Preparation process for compound of proto steroid soap oside and application thereof
A technology of steroidal saponins and compounds is applied in the field of two steroidal saponin compounds, which can solve the problems of single type of medicament and no known botanical fungicide.
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Embodiment 1
[0014] Embodiment one: crude extraction and separation of compound
[0015] Open arrow rhizome dry powder 3kg, soaked repeatedly with 95% and 9L methanol until the leachate was almost colorless, concentrated the methanol extract under reduced pressure to obtain 283g of brown paste, and washed the concentrate with 1500mL petroleum ether, chloroform and ethyl acetate in sequence Fractional extraction, concentrated under reduced pressure to obtain the extracts of each fraction, combined 15.5 g of ethyl acetate extract and chloroform extract, put it on a silica gel (100-200 mesh, 300 g) column, and carried out gradient gradient washing with a mixture of chloroform and methanol De, chloroform and methanol mixing ratio, the volume ratio is 9: 1 and 8: 1, receive as a fraction by 400mL, and carry out the in vitro biological activity tracking test to Phytophthora litchie by spore germination method, get 22-26 fraction 1.78g And 27-37 fraction 1.32g two active parts.
Embodiment 2
[0016] Embodiment two: the extraction and separation of compound I
[0017] The 22nd-26th fraction described in Example 1 was put on a silica gel (200-300 mesh, 60g) column, and eluted with chloroform and methanol. The volume ratio of chloroform and methanol was 8:1.5, and 50 mL was accepted as a fraction. In addition, the spore germination method was used to carry out the in vitro biological activity tracking test on Pythophthora litchie, and 0.37g of the active part of the 9-12 fraction was obtained. Put this active part on the reversed-phase silica gel (RP-18) column, elute with methanol and water mixed solution, methanol and water volume ratio are 8: 2, receive by 10mL as a cut, and use spore germination method to the peronospora of litchi The in vitro biological activity tracking test was carried out, and 0.11 g of the active part of the 11th-15th fraction was obtained. Put the active part on a gel (Sephadex LH-20) column, elute with tetrahydrofuran, receive 2 mL as a fr...
Embodiment 3
[0018] Embodiment three: the extraction and separation of compound II
[0019] Put the 27th-37th fraction described in Example 1 on a reverse-phase silica gel column (RP-18), elute with methanol and water mixture, methanol and water volume ratio 8:2, receive 10 mL as a fraction, and use spores The in vitro biological activity tracking test was carried out on Pythophthora litchie by germination method, and 852 mg of the active part of the 17th-30th fraction was obtained, which was compound II.
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Abstract
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