Berberine additive product, medicament containing the same and preparation thereof
An adduct, berberine technology, applied in the field of prodrugs, can solve the problems of limiting the application of berberine, bactericidal effect affecting the balance of intestinal flora, etc., to improve bioavailability, simple synthesis method, and reduce pathology The effect of hyperglycemia
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Embodiment 1
[0020] Add 40g of berberine hydrochloride, add 500ml of water, stir in a water bath at 60°C to make a suspension, take it out, let it cool to about 40°C, add about 60ml of 20% (g / ml) sodium hydroxide dropwise until the pH is 11-12 , put it in an ice bath to cool to room temperature, add 40ml of acetone dropwise under continuous stirring to obtain a yellow precipitate, filter it to dryness, wash with 5000ml of water to pH 6-7, and dry at 60°C. Recrystallized with acetone, the resulting product was used for solubility determination, structure analysis and purity determination.
[0021] 1. Solubility
[0022] The compound is yellow or yellow-brown powder, almost insoluble in water, slightly soluble in ethanol, slightly soluble in acetonitrile and acetone.
[0023] 2. Structural analysis
[0024] 2.1 Proton NMR spectrum is as follows (the solvent is deuterated dimethyl sulfoxide):
[0025] 1 H NMR, δ7.250 (1H, s, H-1), 6.850 (1H, d, J=8.1Hz, H-11), 6.755 (1H, s, H-4), 6.715 (1...
Embodiment 2
[0043] Take 30g of berberine hydrochloride, put it in a three-neck flask, install a stirrer in the middle mouth, install a reflux device in one mouth, add 200ml of water to the other side of the feeding mouth, start stirring, slowly add 30ml of acetone, and heat to 60°C in a water bath , so that the reflux. Prepare 36ml of 20% (g / ml) sodium hydroxide solution, add it dropwise slowly, and stir constantly. After the dropwise addition, stir for 2 hours. After the reaction is over, put it into cold water to cool it, and filter the crystals with a Buchner funnel. Wash with 4000ml of water and dry at 60°C to obtain acetone berberine adduct.
Embodiment 3
[0045]Take 30g of berberine hydrochloride, put it in a three-neck flask, install a stirrer in the middle mouth, install a reflux device in one mouth, add 200ml of water to the other side of the feeding mouth, start stirring, slowly add 38ml of methyl ethyl ketone, and heat in a water bath to 80°C , so that the reflux. Prepare 36ml of 20% (g / ml) sodium hydroxide solution, add it dropwise slowly, and stir constantly. After the dropwise addition, stir for 2 hours. After the reaction is over, put it into cold water to cool it, and filter the crystals with a Buchner funnel. Wash with 4000ml of water and dry at 60°C to obtain methyl ethyl ketone berberine adduct.
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