Novel mangiferin calcium salts, the method for its preparation and its use
A technology of mangiferin calcium salt and mangiferin, which is applied in medical preparations containing active ingredients, pharmaceutical formulations, metabolic diseases, etc., can solve the problems of mangiferin solubility, bioavailability, absorption defects, etc., and achieves stable properties and yields. high effect
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preparation example 1
[0075] Preparation Example 1: Preparation of Mangiferin
[0076] 100kg Anemarrhena decoction pieces were extracted twice at 80°C with 80% ethanol, concentrated, adsorbed by macroporous resin, washed with water, eluted with 40% ethanol, and the eluate was concentrated under reduced pressure to obtain crude mangiferin. The crude mangiferin was purified by solvent-dioxane-water recrystallization to obtain pure mangiferin. The mangiferin sample was identified with the mangiferin reference substance, and the obtained sample was determined to be mangiferin. The purity was determined to be 98.5% by HPLC. .
[0077] Compound Identification:
[0078] 1 HNMR (DMSO-d 6 ) (δppm), 4.60 (1H, d, J=9.8Hz) is a glucose end group proton, and exists in the form of B-glycosidic bond; and 6.37 (1H, s), 6.86 (1H, s) and 7.39 (1H, s) Signal of 3 aromatic protons.
[0079] 13 CNMR (DMSO-d 6 )(δppm): 162.7(C-1), 108.4(C-2), 164.7(C-3), 94.2(C-4), 157.1(C-4a), 102.2(C-4b), 103.5(C -5), 154.9(C-...
Embodiment 1
[0084] Embodiment 1: the preparation of mangiferin monosodium salt
[0085]Add 42.2g (0.1mol) of mangiferin, 1800ml of water, and 600ml of ethanol into the reactor to fully suspend, add 8.4g (0.1mol) of sodium bicarbonate into water to make a 0.5% (w / v) solution, and slowly add the In the suspension, react until clarification, filter, add an appropriate amount of absolute ethanol-ethyl acetate (1:1.5v / v) to the solution, stir well, a large amount of precipitates precipitate, filter with suction, and dry the solid below 60°C , to obtain 31.2 g of mangiferin monosodium salt as light yellow solid, with a yield of 74.0%. The purity of the sample was determined to be 98.6% by HPLC.
Embodiment 2
[0086] Embodiment 2: the preparation of mangiferin monosodium salt
[0087] Add 42.2g (0.1mol) of mangiferin, 1800ml of water, and 900ml of ethanol into the reactor to fully suspend, add 5.30g (0.05mol) of sodium carbonate with water to make a 0.5% (w / v) solution, and slowly add the mixture in a stirring state. Suspension, react until clarification, filter, add a proper amount of acetone to the solution, stir well, a large amount of precipitate precipitates, filter with suction, dry the solid below 60°C, and obtain 31.4g of light yellow solid mangiferin monosodium salt, yield was 74.5%. The purity of the sample was determined to be 98.5% by HPLC.
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