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Preparation method of ibuprofen-nicotinamide eutectic crystals

A technology of nicotinamide and co-crystal, which is applied in the field of preparation of ibuprofen-nicotinamide co-crystal of antipyretic and analgesic drug, can solve the problems of large consumption of organic solvent, long preparation time, low processing capacity, etc., and increase water solubility High performance, simple operation, and improved thermal stability

Active Publication Date: 2013-09-18
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the solubility of nicotinamide in methanol and ethanol is all small, and the solubility of ibuprofen-nicotinamide co-crystal in two solvents is all very large, so the yield of the co-crystal preparation process of this method is very low, about 23.4 %, and the consumption of organic solvents and energy is large, the preparation time is long, and the processing capacity is low

Method used

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  • Preparation method of ibuprofen-nicotinamide eutectic crystals
  • Preparation method of ibuprofen-nicotinamide eutectic crystals
  • Preparation method of ibuprofen-nicotinamide eutectic crystals

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Dissolve 18.00g of ibuprofen solid in 100ml of ethanol-water mixed solvent, ethanol / water=5 / 1 (ml / ml), and dissolve completely under stirring at 60°C, then add 10.66g of nicotinamide, and stir until fully reacted The solution is clarified and begins to cool down. The cooling rate is 8°C / hr, and crystal grains begin to appear at 20°C. Then, the temperature is cooled to 5°C, and the crystal is grown for 1hr. The magma was filtered and dried at 20° C. for 8 hr to obtain 16.04 g of white crystalline ibuprofen-nicotinamide cocrystals. The product has high crystallinity, large crystal size and smooth surface. The yield of the eutectic product is 55.96%, and the melting point is 94.0° C. The XRD spectrum of the eutectic product is as follows figure 2 , the scanning electron microscope photo as image 3 As shown, the differential scanning calorimetry spectrum is shown as Figure 4 shown.

Embodiment 2

[0026] Dissolve 19.60g of ibuprofen solid in 100ml of methanol-water mixed solvent, methanol / water=1 / 1 (ml / ml), and dissolve completely under stirring at 67°C, then add 10.89g of nicotinamide, and stir until fully reacted The solution is clarified and begins to cool down. The cooling rate is 10°C / hr. At 25°C, crystal grains begin to appear, then cool down to 0°C and grow crystals for 3hr. The crystal slurry is filtered and dried at 35°C for 10hr to obtain 21.34g white crystalline ibuprofen-niacinamide co-crystal. The product has high crystallinity, large crystal size and smooth surface. The yield of the eutectic product is 69.99%, and the melting point is 94.5°C.

Embodiment 3

[0028] Dissolve 25.00g of ibuprofen solid in 100ml of acetone-water mixed solvent, acetone / water=8 / 1 (ml / ml), and dissolve completely under stirring at 70°C, then add 16.67g of nicotinamide, and stir until fully reacted The solution was clarified and began to cool down at a cooling rate of 5°C / hr. Crystal grains began to appear at 15°C, then cooled to 2°C and grown for 1.5 hours. The crystal slurry was filtered and dried at 40°C under atmospheric pressure After 5 hours, 27.08 g of white crystalline ibuprofen-nicotinamide co-crystals were obtained. The product has high crystallinity, large crystal size and smooth surface. The yield of the eutectic product is 64.99%, and the melting point is 93.8°C.

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Abstract

The invention relates to a preparation method of ibuprofen-nicotinamide eutectic crystals. The preparation method comprises the following steps of: at the temperature of 70 to 60 DEG C, dissolving ibuprofen solids into a mixed solvent, wherein the concentration of the ibuprofen in the solution is 0.1 to 0.25g / ml, adding nicotinamide solids while stirring, wherein the mass ratio of ibuprofen to nicotinamide is (1.4:1) to (1.8:1), stirring, reacting fully until the solution is clear, reducing the temperature of the solution, wherein crystals start to separate at the temperature of 25 to 15 DEG C, then keeping on reducing the temperature to 0 to 5 DEG C, growing the crystals for 1 to 3 hours, filtering crystal pulp and drying, so as to obtain white ibuprofen-nicotinamide eutectic crystals. The dissolvability of the ibuprofen-nicotinamide eutectic crystals prepared by the preparation method is 158g / L in water, compared with the 100g / L dissolvability of the existing buprofen salts, the dissolvability is greatly improved, and the water solubility is increased accordingly; the preparation method is simple, the cost is low, and the quality is easy to control; the mass yield of the product is 56% to 70%.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical synthesis chemistry, and relates to a preparation method of an antipyretic and analgesic drug ibuprofen-nicotinamide co-crystal, which improves the water solubility of ibuprofen. Background technique [0002] Ibuprofen, molecular formula C 13 h 18 o 2 ; Niacinamide, the molecular formula is C 6 h 6 ON 2 , commonly known as vitamin B3, can be used to supplement nutrition and treat glossitis and dermatitis diseases. It is safe for human body and can be eaten; the molecular formula of ibuprofen-nicotinamide cocrystal is C 19 h 24 o 3 N 2 , the chemical structure is shown below. [0003] [0004] Ibuprofen is the No. 1 drug in the national non-prescription drug western medicine ingredient catalog announced by the State Drug Administration on July 24, 1999, and it is also the drug of choice recommended by the International Association Against Rheumatism. The curative effect of ibupr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/82C07C57/30
Inventor 尹秋响沈致名龚俊波侯宝红张美景王静康谢闯鲍颖王召周丽娜
Owner TIANJIN UNIV
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