Zeng Hualiang, Liu Qi, Yu Jingang, Jiang Xinyu, Wu Zhiliang, Wang Meiling, Chen Miao, Chen Xiaoqing
College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China.
College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China; China Division of Physical Biology & Bioimaging Center, Shanghai Synchrotron Radiation Facility, Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Nov 1;1004:10-6. doi: 10.1016/j.jchromb.2015.09.017. Epub 2015 Sep 26.
A novel one-step separation strategy-tandem high-speed counter-current chromatography (HSCCC) was developed with a six-port valve serving as the switch interface. Nine structural analogues including three isomers were successfully isolated from Poria cocos (Schw.) Wolf. by one step. Compared with conventional HSCCC, peak resolution of target compounds was effectively improved in tandem one. Purities of isolated compounds were all over 90% as determined by HPLC. Their structures were then identified via UV, MS and (1)H NMR, and eventually assigned as poricoic acid B (1), poricoic acid A (2), 3β,16α-dihydroxylanosta-7, 9(11), 24-trien-21-oic acid (3), dehydrotumulosic acid (4), polyporenic acid C (5), 3-epi-dehydrotumulosic acid (6), 3-o-acetyl-16α-hydroxydehydrotrametenolic acid (7), dehydropachymic acid (8) and dehydrotrametenolic acid (9) respectively. The results indicated that tandem HSCCC can effectively improve peak resolution of target compounds, and can be a good candidate for HSCCC separation of structural analogues.
开发了一种新型的一步分离策略——串联高速逆流色谱法（HSCCC），以六通阀作为切换接口。通过一步从茯苓中成功分离出包括三种异构体在内的九种结构类似物。与传统的HSCCC相比，串联HSCCC有效提高了目标化合物的峰分辨率。通过高效液相色谱法测定，分离得到的化合物纯度均超过90%。然后通过紫外光谱、质谱和氢核磁共振对其结构进行鉴定，最终分别确定为茯苓酸B（1）、茯苓酸A（2）、3β,16α-二羟基羊毛甾-7,9(11),24-三烯-21-酸（3）、去氢土莫酸（4）、多孔酸C（5）、3-表-去氢土莫酸（6）、3-O-乙酰基-16α-羟基去氢栓菌酸（7）、去氢茯苓酸（8）和去氢栓菌酸（9）。结果表明，串联HSCCC能有效提高目标化合物的峰分辨率，可作为HSCCC分离结构类似物的良好选择。
