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Continuous chromatography separation and purification method for lincomycin

A continuous chromatography and lincomycin technology, which is applied in the field of separation and purification of the antibacterial drug lincomycin, can solve the problems of high impurity content, long production process time, low content of lincomycin hydrochloride, etc., and achieve product composition and The effect of maintaining stable concentration and reducing the amount of resin used

Active Publication Date: 2018-01-23
JIANGXI GUOYAO PHARMA LLC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] After research, we found that the current production process of lincomycin is relatively traditional, the content of lincomycin hydrochloride produced is not high, and the content of impurities is also high, and the production process takes a long time, which cannot meet the market demand

Method used

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  • Continuous chromatography separation and purification method for lincomycin
  • Continuous chromatography separation and purification method for lincomycin
  • Continuous chromatography separation and purification method for lincomycin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Step 1, applying the lincomycin fermentation filtrate to a continuous chromatographic column to obtain an eluate;

[0064] In step 2, the eluate is concentrated, crystallized and dried to obtain pure lincomycin.

[0065] Wherein, the continuous chromatographic column mentioned in step 1, the resin is selected from: macroporous adsorption resin HZ-802, the resin particle diameter is 50-100 mesh, and the uniformity is above 95%.

[0066] Wherein, the process of concentrating and drying the eluate described in step 2 is as follows: concentrating under reduced pressure, the vacuum degree is 0.02-0.15Mpa, the operating temperature is 35-90°C, and concentrating until the mass concentration of lincomycin is 25%. ~70% to obtain a concentrated solution; the concentrated solution is crystallized with acetone to obtain a solid.

[0067] Wherein, the continuous chromatography is selected from: a disc conveying continuous chromatography separation system or a simulated moving bed c...

Embodiment 2

[0093] Proceed as follows:

[0094] Step 1, applying the lincomycin fermentation filtrate to a continuous chromatographic column to obtain an eluent;

[0095] In step 2, the eluate is concentrated, crystallized and dried to obtain pure lincomycin.

[0096] Wherein, the continuous chromatographic column mentioned in step 1, the resin is selected from: macroporous adsorption resin HZ-802, the resin particle diameter is 50-100 mesh, and the uniformity is above 95%.

[0097] Wherein, the process of concentrating and drying the eluate described in step 2 is as follows: concentrating under reduced pressure, the vacuum degree is 0.02-0.15Mpa, the operating temperature is 35-90°C, and concentrating until the mass concentration of lincomycin is 25%. ~70% to obtain a concentrated solution; the concentrated solution is crystallized with acetone to obtain a solid.

[0098] Wherein, the continuous chromatography is selected from: a disc conveying continuous chromatography separation syst...

Embodiment 3

[0134] Embodiment 3, the comparison of purification method of the present invention and existing purification method

[0135] In order to investigate the best preparation method of lincomycin, the preparation method of the present invention was compared with the existing technology, wherein: scheme 1: the fermentation broth is filtered to remove the mycelium after acidification treatment, and the filtrate is adjusted to pH to 11. Add butanol to it for extraction and refining, add HCL solution for back extraction, concentrate under reduced pressure, adsorb on activated carbon, crystallize, and dry to obtain lincomycin hydrochloride raw material drug. Scheme 2: Purification method of the present invention (Example 2). The result shows that the purity index of lincomycin purified by the purification method of the present invention is obviously better than that of the existing purification method.

[0136]

[0137]

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Abstract

The invention relates to a continuous chromatography separation and purification method for lincomycin. Efficient separation of component A of lincomycin is realized by using a continuous chromatography technology. The method comprises the following steps: enabling a lincomycin fermented filter liquor obtained through biological fermentation to enter into a continuous chromatography system, carrying out adsorption, impurity washing, lincomycin elution, eluant collection and chromatographic column regeneration, concentrating a collected eluant and then carrying out salt decoloration to obtain lincomycin hydrochloride. The lincomycin obtained by adopting the method is high in yield, high in purity, low in cost and environmentally-friendly, and is applicable for industrial production. The method has the advantages of short production process time and high product yield, the content of lincomycin hydrochloride (dry basis) in the prepared final product reaches more than 99%, and the disadvantages that the lincomycin hydrochloride produced in the prior art is not high in content and long in production process time are overcome.

Description

technical field [0001] The invention belongs to the field of pharmacy and relates to a method for separating and purifying an antibacterial drug lincomycin. Background technique [0002] Lincomycin (C 18 h 34 N 2 o 6 S) Also known as lincomycin and lincomycin, it is an effective inhibitor of Gram-positive bacteria. Its principle of action is to act on the 50S subunit of the ribosome of sensitive bacteria, prevent the extension of the peptide chain, and inhibit bacterial cells. of protein synthesis. At high concentrations, it is also bactericidal against highly sensitive bacteria. Lincomycin has slow development of drug resistance, good tissue permeability, and good curative effect on respiratory system infection, so lincomycin is widely used in clinical treatment. As resistance to other antibiotics such as penicillin is gradually discovered, leading to the restriction of the use of these antibiotics, the demand for lincomycin is gradually increasing. [0003] The linc...

Claims

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Application Information

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IPC IPC(8): C07H15/16C07H1/06
Inventor 万义斌葛友群左飞鸿杨明余承祥卢佰福李进进刘威潘磊邓愍民
Owner JIANGXI GUOYAO PHARMA LLC
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