Spherical crystal of spiramycin antibiotics and preparation method thereof

A technology of spiramycin and antibiotics, which is applied in the field of spherical crystals of spiramycin antibiotics and its preparation, and can solve the problem of no spherical crystals of spiramycins antibiotics and the like

Active Publication Date: 2020-09-22
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] However, there is no relevant technology on how to realize the spherical crystallization of spiramycin antibiotics at present.

Method used

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  • Spherical crystal of spiramycin antibiotics and preparation method thereof
  • Spherical crystal of spiramycin antibiotics and preparation method thereof
  • Spherical crystal of spiramycin antibiotics and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-7

[0060] Embodiment 1-7 implementation steps are:

[0061] 1) Weigh 1 g of acylated spiramycin sample raw material in a test tube with a stopper, transfer a certain amount of isopropanol (good solvent), shake, and completely dissolve into a yellow clear solution;

[0062] 2) Weigh K 2 HPO 4 , The auxiliary material HPMC is placed in the jacketed kettle, and 100 mL of water (poor solvent) is added to dissolve it, and the three-blade oblique blade is used to stir and set the rotating speed. Turn on the super constant temperature tank, set the temperature, and heat the jacketed kettle;

[0063] 3) When the temperature in the kettle is stable, pour the acylated spiramycin solution into the jacketed kettle at one time, the good solvent and the poor solvent form a quasi-emulsion, and the system becomes turbid;

[0064] 4) Stop stirring after crystal formation and aging. Filter to obtain pale yellow acylated spiramycin spherical crystals, wash and dry for 24h, collect and detect pa...

Embodiment 1

[0068] K in poor solvent 2 HPO 4 Choice of quality scores

[0069] During the spherical crystallization experiment, the pH of the aqueous phase was close to 9. At this time, the phosphorus element in the phosphate solution was replaced by HPO. 4 2- Form exists, which can hinder the ionization of acylated spiramycin in water. The solubility of acylated spiramycin in phosphate solution is as image 3 As shown, with the increase of phosphate content, the solubility of acylated spiramycin in phosphate aqueous solution decreased linearly. Therefore, during the preparation of spherical crystals, adding phosphate to the aqueous phase can reduce the loss of acylated spiramycin due to dissolution, thereby increasing the yield. like Figure 4 As shown, when the phosphate concentration in the solution reaches about 2%, the crystallization yield is significantly improved. Therefore, according to the research in this example, after the phosphate is added to the poor solvent, the con...

Embodiment 2

[0071] Choice of good solvent

[0072] Figure 5 for V 异丙醇 :V 水溶液 (mL / mL)=0.02, 0.03 Appearance and surface structure of acylated spiramycin spherical crystal products, the upper row of pictures is V 异丙醇 :V 水溶液 (mL / mL)=0.02 Appearance and surface structure of acylated spiramycin spherical crystal product, the bottom row of pictures is V 异丙醇 :V 水溶液 (mL / mL)=0.03 Appearance and surface structure of the spherical crystalline product of acylated spiramycin. Experiments show that the more isopropanol is used, the more "loose" product structure and the larger the particle size is.

[0073] When the volume ratio of the good solvent and the poor solvent is small, the average concentration in the droplet is higher than that when the solvent ratio is large, forming more dense spherical particles; on the contrary, when the volume ratio of the solution is large, the final spherical crystal product has larger internal voids. The surface hole structure is more obvious.

[0074] On th...

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Abstract

The invention relates to a preparation method of a spiramycin antibiotic spherical crystal. The preparation method comprises the following steps: mixing a good solvent dissolved with spiramycin antibiotics with a poor solvent, enabling the mixed solution to form an emulsion-like system under the emulsifying and stirring effects of auxiliary materials, gradually separating out the spiramycin antibiotics along with volatilization of the good solvent, and forming the spherical crystal. Compared with the prior art, the spiramycin antibiotic spherical crystal product provided by the invention has the mean particle size D43 of 200-400 microns, and the uniformity is 0.2 or higher.

Description

technical field [0001] The invention belongs to the technical field of drug crystallization, in particular to spherical crystals of spiramycin antibiotics and a preparation method thereof. Background technique [0002] Spiramycin antibiotics are a class of multi-component macrolide antibiotics, including a series of structurally similar spiramycin derivatives. The general chemical structure is as follows. figure 1 shown. Spiramycin antibiotics include spiramycin and acylated spiramycin, spiramycin and acylated spiramycin have similar molecular structures, and both contain two dimethylamine groups, but figure 1 Medium R 2 groups exist differently. Spiramycin antibiotics mainly include spiramycin, acylated spiramycin, and isoacylated spiramycin. The components and structural differences of common spiramycin antibiotics are shown in Table 1. [0003] Table 1 Components and structural differences of spiramycin antibiotics [0004] [0005] For such as figure 1 The spira...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06
CPCC07B2200/13C07H1/06C07H17/08
Inventor 陈葵蓝粤山武斌纪利俊吴艳阳朱家文
Owner EAST CHINA UNIV OF SCI & TECH
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