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Vernemulin hydrochloride hydrate crystal form, preparation method thereof, and pharmaceutical composition containing the crystal form

A technology of warnemulin hydrochloride and hydrate, which is applied in the field of crystallization of veterinary medicine and chemical engineering, can solve the problems of difficult industrialization of the crystallization process, unexplained no solvate, no improvement in bulk density, etc., and achieves simple operation steps and preparation process, No irritating smell, high bulk density effect

Active Publication Date: 2021-08-03
TIANJIN RINGPU BIO TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chinese patent CN108892629A proposes a preparation method of warnimulin hydrochloride methyl tert-butyl ether solvate, and prepares ansolvate from the solvate, but the bulk density of the ansolvate is only 0.305g / ml, which is heaped with amorphous matter Density did not improve compared to that, and it is unclear whether the resulting ansolvate was crystalline
However, the crystallization process in this invention is not easy to be industrialized, and although the crystalline compound has been improved to a certain extent on the hygroscopicity, the problem of its hygroscopicity still exists.

Method used

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  • Vernemulin hydrochloride hydrate crystal form, preparation method thereof, and pharmaceutical composition containing the crystal form
  • Vernemulin hydrochloride hydrate crystal form, preparation method thereof, and pharmaceutical composition containing the crystal form
  • Vernemulin hydrochloride hydrate crystal form, preparation method thereof, and pharmaceutical composition containing the crystal form

Examples

Experimental program
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Effect test

Embodiment 1

[0059] Take 10g of vernimulin hydrochloride raw material, add 30ml of methanol, then add 20ml of purified water, heat up to 40°C to dissolve, keep stirring for 1 hour, then slowly cool down to 5°C, stir and crystallize for 4h, filter; the filter cake is dissolved in 100ml Stir in n-hexane for 6 hours, and filter; the filter cake was vacuum-dried at 30°C to obtain 9.5 g of warnemulin hydrochloride hydrate, with a yield of 95%, a normalized purity of 99.63%, and a water content of 6.9%.

Embodiment 2

[0061] Take 10g of vonemulin hydrochloride crude drug, add 40ml of ethyl acetate, then add 50ml of purified water, heat up to 60°C to dissolve, keep stirring for 1 hour, then slowly cool down to 10°C, stir and crystallize for 8h, filter; the filter cake dissolves Stir in 150ml of n-heptane for 8h, filter; the filter cake was vacuum-dried at 40°C to obtain 9.2g of warnemulin hydrochloride hydrate, the weight yield was 92%, the purity was 98.8%, and the water content was 6.5%.

Embodiment 3

[0063] Take 10g of the crude drug of warnemulin hydrochloride, add 50ml of ethanol, then add 35ml of purified water, heat up to 55°C to dissolve, heat and stir for 1 hour, then slowly cool down to -5°C, stir and crystallize for 10h, filter; filter cake at 35°C After vacuum-drying at ℃ for 12 hours, place it above a saturated potassium nitrate aqueous solution (92.5% RH), and place it for 16 hours to obtain the 2.5 hydrate crystal form of warnemulin hydrochloride, with a water content of 6.8%;

[0064] At a temperature of 40°C, dry for 20 hours to constant weight to obtain the crystalline form of warnemulin hydrochloride 1.5 hydrate, with a water content of 4.6%;

[0065] Continue drying at 60° C. for 20 h to constant weight to obtain 8.9 g of 1.25 hydrate crystal form of warnemulin hydrochloride, with a yield of 89%, an HPLC purity of 98.9%, and a water content of 3.7%.

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Abstract

The invention relates to a crystal form of warnemuline hydrochloride hydrate, a preparation method thereof and a pharmaceutical composition containing the crystal form. Specifically, the present invention relates to the crystalline form of warnimulin hydrochloride hydrate, the characteristic peaks 2θ of the crystalline form in the X-ray powder diffraction spectrum are at 9.2±0.2°, 9.5±0.2°, 10.3±0.2°, 11.8±0.2 °, 12.3±0.2°, 12.8±0.2°, 15.1±0.2°, 17.5±0.2°, 18.2±0.2° display. The warnemulin hydrochloride hydrate crystal form has a large bulk density, no hygroscopicity and good stability. The present invention also provides a method for preparing the above-mentioned warnemuline hydrochloride hydrate crystal form and a pharmaceutical composition containing the crystal form, which can be used in the preparation of various preparations, such as soluble powder, oral liquid, sustained release Granules, injections and other dosage forms have broad prospects for clinical use.

Description

technical field [0001] The invention belongs to the technical field of veterinary medicine and chemical engineering crystallization, and in particular relates to a crystal form of warnemulin hydrochloride hydrate, a preparation method thereof and a pharmaceutical composition containing the crystal form. Background technique [0002] Valnemulin Hydrochloride, the English name is Valnemulin Hydrochloride, the molecular formula is C 31 h 52 N 2 o 5 S·HCl, with a molecular weight of 601.29, is a white powder and is irritating. Its structural formula is as follows: [0003] [0004] Wernimulin hydrochloride is a new generation of pleuromutilin semi-synthetic antibiotics, which belongs to diterpenes and is a special antibiotic for animals. bacterial infection. It is mainly concentrated in the lungs and is an ideal drug for treating various mycoplasma-induced lung diseases. Wernemulin interacts with the 50S subunit on the ribosome of pathogenic microorganisms, thereby inhi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/28C07C323/52A61K31/22A61P31/04
CPCC07C319/28C07C323/52A61P31/04C07B2200/13C07C2603/82
Inventor 李亚玲吴燕子王彪栗栖凤夏雪林刘爱玲李守军付春香
Owner TIANJIN RINGPU BIO TECH
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