Preparation method of apigenin-7-O-beta-D-glucuronide, and use of apigenin-7-O-beta-D-glucuronide
A technology of glucuronide and apigenin, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problem of not finding the extraction of apigenin-7-o-β-D-glucuronide. methods, etc., to achieve simple operation and good effect.
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Embodiment 1
[0096] Apigenin-7-o-β-D-glucuronide preparation method, comprises the following steps:
[0097] Extraction: Weigh 10 kg of Kudiezi medicinal material, add 10 times the amount of 40% ethanol to the Kudiezi medicinal material, soak for 1 hour, reflux extraction twice, each time for 2 hours, combine the extracts, concentrate under reduced pressure at 60°C to obtain a concentration of 1.2 g / ml Concentrate Ⅰ;
[0098] Water precipitation: Add 6 times the amount of deionized water to the concentrated solution Ⅰ, dilute the concentration of the concentrated solution Ⅰ to 0.2g / ml, refrigerate at 4°C for 24 hours, filter, and use the filtrate for later use;
[0099]Purification: First, use macroporous adsorption resin I to purify, weigh 6.67kg of HZ820 macroporous adsorption resin according to the mass ratio of resin to crude drug of 1:1.5, pack the wet resin into a column, adjust the filtrate to pH3.5 with hydrochloric acid, and The filtrate was loaded with a sample concentration of ...
Embodiment 2
[0104] Apigenin-7-o-β-D-glucuronide preparation method, comprises the following steps:
[0105] Extraction: Weigh 20kg of Kudiezi medicinal material, add 15 times the amount of 70% ethanol to the Kudiezi medicinal material, soak for 3 hours, reflux extraction twice, each time for 2 hours, combine the extracts, concentrate under reduced pressure at 40°C to obtain a concentration of 0.8 g / ml Concentrate Ⅰ;
[0106] Water precipitation: add 3 times the amount of deionized water to the concentrated solution Ⅰ, dilute the concentration of the concentrated solution Ⅰ to 0.2g / ml, refrigerate at 10°C for 20h, filter, and use the filtrate for later use;
[0107] Purification: First, use macroporous adsorption resin I to purify. According to the mass ratio of resin to crude drug of 1:1.5, weigh 13.4kg of HZ820 macroporous adsorption resin, pack the wet resin into a column, and adjust the filtrate to pH 4.0 with hydrochloric acid. Load the filtrate with a sample concentration of 0.2g / ml...
Embodiment 3
[0112] Apigenin-7-o-β-D-glucuronide preparation method, comprises the following steps:
[0113] Extraction: Weigh 20kg of Kudiezi medicinal material, add 12 times the amount of 50% ethanol to the Kudiezi medicinal material, soak for 2 hours, reflux extraction twice, each time for 2 hours, combine the extracts, concentrate under reduced pressure at 50°C to obtain a concentration of 1.0 g / ml Concentrate Ⅰ;
[0114] Water precipitation: Add 4 times the amount of deionized water to the concentrated solution Ⅰ, dilute the concentration of the concentrated solution Ⅰ to 0.25g / ml, refrigerate at 6°C for 15 hours, filter, and use the filtrate for later use;
[0115] Purification: First, use macroporous adsorption resin I to purify. According to the mass ratio of resin to crude drug of 1:1.5, weigh 13.4kg of HZ820 macroporous adsorption resin, pack the wet resin into a column, and adjust the filtrate to pH 4.0 with hydrochloric acid. Load the filtrate with a sample concentration of 0....
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