Jiang Liyan, Lu Yanbin, He Shan, Pan Yuanjiang, Sun Cuirong, Wu Tianxing
Department of Chemistry, Zhejiang University, Hangzhou, PR China.
J Sep Sci. 2008 Dec;31(22):3930-5. doi: 10.1002/jssc.200800396.
High-speed counter-current chromatography (HSCCC) was applied to the preparative isolation and purification of two amides from Mallotus lianus Croiz. In a single HSCCC separation, using the two-phase solvent system composed of n-hexane/ethyl acetate/methanol/water (5:1:5:1 v/v), 247.5 mg of the enriched crude sample was separated to afford 10.3 mg of N-isobutyl-2E,4E,12Z-octadecatrienamide and 15.7 mg of (7Z,10Z,18Z)tricosa-7,10,18-trienamide, a novel compound, with the purities of 98.0 and 94.6%, respectively. The HSCCC fractions were analyzed by HPLC and chemical structures of the compounds were identified by 1D- and 2D-NMR, ESI-, and GC-MS.
高速逆流色谱法（HSCCC）被应用于从毛桐（Mallotus lianus Croiz.）中制备分离和纯化两种酰胺。在一次HSCCC分离中，使用由正己烷/乙酸乙酯/甲醇/水（5:1:5:1 v/v）组成的两相溶剂系统，将247.5 mg的富集粗样品进行分离，得到10.3 mg的N-异丁基-2E,4E,12Z-十八碳三烯酰胺和15.7 mg的（7Z,10Z,18Z）-二十三碳-7,10,18-三烯酰胺（一种新型化合物），纯度分别为98.0%和94.6%。通过HPLC对HSCCC馏分进行分析，并通过一维和二维核磁共振、电喷雾电离及气相色谱-质谱联用仪鉴定化合物的化学结构。
