Preparation method of oxytetracycline hydrochloride

The technology of oxytetracycline hydrochloride and oxytetracycline base is applied in the field of preparation of oxytetracycline hydrochloride, which can solve the problems of high production cost, poor fluidity and high apparent density, and achieves low cost, good fluidity, The effect of high apparent density

Inactive Publication Date: 2015-11-25
HEBEI SHENGXUE DACHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention provides a kind of preparation method of oxytetracycline hydrochloride in order to solve the technical problems of environmental pollution, high production cost and poor fluidity caused by a large amount of methanol solvent used in the preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A. Dissolving: Add 50g of oxytetracycline base to 350mL of ethanol, then add 3.85mL of hydrochloric acid-ethanol mixed solution, stir, heat to 41°C until completely dissolved, and obtain a mixed solution;

[0028] B, active carbon decolorization treatment: add 0.1g active carbon in the mixed solution that step A obtains, filter, obtain oxytetracycline ethanol solution;

[0029] C. Crystallization by cooling: add 5 mL of concentrated hydrochloric acid to the oxytetracycline ethanol solution obtained in step B, stir, cool to 6° C. to crystallize, filter after 1.5 h, wash the filter cake with 6° C. ethanol, and obtain oxytetracycline hydrochloride wet product;

[0030] D. Drying: The wet product of oxytetracycline hydrochloride obtained in step C was dried in a vacuum drying oven at 60° C. for 6 hours to obtain 48 grams of finished product of oxytetracycline hydrochloride, which was tested to meet the standards of the Chinese Pharmacopoeia.

[0031] The above-mentioned emb...

Embodiment 2

[0035] A. Dissolving: Add 50g of oxytetracycline base to 405mL of ethanol, then add 4.5mL of hydrochloric acid-ethanol mixed solution, stir, heat to 43°C until completely dissolved, and obtain a mixed solution;

[0036] B, active carbon decolorization treatment: add 0.16g active carbon in the mixed solution that step A obtains, filter, obtain oxytetracycline ethanol solution;

[0037] C. Crystallization by cooling: add 6 mL of concentrated hydrochloric acid to the oxytetracycline ethanol solution obtained in step B, stir, cool down to 10° C. to crystallize, filter after 3 hours, wash the filter cake with 6° C. ethanol, and obtain the wet product of oxytetracycline hydrochloride;

[0038] D. Drying: The wet product of oxytetracycline hydrochloride obtained in step C was dried in a vacuum drying oven at 80° C. for 7 hours to obtain 45 grams of finished product of oxytetracycline hydrochloride, which was tested to meet the standards of the Chinese Pharmacopoeia.

[0039] The abov...

Embodiment 3

[0043] A. Dissolution: Add 50g of oxytetracycline base to 450mL of ethanol, then add 6.5mL of hydrochloric acid-ethanol mixed solution, stir, heat to 42°C until completely dissolved to obtain a mixed solution;

[0044] B, active carbon decolorization treatment: add 0.2g active carbon in the mixed solution that step A obtains, filter, obtain oxytetracycline ethanol solution;

[0045] C. Crystallization by cooling: add 7 mL of concentrated hydrochloric acid to the oxytetracycline ethanol solution obtained in step B, stir, cool down to 10° C. to crystallize, filter after 2 hours, wash the filter cake with 6° C. ethanol, and obtain oxytetracycline hydrochloride wet product;

[0046] D. Drying: The wet product of oxytetracycline hydrochloride obtained in step C was dried in a vacuum drying oven at 70° C. for 7.5 hours to obtain 42 grams of finished product of oxytetracycline hydrochloride, which met the standards of the Chinese Pharmacopoeia.

[0047] The above-mentioned embodiment i...

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Abstract

The invention provides a preparation method of oxytetracycline hydrochloride. Oxytetracycline dihyclorate serves as a starting material, is sequentially subjected to alcohol dissolution and acid alcohol dissolution procedures and activated carbon decoloration treatment and cooling crystallization procedures and is dried to obtain finished oxytetracycline hydrochloride; in the alcohol dissolution procedure, the mass-to-volume ratio of oxytetracycline to alcoholic solution is 1:(7-9); and in the acid alcohol dissolution procedure, the mass-to-volume ratio of the oxytetracycline to acid alcohol solution is 1: (0.077-0.13). The oxytetracycline hydrochloride prepared by the method is large in size, good in flowability, high in observent density, low in energy consumption in a production process and low in cost; and because ethyl alcohol serves as crystallization solvent, the oxytetracycline hydrochloride is non-toxic and harmless, and does not pollute environments.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation and relates to the preparation of antibiotics, in particular to a preparation method of oxytetracycline hydrochloride. The oxytetracycline hydrochloride product prepared by the method has good fluidity and high apparent density. Background technique [0002] Oxytetracycline hydrochloride, also known as oxytetracycline hydrochloride, oxytetracycline hydrochloride, or oxytetracycline hydrochloride, is an antibiotic widely used in humans and animals, and is clinically used to treat various diseases, such as rickettsiasis, including Epidemic typhus, endemic typhus, scrub typhus; infection caused by Mycoplasma pneumoniae; chlamydial infection, including psittacosis, venereal lymphoid edema, nonspecific urethritis, salpingitis, and trachoma; relapsing fever; Brucella disease; cholera; plague and tularemia, etc. The dosage forms of oxytetracycline hydrochloride are tablets, capsules, powder...

Claims

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Application Information

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IPC IPC(8): C07C237/26C07C231/12C07C231/24
Inventor 荆敬超赵宝华
Owner HEBEI SHENGXUE DACHENG PHARMA
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