苷和锦葵素-3,5-O-双葡萄糖苷-香豆酰，产品纯度分别达到了99.54%和98.28% 。方法 具有简单易行、经济快速、易于放大等特点，适用于刺葡萄花色苷标准品的大规模制备。 关键词：刺葡萄；锦葵素；半制备液相色谱；超高效液相色谱- 四极杆飞行时间质谱 Vitis davidii Preparation of Monomeric Anthocyanins from Foex by Semi-Preparative HPLC 1 1,* 2 WANG Weiqian , DENG Jiehong , LIU Yonghong (1. College of Food Science and Technology, Hunan Agricultural University, Changsha 410128, China; 2. Hunan Biological and Electromechanical Polytechnic, Changsha 410127, China) Abstract: A semi-preparative high performance liquid chromatographic (HPLC) method using an XCharge C18 preparative column (20 mm × 250 mm, 10 μm) was established for the preparation of anthocyanins monomers with high purity from crude extracts of Vitis davidii Foex after purification with macroporous resin HP-20. The effects of experimental conditions including mobile phase gradient elution conditions, flow rate and injection volume were investigated on the separation efficiency of anthocyanins. The optimal chromatographic conditions were determined as follows: mobile phase, a mixture of methanol and 3% formic acid water for gra