反应详情

温度

37 °C

20 g of the extract prepared in Example 1 was taken in 100 ml of 0.1M acetic acid buffer solution (pH 4.5) and 2.5 g of enzymes (0.5 g of hesperidinase, 0.5 g of naringinase, 0.5 g of cellulase, 0.2 g of β-glucuronidase, 0.5 g of β-galactosidase, 0.3 g of amyloglucosidase; supplied by Sigma) was added thereto. The solution was stirred in a water bath at 37° C. for 48 hours. When icariin completely disappeared by periodically confirming by thin layer chromatography, the reaction was finished by heating in hot water (80 to 100° C.) for 10 minutes. The reaction was concentrated under pressure to remove the solvent. The residue was added to ethanol (200 ml), stirred (3 times) and subjected to filtration to remove precipitated salts. The filtrate was concentrated under pressure to obtain a crude product, which was then separated by silica gel column chromatography (chloroform:methanol=8:1 to 4:1) to give 1.1 g of icaritin, 1.2 g of icariside 1 and 0.9 g of icariside II.

1. addition2.5 g of enzymes (0.5 g of hesperidinase, 0.5 g of naringinase, 0.5 g of cellulase, 0.2 g of β-glucuronidase, 0.5 g of β-galactosidase, 0.3 g of amyloglucosidase; supplied by Sigma) was added
2. concentrationThe reaction was concentrated under pressure
3. customto remove the solvent
4. additionThe residue was added to ethanol (200 ml)
5. stirringstirred (3 times)
6. filtrationsubjected to filtration
7. customto remove
8. customprecipitated salts
9. concentrationThe filtrate was concentrated under pressure
10. customto obtain a crude product, which
11. customwas then separated by silica gel column chromatography (chloroform:methanol=8:1 to 4:1)