反相制备液相色谱分离白花败酱草异戊烯基黄酮
白花败酱草,黄酮,制备色谱,,白花败酱草,黄酮,制备色谱,摘要,关键词,1引言,2实验部分,3结果与讨论,References
摘 要 用半制备型反相高效液相色谱(RPLC)对白花败酱草氯仿萃取物进行了分离制备。色谱柱为YWG C18 (200 mm × 10.0 mm i.d., 10 μm),流动相为乙腈∶水∶乙酸(55∶45∶1,V/V),检测波长280 nm,流速4.0 mL/min,进样750 μL (样品液浓度30 g/L)。在此条件下一次分离得到5个单体化合物,经理化反应和光谱分析分别鉴定为bolusanthol B(1), (2S)5, 7, 2′, 6′tetrahydroxy6lavandulylated flavanone(2),(2S)5, 2′, 6′trihydroxy2″, 2″dimethylpyrano \[5″, 6″∶6, 7\] flavanone(3),orotinin (4) 和orotinin5methyl ether(5)。其中2和3为新化合物,1、4和5为首次从败酱属植物中分离得到。关键词 白花败酱草,黄酮,制备色谱
Isolation and Purification of Prenylated Flavonoids from Patrinia Villosa Juss by Reversed Phase Preparative Liquid Chromatography
Peng Jinyong, Fan Guorong, Wu Yutian, Chen Hongyuan
(Shanghai Key Laboratory for Drug Metabolism, College of Pharmacy, The Second Military Medical University, Shanghai 200433)
(Institute of Analysis, Nanjing University, Nanjing 210000)
Abstract A semipreparative reversed phase liquid chromatography (RPLC) was used to isolate the chemical constituents from the chloroform extract of Patrinia villosa Juss. The separation condition was optimized as follows: the column was YWG C18 (10.0 mm × 200 mm i.d., 10 μm), the mobile phase was composed of CH3CNH2OHAC (55∶ 45∶2, V/V) at a flow rate of 4.0 mL/min, the detection wavelength and sample size were set at 280 nm and 750 μL (30 g/L). Under the optimized conditions, five compounds were isolated by RPLC in one run. Their chemical structures were identified as bolusanthol B (1); (2S)5, 7, 2′, 6′tetrahydroxy6lavandulylated flavanone (2); (2S)5, 2′, 6′trihydroxy2″, 2″dimethylpyrano \[5″, 6″: 6, 7\] flavanone (3); orotinin (4) and orotinin 5methyl ether (5) by spectroscopic methods including ultraviolet, infrared, electrospray mass spectromctry, 1D nuclear magnetic resonance (NMR) and 2D NMR techniques. Among them, compounds 2 and 3 were new compounds, and compounds 1, 4 and 5 were isolated from the P. genius for the first time. ......
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