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A crystallization method for preparing azithromycin with millimeter-scale large particle size

A technology of azithromycin and large particle size, which is applied in the field of crystallization of azithromycin with millimeter-scale large particle size, can solve the problem of high product purity, achieve high product purity, realize industrial production, and have good fluidity

Active Publication Date: 2020-07-24
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the deficiencies of the above-mentioned technologies, the object of the present invention is to provide a crystallization method for preparing azithromycin with millimeter-scale large particle size. The prepared azithromycin crystalline product is a white crystal, and the shape of the product is a rhombic column with a pointed end, and the crystal does not aggregate. Monodispersed millimeter-sized large-size particles; product purity up to 99.8%; no breakage phenomenon; good bulk density, up to 0.58g / mL or more; good fluidity, angle of repose can be less than 36°; very easy to filter and drying; the elution crystallization method is adopted, the crystallization process is simple, the yield is high, and the product purity is high

Method used

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  • A crystallization method for preparing azithromycin with millimeter-scale large particle size
  • A crystallization method for preparing azithromycin with millimeter-scale large particle size
  • A crystallization method for preparing azithromycin with millimeter-scale large particle size

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Embodiment 1

[0026] Add 5g of azithromycin and 10g of acetone into a crystallizer with stirring, heat it to 50°C and keep it warm. After the azithromycin is completely dissolved, add 2.5g of water. After the system is stable, add 0.5% of the total weight of azithromycin Azithromycin crystals are used as crystal seeds , grow crystals at constant temperature for 30 minutes, slowly add 10 g of water dropwise, and the entire dropping time is controlled at about 5 hours, after adding water, filter and dry to obtain the product. The SEM photo of the product is attached figure 2 As shown in the figure, it can be seen from the figure that the particle size of a single crystal product is greater than 1.4 mm, and the particle size distribution of the product is uniform; the bulk density is 0.58g / mL; the angle of repose is 37.2°; the purity of the product detected by liquid phase is 99.7%.

Embodiment 2

[0028] Add 10g of azithromycin and 50g of acetone into a crystallizer with stirring, keep the temperature at 30°C and keep it warm. After the azithromycin is completely dissolved, add 20g of water. After the system is stable, add azithromycin crystals of 2% of the total weight of azithromycin as crystal seeds , grow crystals at constant temperature for 10 minutes, slowly add 60g of water dropwise, the whole dropping time is controlled at about 10h, after adding water, filter and dry to obtain the product. The SEM photo of the product is attached image 3 As shown, it can be seen from the figure that the particle size of a single crystal product is greater than 1.6 mm, and the particle size distribution of the product is uniform; the bulk density is 0.59g / mL; the angle of repose is 36.5°; the purity of the product detected by liquid phase is 99.8%.

Embodiment 3

[0030] Add 8g of azithromycin and 32g of acetone into the crystallizer with stirring, keep the temperature at 50°C and keep it warm. After the azithromycin is completely dissolved, add 12g of water. After the system is stable, add azithromycin crystals of 1% of the total weight of azithromycin as crystal seeds , grow crystals at constant temperature for 40 minutes, slowly add 40 g of water dropwise, the entire dropwise addition time is controlled at about 8 hours, after adding water, filter and dry to obtain the product. The SEM photo of the product is attached Figure 4 As shown, it can be seen from the figure that the particle size of a single crystal product is greater than 1.5 mm, and the particle size distribution of the product is uniform; the bulk density is 0.60 g / mL; the angle of repose is 37.9°; the purity of the product is 99.8% through liquid phase detection.

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Abstract

The invention relates to a crystallization method for preparing millimeter-level large-granularity azithromycin. An azithromycin crystal product is white crystal, a product morphology is in a prism shape, a cusp is arranged at one end of the prism shape, a bulk density of the azithromycin crystal product is better and can reach 0.58g / mL or more, fluidity of the azithromycin crystal product is good, and a repose angle of the azithromycin crystal product can be smaller than 36 degrees. The method comprises the steps: adding an azithromycin crude product and an acetone solvent into a crystallizerwith stirring to be heated and dissolved; adding water to reach supersaturation, then adding azithromycin seed crystal to grow crystal, then dropwise adding water to make the crystal grow, filteringthe crystal after the water is dropwise added and drying to obtain the azithromycin crystal product. The method utilizes a constant-temperature elution method, has simple technological processes and can obtain the millimeter-level large-granularity azithromycin product by controlling the seed crystal and crystal growth. The product has the advantages of large granularity, no broken phenomenon, high purity, high bulk density, good fluidity and easiness in achieving industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering and medicine, and in particular relates to a crystallization method for preparing azithromycin with millimeter-scale large particle size Background technique [0002] Azithromycin (9-deoxy-9α-aza-9α-methyl-9α-erythromycin A) is a third-generation macrolide antibiotic. The chemical structural formula is: [0003] [0004] Azithromycin kills bacteria by hindering the bacterial transpeptide process and inhibiting bacterial protein synthesis. It has a strong antibacterial effect on Gram-positive bacteria, some Gram-negative bacteria, chlamydia, mycoplasma, etc., and has a significant effect on respiratory tract infections. Azithromycin has high bioavailability, strong antibacterial activity in vivo, strong tissue penetration, significant curative effect, good safety and tolerance. Azithromycin is described in US patents US4517359 and US4474768. [0005] Human pharmacokinetics show ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/00C07H1/06
Inventor 龚俊波吴送姑陈明洋侯宝红杜世超张得江许史杰
Owner TIANJIN UNIV
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