A kind of separation method of lincomycin

A separation method, lincomycin technology, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problem of solvent consumption and complexity, and achieve the effect of moderate solvent consumption and easy operation

Inactive Publication Date: 2016-04-20
SHANGHAI INST OF PHARMA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the large solvent consumption or complex operation of the separation method of lincomycin in the prior art, and the defect that the content of lincomycin B component in the obtained product is relatively high, and a new method is provided. The solvent consumption is moderate, the operation is simple, and the purity of the product lincomycin can reach more than 98%, and the separation method of lincomycin with a content of lincomycin B component below 0.5%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Adjust the pH of lincomycin fermentation broth (unit: 7560u / ml, volume: 1.3L) to 2.0 with oxalic acid, filter the acidified solution with plate and frame, adjust the pH of the acidified solution to 9.5 with sodium hydroxide, and then filter to obtain filtrate;

[0034] Use PS / DVB reversed-phase adsorption resin NMPS100 to adsorb it (the diameter of the chromatography column is about 4cm, and the height is about 20cm). Remove impurities, remove a large amount of pigment and salt, and basically wash off component B, and then use 1.5BV of n-butanol to wash off lincomycin;

[0035]The n-butanol solution of lincomycin was concentrated under reduced pressure at 60°C to 20% of the original volume, and the pH was adjusted to 0.5 with hydrochloric acid, then the temperature was lowered to 20°C and allowed to stand for 4 hours to crystallize, and the crude crystals were obtained by suction filtration;

[0036] Dissolve the crude crystals of lincomycin with 10 times the volume of...

Embodiment 2

[0038] Adjust the pH of the lincomycin fermentation liquid (unit: 7361u / ml, volume: 1.4L) to 3.0 with oxalic acid, filter the acidified liquid with plate and frame, adjust the pH of the acidified liquid to 9.0 with sodium hydroxide, and then filter to obtain filtrate;

[0039] Select PS / DVB reversed-phase adsorption resin microsphere No. 1 to adsorb it (the diameter of the chromatographic column is about 4cm, and the height is about 20cm). Perform elution to remove impurities, remove a large amount of pigment and salt, and basically wash off component B, and then use 2BV of n-butanol to wash off lincomycin;

[0040] The n-butanol solution of lincomycin was concentrated under reduced pressure at 50°C to 15% of the original volume, and the pH was adjusted to 1.0 with hydrochloric acid, then the temperature was lowered to 25°C and allowed to stand for 6 hours to crystallize, and the crude crystals were obtained by suction filtration;

[0041] Dissolve the crude crystals of linco...

Embodiment 3

[0043] Adjust the pH of lincomycin fermentation liquid (unit: 7862u / ml, volume: 1.0L) to 3.5 with oxalic acid, filter the acidified solution with plate and frame, adjust the pH of the acidified solution to 10.0 with sodium hydroxide, and then filter to obtain filtrate;

[0044] Select PS / DVB reversed-phase adsorption resin NMPS100 to adsorb it (the diameter of the chromatographic column is about 4cm, and the height is about 20cm). Remove impurities, remove a large amount of pigment and salt, and basically wash off component B, and then use 2.5BV of n-butanol to wash off lincomycin;

[0045] The n-butanol solution of lincomycin was concentrated under reduced pressure at 55°C to 25% of the original volume, and the pH was adjusted to 1.5 with hydrochloric acid, then the temperature was lowered to 30°C and allowed to stand for 8 hours to crystallize, and the crude crystals were obtained by suction filtration;

[0046] Dissolve the crude crystals of lincomycin with 13 times the vo...

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Abstract

The invention discloses a method for separation of lincomycin. The method comprises the following steps of acidizing a lincomycin-containing fermentation liquor, carrying out filtration, carrying out alkalinity regulation, carrying out filtration again, collecting a filtrate, treating the filtrate as a sample liquid by a polystyrene-divinylbenzene reversed-phase adsorption resin, carrying out elution purification of the filtrate by an alkaline aqueous solution having a pH value the same as a pH value of the filtrate, eluting lincomycin by n-butanol, collecting the n-butanol solution of lincomycin, carrying out concentration, acidification and crystallization, and carrying out recrystallization by acetone. The method provided by the invention has the advantages of appropriate solvent consumption, simple processes, high product lincomycin purity more than 98%, and low lincomycin component B content less than 0.5%.

Description

technical field [0001] The invention relates to a method for separating lincomycin. Background technique [0002] Lincomycin (Lincomycin) is a lincosamine-type alkaline antibiotic, easily soluble in water and methanol, and its hydrochloride is used clinically, mainly for the treatment of infections caused by Gram-positive bacteria. During the fermentative production of lincomycin by Streptomyces lincolnensis, in addition to lincomycin, other structural analogues such as lincomycin B component are also produced. Component B of lincomycin is a toxic component that needs to be removed, otherwise it will affect the quality of the product, especially when the content of component B is strictly controlled when processing lincomycin derivatives. [0003] The traditional process generally adopts the solvent extraction method to extract lincomycin from the fermentation broth. Among them, the disadvantages of the butanol extraction method are that the solvent consumption is large, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/16C07H1/06
Inventor 李继安林惠敏陈代杰陈舟舟
Owner SHANGHAI INST OF PHARMA IND CO LTD
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