【摘 要】
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Objective:To develop a high-speed counter-current chromatography (HSCCC) method for the systematic separation and purification of iridoid glycosides and crocetin derivatives on a preparative scale fro
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Objective:To develop a high-speed counter-current chromatography (HSCCC) method for the systematic separation and purification of iridoid glycosides and crocetin derivatives on a preparative scale from Gardenia.Method : After fractionation using HPD100 column chromatography, n-butanol ∶ ethanol∶ water (10∶1 ∶ 10, v/v) was selected to purify gardenoside, 6β-hydroxy geniposide and geniposidic acid from fraction A; ethyl acetate∶ n-butanol∶ water (2 ∶ 1.5∶3, v/v) was used to isolate geniposide from fraction B; crocin-1, crocin-2, crocin-3 and crocin-4 were purified by hexane∶ ethyl acetate∶ n-butanol ∶ water (1 ∶ 2 ∶ 1 ∶ 5, v/v) from fraction C.The head-to-tail elution mode was used with a flow rate of 8.0mL/min and a rotary speed of 600 rpm.Results : After HSCCC isolation,151.lmg of gardenoside,52.2mg of 6β-hydroxy geniposide and 24.5mg of geniposidic acid were obtained from 800mg of fraction A;587.2mg of geniposide was obtained from 800mg of Fraction B ;246.2mg of crocin-1,34.2mg of crocin-2,24.4mg of crocin-3 and 24.7mg of crocin -4 were obtained from 1000mg of fraction C.Their purities were found by UPLC analysis to be 91.7% ,93.4% ,92.5% ,98.2% ,94.1% ,96.3% ,94.1% and 98.9% respectively.Conclusion:The present results demonstrates that the main iridoid glycosides and crocetin derivatives in Gardenia can be obtained efficiently from extracts using HSCCC.
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