Wang Li-Tao, Gao Ming-Zhu, Yang Qing, Cui Qi, Jian Yue, Fan Xiao-Hong, Yao Li-Ping, Fu Yu-Jie
The College of Forestry, Beijing Forestry University, Beijing, People's Republic of China.
Key Laboratory of Forest Plant Ecology, Ministry of Education, Northeast Forestry University, Harbin, People's Republic of China.
J Chromatogr Sci. 2019 Aug 16;57(8):738-744. doi: 10.1093/chromsci/bmz050.
Morus alba L. is a medicinal plant that contains a high amount of caffeoylquinic acids such as 3-caffeoylquinic acid (3-CQA), 5-caffeoylquinic acid (5-CQA) and 4-caffeoylquinic acid (4-CQA). This study aimed to establish a fast and efficient method for separating caffeoylquinic acids from mulberry leaves by using high-speed countercurrent chromatography coupled with macroporous resin. D101 resin showed better adsorption and desorption capacity for three caffeoylquinic acids among six macroporous resin adsorbents. The contents of 3-CQA, 5-CQA and 4-CQA reached for 4.77%, 18.95% and 9.84% through one cycle of D101 resin, which were 3.13-fold, 4.57-fold and 4.78-fold more than those in crude extracts, respectively. With a two-phase solvent system of ethyl acetate-water (1:1, V/V), >93% purity of target compounds were obtained in one cycle during 150 min with the recovery yields of 80.59%, 99.56% and 94.21% for 3-CQA, 5-CQA and 4-CQA, respectively. The structural identification of target compounds was carried out by ESI-MS, 1H NMR and 13C NMR spectra. The present result represented an easy and efficient separation strategy for the utilization of mulberry resource.
桑树是一种药用植物，含有大量的咖啡酰奎宁酸，如3 - 咖啡酰奎宁酸（3 - CQA）、5 - 咖啡酰奎宁酸（5 - CQA）和4 - 咖啡酰奎宁酸（4 - CQA）。本研究旨在建立一种利用高速逆流色谱结合大孔树脂从桑叶中分离咖啡酰奎宁酸的快速高效方法。在六种大孔树脂吸附剂中，D101树脂对三种咖啡酰奎宁酸表现出更好的吸附和解吸能力。通过D101树脂一个循环，3 - CQA、5 - CQA和4 - CQA的含量分别达到4.77%、18.95%和9.84%，分别比粗提物中的含量高3.13倍、4.57倍和4.78倍。在乙酸乙酯 - 水（1:1，V/V）的两相溶剂体系中，在150分钟的一个循环内获得了纯度>93%的目标化合物，3 - CQA、5 - CQA和4 - CQA的回收率分别为80.59%、99.56%和94.21%。通过电喷雾电离质谱（ESI - MS）、核磁共振氢谱（1H NMR）和核磁共振碳谱（13C NMR）对目标化合物进行了结构鉴定。本研究结果为桑树资源的利用提供了一种简便高效的分离策略。
