A crystallization method for improving bulk density, fluidity and preparing non-agglomerated azithromycin

A technology of azithromycin and fluidity, which is applied in the field of increasing bulk density, fluidity and preparing non-agglomerated azithromycin crystals, which can solve the problems of small bulk density and poor fluidity, and achieve good fluidity, easy industrial production, and high purity high effect

Active Publication Date: 2021-05-04
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the serious coalescence phenomenon of the product prepared by this method, the bulk density is small and the fluidity is not good. The bulk density is between 0.42g / mL and 0.54g / mL, and the angle of repose representing fluidity is generally greater than 42°

Method used

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  • A crystallization method for improving bulk density, fluidity and preparing non-agglomerated azithromycin
  • A crystallization method for improving bulk density, fluidity and preparing non-agglomerated azithromycin
  • A crystallization method for improving bulk density, fluidity and preparing non-agglomerated azithromycin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 8g of azithromycin to 24g of ethyl formate, heat to 60°C and keep it warm until the azithromycin is completely dissolved, quickly cool down to 50°C at a cooling rate of 30°C / h, add 0.04g of azithromycin seed crystals with a total weight of 0.5%, and grow crystals at constant temperature 0.5h, control the cooling rate at 12.5°C / h and slowly drop to 0°C after 4h, filter the crystals, and dry to obtain the azithromycin product. The microscope photo of the product is attached figure 1 , it can be seen from the figure that the azithromycin crystal grows well without agglomeration; the bulk density of the tested particles is 0.65g / mL; the angle of repose is 32.8°; the purity reaches 99.72%.

Embodiment 2

[0030] Add 20g of azithromycin to 20g of ethyl acetate, heat to 90°C and keep it warm until the azithromycin is completely dissolved, then quickly cool down to 70°C at a cooling rate of 60°C / h, add 0.01g of azithromycin seed crystals with a total weight of 0.05%, and grow crystals at constant temperature 20min, control the cooling rate to 8°C / h and drop to 30°C after 5h, filter and dry the crystals to obtain azithromycin product, the microscopic photo of the product is attached figure 2 , it can be seen from the figure that the azithromycin crystals grow well without agglomeration; the bulk density of the tested particles is 0.63g / mL; the angle of repose is 33.4°; the purity reaches 99.65%.

Embodiment 3

[0032] Add 10g of azithromycin to 50g of methyl acetate, heat it to 50°C and keep it warm until the azithromycin is completely dissolved, then quickly cool down to 40°C at a cooling rate of 30°C / h, add 0.5g of 5% seed crystals of the total weight of azithromycin, and culture at constant temperature crystallize for 40 minutes, control the cooling rate to 17.5°C / h and drop to 5°C after 2h, filter and dry the crystals to obtain the azithromycin product, and the microscopic photos of the product show that the azithromycin crystals grow well without agglomeration. The particle size distribution of the product is attached image 3 As shown, it can be seen from the figure that the particles are in a unimodal distribution; the main particle size is about 200 microns; the bulk density of the tested particles is 0.60g / mL; the angle of repose is 34.0°; the purity reaches 99.69%.

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Abstract

The invention relates to a crystallization method for improving bulk density, fluidity and preparing non-agglomerated azithromycin. After heating the azithromycin and an ester organic solvent to dissolve at 40-90°C, the temperature is rapidly lowered at a cooling rate of 30-60°C / h to reach Saturated, add azithromycin seed crystals before crystal out, grow crystals, then slowly cool down to the crystallization end point temperature at a cooling rate of 5°C / h-25°C / h, filter the suspension, and dry to obtain azithromycin crystal products. The fluidity and bulk density of the prepared product are obviously better than the fluidity and bulk density of the product obtained by dissolving acetone and elution with water used in current industrial production. The bulk density of the product is as high as 0.59g / mL~0.65g / mL; the fluidity of the product is relatively good, and the angle of repose can be less than 34°; the purity of the product is as high as 99.6%. Moreover, the crystallization method of the present invention is the conventional cooling crystallization of a single solvent, the process is simple, and industrial production is easy to realize.

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 improving bulk density, fluidity and preparing non-agglomerated azithromycin 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 and protected in US patents US4517359 and US4474768. [0005] Hu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/00C07H1/06
CPCC07H1/06C07H17/00
Inventor 龚俊波吴送姑杜世超侯宝红陈明洋许史杰张得江
Owner TIANJIN UNIV
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