Purification of Four Flavonoid Glycosides from Lotus (Nelumbo nucifera Gaertn) plumule by Macroporous Resin Combined with HSCCC
Purification of Four Flavonoid Glycosides from Lotus (Nelumbo nucifera Gaertn) plumule by Macroporous Resin Combined with HSCCC
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大孔树脂结合HSCCC纯化荷花胚芽中四种黄酮苷
DOI：
10.1093/chromsci/bmx088
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发表时间：
2018
影响因子：
1.3
通讯作者：
Xu Gang
中科院分区：
文献类型：
--
作者：
Wu Lei;Xiong Wei;Hu Ju-wu;Gu Zhen;Xu Jian-guo;Si Chuan-ling;Bae Young-soo;Xu Gang
采用高速逆流色谱（HSCCC）结合大孔吸附树脂（MR）分离纯化中药莲子心中4种黄酮苷类化合物。采用高效液相色谱法（HPLC），以乙酸乙酯-正丁醇-水（1：2：3，v/v/v）为极性两相溶剂体系，以下层水相为移动的相，采用头-尾洗脱方式进行了制备规模的研究。在一步HSCCC分离中，从240 mg样品中获得槲皮素-3-O-β-D-吡喃葡萄糖苷（15 mg）、异鼠李素-3-O-β-D-吡喃葡萄糖苷（13 mg）、芹菜素6-C-β-D-吡喃葡萄糖基-8-C-α-L-吡喃阿拉伯糖苷（18 mg）和芹菜素6，8-二-C-β-D-吡喃葡萄糖苷（48 mg）。经HPLC测定，各化合物的纯度均在95%以上。通过电喷雾质谱（ESI-MS-MS）和核磁共振（NMR）方法鉴定了分离的化合物的化学结构。其中4个化合物均为首次从LP中分离得到。
High-speed counter-current chromatography (HSCCC) combined with macroporous resin (MR) column was successfully applied to the isolation and purification of four flavonoid glycosides from the medicinal herb Lotus plumule (LP). A polar two-phase solvent system composed of ethyl acetate–n-butanol–water (1:2:3, v/v/v) was selected by high-performance liquid chromatography (HPLC) and run on a preparative scale where the lower aqueous phase was used as the mobile phase with a head-to-tail elution mode. Quercetin-3-O-β-D-glucopyranoside (15 mg), isorhamnetin-3-O-β-D-glucopyranoside (13 mg), apigenin 6-C-β-D-glucopyranosyl-8-C-α-L-arabinopyranoside (18 mg) and apigenin 6,8-di-C-β-D-glucopyranoside (48 mg) were obtained in a one-step HSCCC separation from 240 mg of the sample. The purity of each compound was over 95% as determined by HPLC. Chemical structures of the isolated compounds were identified by electrospray ionization mass spectrometry (ESI–MS-MS) and nuclear magnetic resonance (NMR) methods. Moreover, the four compounds were isolated from LP for the first time.