Composition comprising salvianolate and application of composition
A salvianolic acid and substance technology, applied in the field of drug research and development, can solve the problems of poor chemical stability of salvianolic acid A, easy water absorption and deterioration, etc.
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Embodiment 1
[0042] Embodiment 1: the preparation of salvianolic acid compound
[0043] 1. Preparation of salvianolic acid A
[0044] Take 100g of Salvia miltiorrhiza powder, add 8 times the amount of water, warm soak at 80°C for 3 times, each time for 1 hour, filter, combine the filtrate, centrifuge at 4000 rpm for 10 minutes, take the supernatant and pass it through a 1400 macroporous adsorption resin column , wash with water until the sugar detection reaction is negative, then use 20% ethanol to elute to FeCl 3 If the reaction is negative, change it to 40% ethanol to elute until the FeCl3 reaction is negative, collect the eluate, concentrate under reduced pressure at 60°C until there is no alcohol smell, add hydrochloric acid to adjust the pH value to 3-5, and use a liquid of 1.5 Double the volume of ethyl acetate and extract 4 times, combine the ethyl acetate phases, concentrate the ethyl acetate extract under reduced pressure to an extract, and dry under vacuum at 60°C for 6 hours to...
Embodiment 2
[0047] Embodiment 2: the preparation of the metformin salt of salvianolic acid B
[0048] Method one: Metformin hydrochloride (17mg, 0.1mmol) is dissolved in 0.2 milliliters of water and it is added dropwise to the aqueous solution of 0.3 milliliters of salvianolic acid B (72mg, 0.1mmol), a large amount of solids are produced, then add sodium bicarbonate ( 8.4mmol, 0.1mmol) a large number of bubbles were generated, continue to stir for 5 minutes, and then add 1 ml of ethanol, the reaction solution becomes clear, then add acetone, a small amount of solid is precipitated out, the amount is very small.
[0049] Method two: Metformin hydrochloride (17mg, 0.1mmol) and sodium bicarbonate (8.4mg, 0.1mmol) were dissolved in 0.2 ml of water and added dropwise to the 0.3 ml aqueous solution of salvianolic acid B (72mg, 0.1mmol), Solids and bubbles are produced, continue to stir for 5 minutes, pour out the liquid phase, and dry the remaining brown oil to obtain a brown solid, send 1 H-N...
Embodiment 3
[0055] Embodiment 3: the preparation of the metformin salt of salvianolic acid A
[0056] Method 1: Add metformin hydrochloride (165.6mg, 1mmol) and potassium hydroxide (56mg, 1mmol) to 5ml of ethanol, stir at 40°C for 4 hours, filter, and dissolve salvianolic acid A (494mg, 1mmol) in 5ml of ethanol Add acetic acid (120mg, 2mmol) and add the filtrate to the above mixture. After the addition is complete, add ethyl acetate (100ml) and a large amount of solids will precipitate out. Stir for 10 minutes, let stand, pour out the liquid phase, and extract the solids Dry to obtain a bright yellow solid, which is sent to 1H-NMR for detection, and the spectrum shows that the purity of the above-mentioned salt is better (see attached Figure 6 ).
[0057] Method 2: Metformin hydrochloride (87mg, 0.5mmol) and potassium hydroxide (28mg, 0.5mmol) were added to 2.5ml of ethanol, stirred at 50°C for 2 hours, filtered, and the filtrate was set aside; salvianolic acid A (247mg, 0.5mmol) Disso...
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