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Oxytetracycline hydrochloride preparation method

The technology of oxytetracycline hydrochloride and oxytetracycline base is applied in the field of preparation of oxytetracycline hydrochloride, which can solve the problems of low product quality and yield, long cooling crystallization time, and increase the impurity content of dehydrated oxytetracycline, so as to reduce impurities. The effect of generation, uniform crystal size

Inactive Publication Date: 2019-03-08
盐城市大丰区天生联合药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing technology has the following problems: 1. Oxytetracycline hydrochloride has different crystal forms and sizes, and the quality yield of the product is lower than 90%. The content of impurities such as toxin and β-apo-oxytetracycline

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0016] Take 1500L of methanol, 350Kg of oxytetracycline base, and 35Kg of calcium chloride, add oxytetracycline base and calcium chloride into methanol and adjust the temperature to about 30°C, stir evenly and filter to obtain the filtrate.

[0017] Then, the temperature of the filtrate was controlled within the range of 24-26° C., and a methanol solution of hydrochloric acid equivalent to 26 Kg of hydrogen chloride was added into the filtrate to obtain a mixed solution. The mixed solution was stirred intermittently to precipitate oxytetracycline hydrochloride. The intermittent stirring was specifically: the total stirring time was 4 hours, the stirring was carried out for 5 minutes every 30 minutes, and the stirring speed was 15-20 r / min.

[0018] After the intermittent stirring was finished, the temperature of the mixed solution was lowered to 0° C., and oxytetracycline hydrochloride was fully separated out. At this point, the mixed solution is centrifuged to obtain a wet pr...

Embodiment 2

[0023] Take 2100L of methanol, 500Kg of oxytetracycline base, and 50Kg of calcium chloride, add oxytetracycline base and calcium chloride into methanol and adjust the temperature to about 30°C, stir evenly and filter to obtain the filtrate.

[0024] Then, the temperature of the filtrate was controlled within the range of 21-23° C., and a methanol solution of hydrochloric acid equivalent to 26 Kg of hydrogen chloride was added to the filtrate to obtain a mixed solution. The mixed solution was stirred intermittently to precipitate oxytetracycline hydrochloride. The intermittent stirring was specifically: the total stirring time was 4 hours, the stirring was carried out for 5 minutes every 30 minutes, and the stirring speed was 10-15 r / min.

[0025] After the intermittent stirring was finished, the temperature of the mixed solution was lowered to 0° C., and oxytetracycline hydrochloride was fully separated out. At this point, the mixed solution is centrifuged to obtain a wet prod...

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Abstract

The invention discloses an oxytetracycline hydrochloride preparation method which comprises the following steps: 1, adding oxytetracycline and calcium chloride into methanol, uniformly stirring, and filtering to obtain filtrate, wherein oxytetracycline hydrochloride comprise the following raw materials: 1500-2100 L of methanol, 350-500 Kg of oxytetracycline and 35-50 Kg of calcium chloride; 2, controlling the temperature of the filtrate to 20-26 DEG C, adding a hydrochloric acid-methanol solution to obtain a mixed solution, and performing intermittent stirring on the mixed solution to separateout oxytetracycline hydrochloride, wherein the hydrochloric acid-methanol solution contains 26 Kg of hydrogen chloride; and 3, performing centrifugal separation on the mixed solution after the oxytetracycline hydrochloride is separated out, and drying, thereby obtaining the oxytetracycline hydrochloride. The oxytetracycline hydrochloride preparation method disclosed by the invention has the advantages that the mass yield of the oxytetracycline hydrochloride is stabilized at 96% or higher, and the content of impurities such as dehydrated mycin, alpha-apo-oxytetracycline, and beta-apo-oxytetracycline in the product is low.

Description

technical field [0001] The invention belongs to the field of pharmaceutical production methods, in particular to a preparation method of oxytetracycline hydrochloride. Background technique [0002] In the existing technology, the production process of oxytetracycline hydrochloride all selects methanol as a solvent, dissolves the raw material oxytetracycline base, and after filtering, adds methanol hydrochloride to form a salt; after nearly 10 hours of static cooling crystallization, centrifugation, soil Obtain oxytetracycline hydrochloride. [0003] The existing technology has the following problems: 1. Oxytetracycline hydrochloride has not yet had different crystal forms, and the quality yield of the product is lower than 90%. The content of impurities such as toxin and β-apo-oxytetracycline. Contents of the invention [0004] For solving the problems of the technologies described above, the invention provides a kind of oxytetracycline hydrochloride preparation method, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/26C07C231/12C07C231/24
CPCC07C231/12C07C231/24C07C2603/46C07C237/26
Inventor 陈隽楼彭广荣韦俊
Owner 盐城市大丰区天生联合药业有限公司
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