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Preparation method of occrycetin

A technology of oxytetracycline hydrochloride and preparation steps, which is applied in the field of oxytetracycline preparation, can solve the problems such as the loose combination of small crystal particles, the loose structure of oxytetracycline hydrochloride, and the difficulty in flowing, and achieves a compact internal structure and is not easily broken. , the effect of no methanol residue

Inactive Publication Date: 2016-10-26
仇颖超
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem mainly solved by the present invention: In the process of preparing oxytetracycline hydrochloride in the current traditional method, it is necessary to add an appropriate amount of hydrogen chloride methanol solution, which easily causes the residue to exceed the standard, the content is low, and the internal structure of the prepared oxytetracycline hydrochloride is loose , the combination of small crystal particles is not tight, it is easy to break, and becomes a small single crystal, which is not easy to flow. It provides a method of combining the prepared modified emulsion with the prepared thyme monoglucoside extract and polyvinyl alcohol. , phenol mixed, sodium hydroxide solution was added dropwise and heated in a water bath, filtered and dried to obtain adsorption microspheres adsorbed into the prepared oxytetracycline hydrochloride dispersion, mixed with deionized water after rotary steaming, heated in a water bath under stirring, filtered to The filtrate is rotary evaporated to dryness, thereby obtaining the preparation method of oxytetracycline hydrochloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0021] Firstly, dry thyme is collected, pulverized and sieved to prepare 70-mesh thyme powder, then the thyme powder is mixed with methanol at a mass ratio of 1:5, heated in a water bath at 65°C for 3 hours, and centrifuged at 1600r / min Separated for 10 minutes, collected the supernatant and evaporated to dryness at 65° C. to prepare thyme monoglucoside extract, and set aside; then weighed 25 parts of chitosan, 20 parts of glacial acetic acid solution, 30 parts of liquid paraffin and 15 parts of sorbitan fatty acid ester were placed in a three-necked flask, stirred and mixed at room temperature for 10 minutes to prepare a modified emulsion; then weighed 40 parts of modified emulsion in parts by weight. Emulsion, 10 parts of polyvinyl alcohol, 10 parts of phenol and 20 parts of the Thyme single-glucoside extract prepared above are placed in a three-necked flask, and after stirring and mixing for 10 minutes, 1mol / L sodium hydroxide solution is added dropwise to it until the pH re...

example 2

[0024]Firstly, dry thyme is collected, crushed and sieved to prepare thyme powder of 75 mesh, then the thyme powder is mixed with methanol at a mass ratio of 1:5, then heated in a water bath at 75°C for 4 hours, and centrifuged at 1700r / min Separation for 13 minutes, collecting the supernatant and rotatively evaporating to dryness at 75°C to prepare a thyme monoglucoside extract, and set aside; then weigh 30 parts of chitosan, 30 parts of glacial acetic acid solution, 35 parts of liquid paraffin and 20 parts of sorbitan fatty acid ester were placed in a three-necked flask, stirred and mixed at room temperature for 13 minutes to prepare a modified emulsion; then weighed 45 parts of modified emulsion in parts by weight. Emulsion, 13 parts of polyvinyl alcohol, 13 parts of phenol and 25 parts of Thyme single-glucoside extracts prepared above are placed in a three-necked flask, and after stirring and mixing for 13 minutes, 1mol / L sodium hydroxide solution is added dropwise to it un...

example 3

[0027] Firstly, dry thyme is collected, pulverized and sieved to prepare 80-mesh thyme powder, then the thyme powder is mixed with methanol at a mass ratio of 1:5, then heated in a water bath at 80°C for 5 hours, and centrifuged at 1800r / min Separation for 15 minutes, collecting the supernatant and rotatively evaporating to dryness at 80°C to prepare a thyme monoglucoside extract, and set aside; then weigh 35 parts of chitosan, 40 parts of glacial acetic acid solution, 40 parts of liquid paraffin and 25 parts of sorbitan fatty acid ester were placed in a three-necked flask, stirred and mixed at room temperature for 15 minutes to prepare a modified emulsion; then weighed 50 parts of modified emulsion in parts by weight. Emulsion, 15 parts of polyvinyl alcohol, 15 parts of phenol and 30 parts of Thyme monoglucoside extract prepared above are placed in a three-necked flask, after stirring and mixing for 15 minutes, 1mol / L sodium hydroxide solution is added dropwise to it to pH to ...

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Abstract

The invention discloses a preparation method of occrycetin, which belongs to the technical field of oxytetracycline preparation. The preparation method comprises the following steps of mixing prepared modified emulsion with prepared thyme monoterpene glycoside extracts, polyvinyl alcohol and phenol, dropwise adding a sodium hydroxide solution, heating in water bath, filtering and drying, so as to obtain adsorption microspheres which are adsorbed into prepared occrycetin dispersion liquid, spirally evaporating, then mixing with deionized water, heating in water bath in a stirring state, filtering, and spirally evaporating filtrate so as to be dry and obtain the occrycetin. Examples show that the preparation method has the advantages of low cost and simple, convenient process and no damage to personnel and environment in the whole operating process, the prepared product has the advantages of compact internal structure, difficulty in breaking, good flowability and water solubility, no residual methanol and good quality, and the yield can be stabilized to 95 to 98%.

Description

technical field [0001] The invention discloses a preparation method of oxytetracycline hydrochloride, which belongs to the technical field of oxytetracycline preparation. 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, powders, eye drops and ointments. [0003] The traditional preparation method of oxytetracycline hydrochloride is: dissolve oxytetracycline in the anhydrou...

Claims

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Application Information

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IPC IPC(8): C07C237/26C07C231/24A61K31/65A61P1/00A61P31/04A61P11/00
CPCC07C231/24A61K31/65A61K36/53C07C237/26
Inventor 仇颖超张明高玉刚
Owner 仇颖超
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