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Method for directionally preparing theophylline-saccharin eutectic through membrane technology

A membrane technology, theophylline technology, applied in the field of preparation of theophylline-saccharin co-crystal, can solve the problem of not being able to obtain pure co-crystal

Inactive Publication Date: 2012-12-19
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Theophylline-saccharin co-crystals are typical asymmetric phase diagram systems in conventional solvents such as methanol and ethanol, and pure co-crystals cannot be obtained by solution evaporation

Method used

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  • Method for directionally preparing theophylline-saccharin eutectic through membrane technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Add 50ml of fresh Piranha solution into a large beaker, put the cut glass piece (20X20mm) into it, heat at a constant temperature of 70°C for 120 minutes, take out the glass piece, and wash with deionized water, isopropyl Wash carefully with alcohol, absolute ethanol and n-hexane, and dry to obtain hydroxylated glass flakes. Put the hydroxylated glass flakes into 60mL of 10mM aqueous solution containing 3-chloropropyltrimethoxysilane at room temperature, airtight Place it under the same conditions for 100 minutes to obtain a silanized glass sheet; wash the silanized glass sheet with fresh n-hexane, put it in anhydrous methanol for 10 minutes; wash it with anhydrous methanol, and dry it at 50°C 12h, a silane monomolecular self-assembled film was obtained on the surface of the glass sheet;

[0018] (2) Add 3.0g of theophylline and saccharin with a molar ratio of 1:1 into a container containing 100mL of methanol, heat to 50°C to dissolve all the solids; cool to 25°C, p...

Embodiment 2

[0021] (1) Add 50ml of fresh Piranha solution into a large beaker, put the cut glass piece (20X20mm) into it, heat at a constant temperature of 90°C for 90 minutes, take out the glass piece, and wash with deionized water, isopropyl Wash carefully with alcohol, absolute ethanol and n-hexane, and dry to obtain hydroxylated glass flakes. Put the hydroxylated glass flakes into 60mL of 15mM aqueous solution containing 3-aminopropyltrimethoxysilane at room temperature, airtight Place it under the same conditions for 150 minutes to obtain a silanized glass sheet; wash the silanized glass sheet with fresh n-hexane, put it in anhydrous methanol for 5 minutes; wash it with anhydrous methanol, and dry it at 80°C 8h, a silane monomolecular self-assembled film was obtained on the surface of the glass sheet;

[0022] (2) Add 4.0g of theophylline and saccharin with a molar ratio of 1:3 into a container containing 100mL of ethanol, heat to 50°C to dissolve all the solids; cool to 30°C, put T...

Embodiment 3

[0025] (1) Add 50ml of fresh Piranha solution into a large beaker, put the cut glass piece (20X20mm) into it, heat at a constant temperature of 80°C for 100 minutes, take out the glass piece, and wash with deionized water, isopropyl Wash carefully with alcohol, absolute ethanol and n-hexane, and dry to obtain hydroxylated glass flakes. Put the hydroxylated glass flakes into 60mL aqueous solution containing n-propyltrimethoxysilane with a concentration of 20mM at room temperature and under airtight conditions. Place it for 150 minutes to obtain a silanized glass sheet; wash the silanized glass sheet with fresh n-hexane, put it into anhydrous methanol for 20 minutes; wash it with anhydrous methanol, and dry it at 70°C for 10 hours. A silane monomolecular self-assembled film was obtained on the surface of the glass sheet;

[0026] (2) Add 5.0g of theophylline and saccharin with a molar ratio of 1:5 into a container containing 100mL of ethanol, heat to 50°C to dissolve all the sol...

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Abstract

The invention discloses a method for directionally preparing theophylline-saccharin eutectic through a membrane technology. The method comprises the steps of: 1) dipping a glass sheet in Piranha solution, heating the solution, taking out the glass sheet, washing the glass sheet, drying the glass sheet to obtain a hydroxylated glass sheet, placing the hydroxylated glass sheet in water solution containing silane coupling agent, and hermetically placing at room temperature to obtain a glass sheet with a silanized surface; and washing and drying the glass sheet to obtain a silane single-molecule self-assembled monolayer on the surface of the glass sheet; and 2) adding theophylline and saccharin into a container containing methanol or ethanol, heating to dissolve solids; and cooling the solution, placing the glass sheet with the single-molecule self-assembled monolayer on the surface, slowly evaporating solvent at constant temperature being 25-40DEG C, growing a large quantity of theophylline-saccharin eutectic crystals on the surface of the single-molecule self-assembled monolayer within 2-7 days, taking out the glass sheet on which the eutectic crystals grow, washing the glass sheet, and taking the theophylline-saccharin eutectic crystals down after the surface of the glass sheet is dried. According verification through XRD (X-Ray Diffraction), by adopting the method, pure theophylline-saccharin eutectic can be obtained within a wider concentration range.

Description

technical field [0001] The invention relates to a method for preparing co-crystals using film orientation technology, and belongs to the technical field of preparation of theophylline-saccharin co-crystals. Background technique [0002] As a new solid state of today's drugs, co-crystals have unique physicochemical properties and bioavailability that are different from traditional drugs. In fact, the selection of ligand molecules in the co-crystal of a specific system needs to follow the principle of similar solubility, that is, the solubility of ligand molecules should not be too much higher than that of the active ingredient of the drug. Otherwise, an asymmetric phase diagram would result. On the basis of fully understanding the phase equilibrium law of the two solutions, the asymmetrical phase diagram can be dealt with by solvent evaporation and suspension crystallization. However, this is what is known based on binary or ternary phase diagrams. Therefore, obtaining pur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/08C07D275/06
Inventor 党乐平冯寅年郭晶晶卫宏远
Owner TIANJIN UNIV
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