Andrographolidi natrii bisulfis and preparation method thereof
A technology of sodium bisulfite and andrographolide is applied in the directions of pharmaceutical formulations, medical preparations containing active ingredients, antibacterial drugs, etc., which can solve the problems of increasing the difficulty of operation, increasing the cost and the like, and achieves good stability and impurities. Less, more pure effect
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Embodiment 1
[0018] Take andrographolide 6kg, and add 120L of 95% ethanol, heat and stir to dissolve, and maintain at 70°C; then take 2.2Kg of sodium bisulfite, add water to 73L, stir and dissolve; Pour the solution into the aqueous sodium bisulfate solution in step 2), mix evenly and heat to 70°C; then reflux for 36 minutes, recover the ethanol until there is no alcohol smell, and place it in a refrigerator at 1°C to 9°C for 12 to 48 hours. And extract 3 times with appropriate amount of chloroform, after filtration, concentrate the filtrate in vacuum; place the concentrated solution in step 3) in a crystallization pot with stirring paddle, cool with jacketed cooling water, stir with the paddle paddle at 3°C to 19°C and let stand Crystallize, then filter with suction, and dry the filter cake in vacuum to obtain white sodium bisulfite andrographolide adduct. Its purity is 99.6% as measured by liquid chromatography.
Embodiment 2
[0020] Weigh andrographolide 10kg, and add 145L of 95% ethanol, heat and stir to dissolve, and maintain at 80°C; then take 2.5Kg of sodium bisulfite, add water to 80L, stir and dissolve; Pour the solution into the aqueous solution of sodium bisulfate in step 2), mix evenly and heat to 85°C; then reflux for 30 minutes, recover the ethanol until there is no alcohol smell, and place it in a refrigerator at 1°C to 9°C for 12 to 48 hours. And extract 4 times with appropriate amount of chloroform, after filtration, concentrate the filtrate in vacuum; place the concentrated solution in step 3) in a crystallization pot with stirring paddle, cool with jacketed cooling water, stir with the paddle paddle at 3°C to 19°C and let stand Crystallize, then filter with suction, and dry the filter cake in vacuum to obtain white sodium bisulfite andrographolide adduct. Its purity is 99.8% as measured by liquid chromatography.
Embodiment 3
[0022] Weigh andrographolide 12kg, and add 165L of 95% ethanol, heat and stir to dissolve, and maintain at 85°C; then take 3.2Kg of sodium bisulfite, add water to 86L, stir and dissolve; Pour the solution into the aqueous solution of sodium bisulfate in step 2), mix evenly and heat to 65°C; then reflux for 36 minutes, recover the ethanol until there is no alcohol smell, and place it in a refrigerator at 1°C to 9°C for 12 to 48 hours. And extract 4 times with an appropriate amount of chloroform, after filtration, concentrate the filtrate in vacuum; place the concentrated solution in step 3) in a crystallization pot with a stirring paddle, cool with jacketed cooling water, stir with a paddle paddle at 3°C to 19°C and let stand Crystallization, suction filtration again, filter cake is vacuum-dried, obtains white sodium bisulfite andrographolide adduct, adopts liquid chromatography measurement to know that its purity is 99.74% (as figure 2 shown).
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