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Purification method of oxytetracycline

A technology of oxytetracycline base and purification method, which is applied in the field of purification of oxytetracycline base, can solve the problems of low product yield and purity, cumbersome purification steps, high purification cost, etc., achieve good yield, improve purity, low cost effect

Inactive Publication Date: 2010-12-22
ZHENGZHOU HOUYI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has been used in production until now, the yield and purity of the product are both low, and the purification steps are relatively cumbersome, time-consuming and labor-intensive, and the cost of purification is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The purification method of the oxytetracycline base of the present embodiment, the steps are as follows:

[0021] 1) Add 30 g of oxytetracycline base to be purified into 150 ml of ethanol, add 1% hydrochloric acid by volume, and stir at 30°C for 5 minutes to completely dissolve;

[0022] 2) Cool the solution obtained in step 1) to 0°C, crystals are precipitated, and then filter;

[0023] 3) Dissolve the crystals obtained by filtering in step 2) with high-purity water 5 times its weight, then add saturated sodium bicarbonate solution dropwise to adjust the pH to 4, crystals precipitate, leave for 12 hours, and then filter;

[0024] 4) The crystals obtained by filtering in step 3) were vacuum-dried at 40° C. to obtain purified oxytetracycline base.

Embodiment 2

[0026] 1) Take 50 g of oxytetracycline base to be purified and add it to 500 ml of ethanol, add hydrochloric acid with a volume percentage of 1.5%, and stir at 40°C for 7 minutes to completely dissolve it;

[0027] 2) Cool the solution obtained in step 1) to 2°C, crystals are precipitated, and then filter;

[0028] 3) Dissolve the crystals obtained by filtering in step 2) with 8 times its weight in high-purity water, then add a saturated sodium bicarbonate solution dropwise to adjust the pH to 5, crystals are precipitated, place for 16 hours, and then filter;

[0029] 4) The crystal obtained by filtering in step 3) was vacuum-dried at 50° C. to obtain purified oxytetracycline base.

Embodiment 3

[0031] 1) Take 60 g of oxytetracycline base to be purified and add it to 700 ml of ethanol, add hydrochloric acid with a volume percentage of 1.8%, and stir at 50°C for 10 minutes to completely dissolve it;

[0032] 2) Cool the solution obtained in step 1) to 6°C, crystals are precipitated, and then filter;

[0033] 3) Dissolve the crystals obtained by filtering in step 2) with 10 times the weight of high-purity water, then add dropwise saturated sodium bicarbonate solution to adjust the pH to 6, crystals are precipitated, leave for 18 hours, and then filter;

[0034] 4) The crystal obtained by filtering in step 3) was vacuum-dried at 60° C. to obtain purified oxytetracycline base.

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Abstract

The invention discloses a purification method of oxytetracycline, comprising the following steps of: (1) adding the oxytetracycline to be purified to alcohol, then adding a hydrochloric acid solution and stirring for complete dissolution; (2) cooling the solution obtained in the step (1) to -4 to 8 DEG C to separate out crystals, and then filtering; (3) dissolving the crystals obtained by filtering in the step (2) in high-purity water, adding a sodium bicarbonate solution, regulating the pH to 4-8 to separate out the crystals, and then filtering; and (4) drying the crystals obtained by filtering in the step (3) to obtain the purified oxytetracycline. The alcohol and the high-purity water are respectively used as solvents, and two-time crystallization is carried out to the oxytetracycline by combining the steps of acidification and neutralization, thereby the method greatly improves the purity of the oxytetracycline.

Description

technical field [0001] The invention relates to a method for purifying oxytetracycline base. Background technique [0002] Oxytetracycline (Oxytetracycline base) is a broad-spectrum antibiotic, which not only has an effect on Gram-positive and negative bacteria, but also has inhibitory effects on Rickettsia, Mycoplasma and some protozoa. Oxytetracycline is mainly used as long-acting injection in veterinary clinics, which can reduce the frequency of medication, and the curative effect will not be affected when the total dose is reduced, and it can also reduce the stress on animals. The current domestic oxytetracycline extraction process is to use oxalic acid (or phosphoric acid) as an acidifier to adjust the pH value, use yellow blood salt-zinc sulfate as a purifying agent to remove protein and other polymer impurities, and then use 122 resin to decolorize and further purify the oxytetracycline filtrate , and finally adjust the pH to about 4.8 to crystallize to obtain the ox...

Claims

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Application Information

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IPC IPC(8): C07C237/26C07C231/24
Inventor 吴红云李小娜唐智坡
Owner ZHENGZHOU HOUYI PHARMA
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