Method for separation of lincomycin

A separation method and lincomycin technology, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve problems such as complex and solvent consumption operations, and achieve the effects of moderate solvent consumption and easy operation.

Inactive Publication Date: 2012-10-24
SHANGHAI INST OF PHARMA IND
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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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The lincomycin fermentation broth (unit is 7560u / ml, the volume is 1.3L) is adjusted to pH 2.0 with oxalic acid, and the acidified solution is obtained by plate and frame filtration, and the pH of the acidified solution is adjusted to 9.5 with sodium hydroxide, and then filtered to obtain the solution. filtrate;

[0034] Select PS / DVB reversed-phase adsorption resin NM PS100 to adsorb it (chromatographic column diameter is about 4cm, height is about 20cm), after adsorption on the column at a flow rate of 0.02BV / min, with 4.5BV pH of 9.5 alkaline water Carry out elution and impurity removal, remove a large amount of pigments and salts, and basically wash off the B component, and then use 1.5BV of n-butanol to concentrate lincomycin;

[0035]The n-butanol solution of lincomycin was concentrated to 20% of the original volume under reduced pressure at 60°C, and the pH was adjusted to 0.5 with hydrochloric acid, and then the temperature was lowered to 20°C for 4 hours to cry...

Embodiment 2

[0038] The lincomycin fermentation broth (unit is 7361u / ml, volume is 1.4L) is adjusted to pH 3.0 with oxalic acid, and the acidified solution is obtained by plate and frame filtration, and the pH of the acidified solution is adjusted to 9.0 with sodium hydroxide, and then filtered to obtain the solution. filtrate;

[0039] Select PS / DVB reversed-phase adsorption resin microsphere No. 1 to adsorb it (chromatographic column diameter is about 4cm, height is about 20cm), after adsorption on the column at a flow rate of 0.04BV / min, use 5BV pH to be 9.0 alkali Water is eluted to remove impurities, remove a large amount of pigments and salts, and basically wash off the B component, and then use 2BV of n-butanol to concentrate lincomycin;

[0040] The n-butanol solution of lincomycin was concentrated under reduced pressure to 15% of the original volume at 50°C, and the pH was adjusted to 1.0 with hydrochloric acid, then the temperature was lowered to 25°C and left to stand for 6 h fo...

Embodiment 3

[0043] The lincomycin fermentation broth (unit is 7862u / ml, volume is 1.0L) is adjusted to pH 3.5 with oxalic acid, and the acidified solution is obtained by plate and frame filtration, and the pH of the acidified solution is adjusted to 10.0 with sodium hydroxide, and then filtered to obtain the solution. filtrate;

[0044] Select PS / DVB reversed-phase adsorption resin NM PS100 to adsorb it (chromatographic column diameter is about 4cm, height is about 20cm), after adsorption on the column at a flow rate of 0.03BV / min, use 5.5BV of alkaline water with pH of 10.0 Carry out elution and impurity removal, remove a large amount of pigments and salts, and basically wash off the B component, and then use 2.5BV of n-butanol to concentrate lincomycin;

[0045] The n-butanol solution of lincomycin was concentrated under reduced pressure to 25% of the original volume at 55°C, and the pH was adjusted to 1.5 with hydrochloric acid, and then the temperature was lowered to 30°C for 8h to cr...

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PUM

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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 present invention relates to a separation method of lincomycin. Background technique [0002] Lincomycin (Lincomycin) is a lincosamide basic antibiotic, soluble in water and methanol, its hydrochloride is used clinically, mainly for the treatment of infection caused by Gram-positive bacteria. In the process of producing lincomycin by fermentation with Streptomyces lincolnensis, in addition to lincomycin, other structural analogs such as lincomycin B component are also produced. Lincomycin B component is a toxic component that needs to be removed, otherwise it will affect product quality, especially when processing lincomycin derivatives, the control of B component content is more stringent. [0003] The traditional process generally adopts solvent extraction method to extract lincomycin from fermentation broth. Among them, the butanol extraction method has the disadvantages of large solvent consumption, poor operating conditions and environment, ...

Claims

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Application Information

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IPC IPC(8): C07H15/16C07H1/06
Inventor 李继安蓝鸿
Owner SHANGHAI INST OF PHARMA IND
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