Sodium fusidate novel crystal form and preparation method and application thereof

A technology for sodium fusidate and fusidic acid is applied in the field of drug crystals, can solve problems such as poor fluidity of sodium fusidate, and achieve the effects of good fluidity, environmental friendliness and low production cost

Inactive Publication Date: 2021-06-18
BEIJING ZHENDONG GUANGMING PHARMA RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The first object of the present invention is to provide a new crystal form of sodium

Method used

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  • Sodium fusidate novel crystal form and preparation method and application thereof
  • Sodium fusidate novel crystal form and preparation method and application thereof
  • Sodium fusidate novel crystal form and preparation method and application thereof

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preparation example Construction

[0034] The present invention also provides a preparation method for the new crystal form of sodium fusidate, comprising the following steps:

[0035] Fusidic acid is dissolved in an alcohol solvent at 25-40°C, and sodium methoxide is added to obtain a sodium fusidic acid solution;

[0036] Under the condition of 20-30°C, dichloromethane was added dropwise to the sodium fusidate solution, stirred for 0.5-4 hours, and the solid was collected by solid-liquid separation; the solid was dried to obtain sodium fusidate new crystal form.

[0037] As in different embodiments, fusidic acid can be dissolved in alcohol solvent at 25°C, 30°C, 35°C, 40°C and other conditions.

[0038] In a specific embodiment of the present invention, the ratio of the fusidic acid to the alcohol solvent is 1 g: (1-2) mL. This ratio means that the alcohol solvent is used in an amount of 1 to 2 mL per 1 g of fusidic acid solid. For example, when the amount of fusidic acid solid is 10g, the amount of alcoho...

Embodiment 1

[0057] This embodiment provides a preparation method for a new crystal form of sodium fusidate, comprising the following steps:

[0058] (1) Weigh 20g of fusidic acid solid and place it in a reaction vessel, add 20mL of anhydrous methanol, heat to 40°C to dissolve the fusidic acid solid, then add sodium methoxide solid under stirring to obtain fusidic acid Sodium solution 25mL;

[0059] The molar ratio of the added amount of the sodium methoxide solid to the fusidic acid solid is 1:1.

[0060] (2) Control the temperature at 20°C, under stirring, add dichloromethane dropwise to the sodium fusidate solution obtained in step (1), at a rate of 300mL / h (5mL / min), when dichloromethane When the dropwise addition amount is 600mL, stop the dropwise addition, and continue to stir for 0.5h, then filter with suction, place the filter cake at 40°C and dry for 36h to obtain 14.3g of sodium fusidate crystals, the calculated yield is 68.6% . Its purity was determined to be 98.83% by HPLC. ...

Embodiment 2

[0062] This embodiment provides a preparation method for a new crystal form of sodium fusidate, comprising the following steps:

[0063] (1) Weigh 20g of fusidic acid solid and place it in a reaction vessel, add 40mL of anhydrous methanol, heat to 40°C to dissolve the fusidic acid solid, then add sodium methoxide solid under stirring to obtain fusidic acid Sodium solution 45mL;

[0064] The molar ratio of the added amount of the sodium methoxide solid to the fusidic acid solid is 1:1.

[0065] (2) Control the temperature at 25°C and add 1200 mL of dichloromethane dropwise to the sodium fusidate solution obtained in step (1) under agitation at a rate of 300 mL / h (5 mL / min). Afterwards, stirring was continued for 1 h, and then suction filtered, and the filter cake was dried at 45° C. for 48 h to obtain 15.6 g of sodium fusidate crystals, with a calculated yield of 74.8%. Its purity was determined to be 99.66% by HPLC.

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Abstract

The invention relates to the technical field of medicine crystals, in particular to a sodium fusidate novel crystal form and a preparation method and application thereof. In an X-ray powder diffraction spectrogram of the novel crystal form, the sodium fusidate novel crystal form has characteristic peaks at the positions of 9.646 degrees, 10.882 degrees, 11.034 degrees, 13.840 degrees, 14.046 degrees, 16.577 degrees, 17.318 degrees, 17.687 degrees, 18.072 degrees, 19.868 degrees, 23.036 degrees, 25.489 degrees and 27.400 degrees as shown in 2 theta+/-0.2 degrees. The novel sodium fusidate crystal form prepared by the invention has the advantages of good fluidity, convenience in subpackage and preservation and the like, can be used for preparing a sodium fusidate injection, and is favorable for improving the medicine quality and the like.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical crystals, in particular to a new crystal form of sodium fusidate and a preparation method and application thereof. Background technique [0002] Sodium fusidate (Fusidate Sodium, trade name Lisidine) is the sodium salt of fusidic acid (Fusidate acid), which was first obtained from the fusidic acid lipid globules in the fermentation broth by Danish Leo Pharmaceutical Co., Ltd. in 1962. Extracted from fungi, it belongs to the class of fusidic acid antibiotics. [0003] Sodium fusidate is a brand-new antibiotic. Due to its good safety, low toxicity, rare allergic reactions, and anti-inflammatory coordinating effect, it is effective against other antibiotics (including vancomycin, teicoplanin, Can) uncontrollable MRSA, MRSE (methicillin-resistant Staphylococcus epidermidis) infection, especially effective. Sodium fusidate has a high clinical application value under the current situation of St...

Claims

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Application Information

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IPC IPC(8): C07J13/00A61K31/56A61P31/04A61K9/00
CPCA61K9/0019A61P31/04C07B2200/13C07J13/007
Inventor 吴自成雷飞桂星星
Owner BEIJING ZHENDONG GUANGMING PHARMA RES INST
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