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Dihydrate azithromycin sphaerocrystal and preparation method thereof

A technology of azithromycin and spherical crystals, which is applied in the field of spherical crystals of azithromycin dihydrate and its preparation, and achieves the effects of low equipment requirements, good fluidity and easy operation.

Active Publication Date: 2018-10-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But for azithromycin, no patents and documents have been found to report on its spherical crystal preparation process, so the present invention has important practical value for the production of azithromycin

Method used

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  • Dihydrate azithromycin sphaerocrystal and preparation method thereof
  • Dihydrate azithromycin sphaerocrystal and preparation method thereof
  • Dihydrate azithromycin sphaerocrystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 80g of azithromycin solid to a mixed solvent of 75g of acetone and 25g of ethyl acetate, then raise the temperature to 40°C, set the stirring rate to 1000rpm, and add 200g of deionized water dropwise at 10g / min after the azithromycin is completely dissolved, and then Crystals began to precipitate slowly and gradually formed spherical particles. After the dropwise addition, the crystals were grown at a constant temperature and stirred for 30 minutes, and finally the crystal slurry was filtered with suction. After the filter cake was dried in vacuum at 50°C to constant weight, spherical azithromycin dihydrate was obtained product. The product purity that this method obtains is 99.3%, and the one-way molar yield of crystallization process is 91.5%, and the X-ray powder diffraction pattern of product is as follows figure 2 As shown, the thermal analysis diagram of the product is shown in image 3 , the product looks like Figure 4 As shown, the main particle size is ...

Embodiment 2

[0032] Add 50 g of azithromycin solid into a mixed solvent of 60 g of ethanol and 40 g of isopropyl acetate, set the stirring rate at 800 rpm, keep the temperature at 30° C., and add 250 g of deionized water dropwise at 10 g / min after the azithromycin is completely dissolved. During the process of adding water dropwise, the solution changes from clarification to turbidity and crystals are gradually precipitated out, finally forming spherical particles. After the dropwise addition, grow the crystals at a constant temperature and stirring for 60 minutes, then suction filter the crystal slurry formed, and filter the filter cake at 50 After drying at ℃ to constant weight, the product of spherical azithromycin dihydrate is obtained. The purity of the product obtained by the method is 99.2%, and the single-pass molar yield in the crystallization process is 91.1%, and the appearance of the product is as follows: Figure 5 As shown, the main particle size is 1mm, the particle size dis...

Embodiment 3

[0034]Add 50 g of azithromycin solid into a mixed solvent of 50 g of acetone and 50 g of ethyl acetate, raise the temperature to 30° C., set the stirring rate at 500 rpm, and add 300 g of deionized water dropwise at 10 g / min after the azithromycin is completely dissolved. The crystals began to precipitate slowly, and gradually formed spherical crystals. After the dropwise addition, the crystals were grown at a constant temperature and stirred for 90 minutes, and then the crystal slurry was filtered with suction. After the filter cake was dried at 55°C to constant weight, the spherical azithromycin dihydrate product was obtained. . The product purity that this method obtains is 99.2%, and the one-way molar yield of crystallization process is 90.5%, and product outward appearance is as Figure 6 As shown, the main particle size is 2mm, the particle size distribution is uniform, the angle of repose is 20°, and the product has good fluidity.

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Abstract

The invention relates to a dihydrate azithromycin sphaerocrystal and a preparation method thereof. The sphaerocrystal is high in circular degree and large in particle size, has the diameter reaching to 0.5mm to 4mm, is good in fluidity, and has an angle of repose being 17 degrees to 23 degrees. The method comprises the steps of adding azithromycin solids into a mixed solvent of a good solvent anda bridging agent, then heating to 20 DEG C to 40 DEG C, fully dissolving the solids, adding water for crystallizing under the stirring action, after adding water, growing the grain for 30 to 90min atconstant temperature, then filtering a crystal mush, vacuum drying a filter cake at 50 to 60 DEG C to constant weight to obtain the dihydrate azithromycin sphaerocrystal. The particle size of the product is uniform, the particle size can reach 0.5 to 4mm, the angle of repose is 17 degrees to 23 degrees, and the fluidity is good. The dihydrate azithromycin sphaerocrystal provided by the invention is simple in process flow, has low requirement on equipment, is large in product particle size, high in purity and good in fluidity, can be directly used for tableting, and is easy to realize industrial production.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical crystal separation, and in particular relates to a spherical crystal of azithromycin dihydrate and a preparation method thereof. Background technique [0002] Azithromycin (Azithromycin) is a macrolide antibiotic widely used in clinical treatment and is a broad-spectrum antibacterial drug. It is white or off-white powder, easily soluble in methanol, absolute ethanol, acetone, ethyl acetate or acidic conditions, almost insoluble in water. Melting point 113-115°C, chemical formula C 38 h 72 N 2 o 12 , molecular weight 748.88, chemical structural formula: [0003] [0004] Azithromycin is mainly used clinically for diseases such as respiratory tract infection, urinary system infection, skin and soft tissue infection. It is a drug obtained by modifying the structure of erythromycin. It has a similar antibacterial mechanism to erythromycin, but its antibacterial effect is stronger than ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/00C07H1/06
CPCC07B2200/13C07H1/06C07H17/00
Inventor 郝红勋陈奎侯宝红徐昭黄欣尹秋响王永莉鲍颖谢闯王召
Owner TIANJIN UNIV
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