Method for preparing lincomycin hydrochloride

A technology of lincomycin hydrochloride and its production method, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc.

Active Publication Date: 2011-11-23
XINYU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no report that any manufacturer has produced lincomycin hydrochloride with lincomycin B component less than 0.1% and a single unknown impurity less than 0.05%

Method used

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  • Method for preparing lincomycin hydrochloride
  • Method for preparing lincomycin hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1. A special extraction tower device for lincomycin hydrochloride,

[0023] The structure of the extraction tower is as figure 1 As shown, the special extraction tower device for lincomycin hydrochloride is an extraction tower 1 composed of a closed container, the top of the extraction tower is provided with an extractant outlet 2, the upper part of the side of the extraction tower is provided with an aqueous solution inlet 3, and the lower part of the side of the extraction tower is provided with a secondary Octanol inlet 4, extraction waste liquid outlet 5 is provided at the bottom of the extraction tower. A distributor 6 and a distributor 7 are sequentially provided in the extraction tower to communicate with the inlet 4 of the secondary octanol and the inlet 3 of the aqueous solution, respectively, so that the incoming aqueous solution and secondary octanol are uniformly distributed in the container. The distributor is a coil connected with the aqueous s...

Embodiment 2

[0025] Dissolve 400 kg of lincomycin hydrochloride product with lincomycin hydrochloride B component ≤ 1.0% to 80000 μg / ml with purified water, and adjust the pH value to 10-11 with flake NaOH. Enter the upper part of the above-mentioned lincomycin hydrochloride aqueous solution extraction tower, and simultaneously pass through the secondary octanol of aqueous solution volume 1 / 2 from the bottom of the extraction tower to extract, and most of lincomycin hydrochloride is transferred in the secondary octanol phase (extraction liquid), flows out from the top of the tower, and the raffinate phase waste liquid contains more lincomycin hydrochloride B components and less lincomycin hydrochloride, and flows out from the bottom of the tower.

[0026] Add purified water to the extract and use hydrochloric acid to adjust the pH value to 2-4 for back extraction, transfer lincomycin into the water phase, and separate the lower layer of the water phase extract after standing still. Slowly ...

Embodiment 3

[0029] Dissolve 400 kg of lincomycin hydrochloride product with lincomycin B component ≤ 1.0% in purified water to 100000 μg / ml, and adjust the pH value to 10-11 with flake NaOH. Enter the upper part of the above-mentioned lincomycin hydrochloride aqueous solution extraction tower, and simultaneously pass through the secondary octanol of aqueous solution volume 1 / 3 from the bottom of the extraction tower to extract, and most of lincomycin hydrochloride is transferred in the secondary octanol phase (extraction liquid), flows out from the top of the tower, and the raffinate phase waste liquid contains more lincomycin hydrochloride B components and less lincomycin hydrochloride, and flows out from the bottom of the tower.

[0030] Add purified water to the extract and use hydrochloric acid to adjust the pH value to 2-4 for back extraction, transfer lincomycin into the water phase, and separate the lower layer of the water phase extract after standing still. Slowly add 10-12 times...

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Abstract

The invention relates to a method and a device for preparing lincomycin hydrochloride. On the basis of the prior lincomycin hydrochloride production, repurifying processing procedure is added to prepare lincomycin hydrochloride with lincomycin B component less than or equal to 0.1 percent. The method is characterized by comprising the following steps: lincomycin hydrochloride with B component less than or equal to 1.0 percent is dissolved to have thetconcentration of 80000-100000 microgramme / ml, the pH value is adjusted to 10-11, extraction is carried out in extraction tower with 1 / 2-1 / 3 (weight ratio) of 2-octanol, the extraction temperature is 20-30 DEG C, the pH value of extraction liquid is adjusted to 2-4 by hydrochloric acid for back extraction, and acetone is used for crystallization. By adopting the method and the extraction tower device, the concentration of B component in lincomycin hydrochloride can be effectively reduced to be less than or equal to 0.1 percent, so that thequality of lincomycin hydrochloride is improved, and the yield is increased by 5-7 percent.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and relates to a production method and a device thereof for lincomycin hydrochloride B≤0.1% in lincomycin hydrochloride. Background technique [0002] Lincomycin hydrochloride (lincomycin) is a high-efficiency broad-spectrum, lincosamine antibiotic, which was first obtained from the culture medium of Streptomyces linvaria by American Mason in 1962. The lincomycin (lincomycin) isolated in my country Has the same structure as the former and started production in 1975. [0003] Lincomycin hydrochloride is a lincosamide antibiotic. It is the fermented liquid fermented by aerobic fermentation of lincomycin-producing bacteria (a kind of actinomycetes), which is pretreated, filtered and refined into lincomycin hydrochloride. [0004] In the fermentation production process of lincomycin hydrochloride, in addition to lincomycin hydrochloride, a small amount of lincomycin hydrochloride B component will b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/16C07H1/06A61P31/00
Inventor 黄伟夏守友祖路明
Owner XINYU PHARM CO LTD
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