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Preparation method of chlortetracycline hydrochloride

The technology of chlortetracycline hydrochloride and chlortetracycline, which is applied in the field of preparation of chlortetracycline hydrochloride, can solve the problems of high extraction cost and large pollution of chlortetracycline hydrochloride, and achieves a green and environment-friendly production process, is easy to operate, and has a simple crystallization process. Effect

Pending Publication Date: 2022-03-01
PUCHENG CHIA TAI BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the invention is to solve the problems of high extraction cost and large pollution of aureomycin hydrochloride in the prior art. The invention provides a preparation method of aureomycin hydrochloride. Crystallization kinetics, the preparation method of a kind of chlortetracycline hydrochloride of the present invention, is a kind of chlortetracycline hydrochloride extraction process that can make chlortetracycline hydrochloride product reach quality standard only once solvent crystallization, has reduced extraction greatly The amount of ethanol and hydrochloric acid required in the process of aureomycin hydrochloride not only greatly reduces the production cost, but also reduces the pollution to the environment

Method used

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  • Preparation method of chlortetracycline hydrochloride
  • Preparation method of chlortetracycline hydrochloride
  • Preparation method of chlortetracycline hydrochloride

Examples

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Embodiment 1

[0030] A preparation method of aureomycin hydrochloride, comprising the steps of:

[0031] 1) Cool 20L of chlortetracycline fermentation broth, lower the temperature to 20°C, add oxalic acid at a volume ratio of 2.0% (g / mL), adjust the pH to 1.1 with concentrated hydrochloric acid, and then use a weight-volume ratio of 0.15% (g / mL) Add yellow blood salt (sodium salt) and zinc sulfate to the above fermentation broth, wherein yellow blood salt and zinc sulfate are stirred for 25 minutes according to the weight ratio of 1:1, and then add flocculant according to the volume ratio of 0.5% (mL / mL) No. 1, stirred for 15 minutes, and the stirred fermentation broth was filtered through a plate frame to obtain 10L of acidified filtrate;

[0032] The No. 1 flocculant is selected from polyacrylamide polymers;

[0033] 2) Collect the 10L chlortetracycline acidification filtrate obtained in the previous step (using spectrophotometry to measure its chemical potency as 12300u / ml) and put it i...

Embodiment 2

[0045] A preparation method of aureomycin hydrochloride, comprising the steps of:

[0046] 1) Cool 300L of chlortetracycline fermentation broth, lower the temperature to 15°C, add oxalic acid at a volume ratio of 1.2% (g / mL), adjust the pH to 1.4 with concentrated hydrochloric acid, and then use a mass-volume ratio of 0.1% (g / mL) Add yellow blood salt (potassium salt) and zinc sulfate to the above fermentation broth, wherein yellow blood salt and zinc sulfate are stirred for 20 minutes according to the weight ratio of 1:1, and then add flocculant according to the volume ratio of 1.0% (mL / mL) No. 1, stirred for 10 minutes, and the stirred fermented liquid was filtered through a plate frame to obtain 150 L of acidified filtrate;

[0047] The No. 1 flocculant is selected from polyacrylamide polymers;

[0048] 2) Collect the 150L chlortetracycline acidification filtrate obtained in the previous step (using spectrophotometry to measure its chemical potency as 10000u / ml) and put it...

Embodiment 3

[0058] A preparation method of aureomycin hydrochloride, comprising the steps of:

[0059] 1) Cool 20L of chlortetracycline fermentation broth, lower the temperature to 18°C, add oxalic acid at a volume ratio of 1.5% (g / mL), adjust the pH to 1.2 with concentrated hydrochloric acid, and then use a weight-volume ratio of 0.2% (g / mL) Add yellow blood salt (sodium salt) and zinc sulfate to the above fermentation broth, wherein yellow blood salt and zinc sulfate are stirred for 30 minutes according to the weight ratio of 1:1, and then add flocculant according to the volume ratio of 0.8% (v / v) No. 1, stirred for 20 minutes, and the stirred fermented liquid was filtered through a plate frame to obtain 10 L of acidified filtrate;

[0060] The No. 1 flocculant is selected from polyacrylamide polymers;

[0061] 2) Collect the 10L chlortetracycline acidification filtrate obtained in the above step (using spectrophotometry to measure its chemical potency as 12000u / ml) and put it in the a...

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Abstract

The invention discloses a preparation method of chlortetracycline hydrochloride, which specifically comprises the following steps: acidification, purification, double salt precipitation and crystallization, a chlortetracycline hydrochloride extraction process capable of enabling a chlortetracycline hydrochloride product to reach the quality standard only by one-time solvent crystallization is adopted, and the dosage of ethanol, hydrochloric acid and the like required in the chlortetracycline hydrochloride extraction process is greatly reduced. Not only is the production cost greatly reduced, but also the pollution to the environment is reduced.

Description

technical field [0001] The invention belongs to the technical field of antibiotic extraction and synthesis of veterinary drugs, and in particular relates to a preparation method of aureomycin hydrochloride. Background technique [0002] Chlortetracycline hydrochloride belongs to tetracycline antibiotics. It is a salt formed by combining chlortetracycline and hydrochloric acid produced by Streptomycesaureofacieus fermentation. It is abbreviated as CTC.HCl. It is a broad-spectrum antibiotic widely used. attached image 3 shown. Chlortetracycline hydrochloride is the hydrochloride salt of chlortetracycline, which is golden yellow or yellow crystal, odorless, bitter in taste, gradually darkens when exposed to light, slightly soluble in water or ethanol, almost soluble in acetone, ether or chloroform It is insoluble. As a human medicine, it is mainly used to treat conjunctivitis and trachoma. As a veterinary medicine, it is mainly used to treat diseases such as typhoid fever and...

Claims

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Application Information

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IPC IPC(8): C07C231/24C07C237/26
CPCC07C231/24C07C2603/46C07C237/26
Inventor 陈浩然张向领黄小毛张君启吴新芝杨占英朱正江
Owner PUCHENG CHIA TAI BIOCHEM
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