One Step to Separate Five Alkaloids from Hypecoum leptocarpum by High-Speed Counter-Current Chromatography.
High-speed counter-current chromatography (CCC) was firstly and successfully applied for the preparative separation and purification of alkaloids from crude extract of Hypecoum leptocarpum. After the measurement of partition coefficient of five target alkaloids in the two-phase solvent systems, the CCC was performed well with a two-phase solvent system composed of tetrachloromethane-chloroform-methanol-0.1 M HCl at a volume ratio of 1.5 : 2.5 : 3 : 2 (V/V/V/V). The upper phase was used as the stationary phase, and the lower phase was used as the mobile phase. From 120 mg crude extract, 5 mg leptopidine, 32 mg oxohydrastinine, 27 mg (-)-N-methylanadine, 7 mg N-feruloyltyramine and 3 mg hypecoleptopine could be successfully separated. The amides alkaloid, N-feruloyltyramine, was firstly separated from H. leptocarpum. High-performance liquid chromatography analysis showed that the purity of each of the five target alkaloids was over 92%. Their chemical structures were confirmed by (1)H-NMR and (13)C-NMR data.
Key Laboratory of Tibetan Medicine Research, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, 23 Xin'ning Road, Xining 810008, China University of the Chinese Academy of Sciences, Beijing 100049, China.
Qiulong
Q
Zhang
Key Laboratory of Tibetan Medicine Research, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, 23 Xin'ning Road, Xining 810008, China University of the Chinese Academy of Sciences, Beijing 100049, China.
Tao
T
Ma
Key Laboratory of Tibetan Medicine Research, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, 23 Xin'ning Road, Xining 810008, China University of the Chinese Academy of Sciences, Beijing 100049, China.
Na
N
Hu
Qinghai Red Cross Hospital, Xining 810000, China.
Chenxi
C
Ding
Qinghai Nationalities University, Xining 810016, China.
Yongxin
Y
Liang
Key Laboratory of Tibetan Medicine Research, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, 23 Xin'ning Road, Xining 810008, China University of the Chinese Academy of Sciences, Beijing 100049, China.
Wencong
W
Li
Key Laboratory of Tibetan Medicine Research, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, 23 Xin'ning Road, Xining 810008, China.
Yourui
Y
Suo
Key Laboratory of Tibetan Medicine Research, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, 23 Xin'ning Road, Xining 810008, China Qinghai Nationalities University, Xining 810016, China Key Laboratory for Plateau Crop Germplasm Innovation and Utilization of Qinghai Province, Xining 810001, China cxding@nwipb.cas.cn.
Chenxu
C
Ding
D000470:Alkaloids / Q000302:isolation & purification*; D002251:Carbon Tetrachloride; D002725:Chloroform; D002851:Chromatography, High Pressure Liquid; D003373:Coumaric Acids / Q000302:isolation & purification*; D003377:Countercurrent Distribution / Q000295:instrumentation / Q000379:methods*; D006851:Hydrochloric Acid; D007546:Isoquinolines / Q000302:isolation & purification*; D000432:Methanol; D015394:Molecular Structure; D028101:Papaveraceae / Q000737:chemistry*; D010936:Plant Extracts / Q000737:chemistry*; D012997:Solvents; D014439:Tyramine / Q000031:analogs & derivatives* / Q000302:isolation & purification
D000470:Alkaloids; D003373:Coumaric Acids; D007546:Isoquinolines; D010936:Plant Extracts; D012997:Solvents; C000598487:leptopyrine; C074004:feruloyltyramine; D002725:Chloroform; D002251:Carbon Tetrachloride; D006851:Hydrochloric Acid; D014439:Tyramine; D000432:Methanol