A kind of lincomycin hydrochloride purification process

A lincomycin hydrochloride and process technology, applied in the field of lincomycin hydrochloride purification technology, can solve the problems such as the inability to reduce the B component of lincomycin hydrochloride, and achieve the effects of increasing final yield and improving utilization rate

Active Publication Date: 2017-11-21
JIANGXI GUOYAO PHARMA LLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention proposes a lincomycin hydrochloride purification process, the content of lincomycin hydrochloride B component in the prepared finished product is lower than 1wt%, which solves the problem of lincomycin hydrochloride in the lincomycin hydrochloride finished product produced by the prior art The disadvantage that the element B component cannot be reduced to 1wt%

Method used

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  • A kind of lincomycin hydrochloride purification process

Examples

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Comparison scheme
Effect test

Embodiment 1

[0034] refer to figure 1 , a kind of lincomycin hydrochloride purification process, the resin column selected is or LX-20 type macroporous resin, the lincomycin A component 85wt% in the lincomycin hydrochloride crude product crystallization that selects, lincomycin B component 14wt%, other impurity 1wt%; Technology comprises the following steps:

[0035] S1. Adsorption step: Put 100 kilograms of lincomycin hydrochloride crude product crystals into a dissolving tank, add pure water to dissolve, and obtain an aqueous solution with a titer of 300,000 units, add activated carbon to decolorize the solution, and after decolorization is completed, filter and press Put it into the stock solution irrigation, add pure water to dilute it, adjust the pH of the solution to 10.5, and obtain the stock solution. / hr, detect the titer of the desorption liquid at the outlet of the resin column, and discard the ineffective desorption liquid. When it is detected that the titer of the desorption...

Embodiment 2

[0043] refer to figure 1 , a lincomycin hydrochloride purification process, the resin column selected is LSA-100 type macroporous resin column, lincomycin A component 85wt% in the lincomycin hydrochloride crude product crystallization that selects, lincomycin B Component 14wt%, other impurity 1wt%; Technology comprises the steps:

[0044]S1. Adsorption step: Put 100 kg of lincomycin hydrochloride crude product crystals into a dissolving tank, add purified water to dissolve, and obtain an aqueous solution with a titer of 320,000 units, add activated carbon to decolorize the solution, and after decolorization is completed, filter, press Put it into the stock solution irrigation, add pure water to dilute it, adjust the pH of the solution to 10.6, and obtain the stock solution. / hr, detect the titer of the desorption liquid at the outlet of the resin column, and discard the ineffective desorption liquid. When it is detected that the titer of the desorption solution is 26,000 uni...

Embodiment 3

[0052] refer to figure 1 , a lincomycin hydrochloride purification process, the resin column selected is LSA-100 type macroporous resin column, lincomycin A component 85wt% in the lincomycin hydrochloride crude product crystallization that selects, lincomycin B Component 14wt%, other impurity 1wt%; Technology comprises the steps:

[0053] S1. Adsorption step: put 100 kg of lincomycin hydrochloride crude product crystals into a dissolving tank, add pure water to dissolve, and obtain an aqueous solution with a titer of 350,000 units, add activated carbon to decolorize the solution, and after decolorization is completed, filter and press Put it into the stock solution irrigation, add pure water to dilute it, adjust the pH of the solution to 11.5, and obtain the stock solution. / hr, detect the titer of the desorption liquid at the outlet of the resin column, and discard the ineffective desorption liquid. When it is detected that the titer of the desorption solution is 40,000 uni...

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PUM

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Abstract

The invention discloses a lincomycin hydrochloride purification technology. The technology comprises steps as follows: S1, adsorption: sequentially performing dissolution, decoloration, filtration, dilution, pH adjustment and column loading to obtain a saturated resin column; S2, washing: sequentially performing press-drying, washing and repress-drying to obtain a secondarily dried saturated resin column; S3, analysis: performing analysis with saturated n-butyl alcohol to obtain an analysis solution; S4, concentration and crystallization: sequentially performing hydrochloric acid crystallization, acetone recrystallization and drying to obtain a finished product. The content of a lincomycin hydrochloride component B in the finished product is lower than 1wt%, so that the defect that lincomycin hydrochloride components B in finished lincomycin hydrochloride products produced in the prior art cannot be decreased to 1wt% is overcome.

Description

technical field [0001] The invention relates to a process for preparing lincomycin hydrochloride, in particular to a process for purifying lincomycin hydrochloride. Background technique [0002] The chemical name of lincomycin hydrochloride is 6-(1-methyl-trans-4-propyl-L-2-pyrrolidinecarboxamido)-1-thio-6,8-dideoxy-D-erythro -α-D-galactopyranoside hydrochloride-hydrate, its molecular formula is S3 18 h 34 N 2 o 6 S·HCl·H 2 O, with a molecular weight of 461.02, is mainly used as an antibiotic drug. The production of lincomycin hydrochloride is produced through microbial fermentation. During the fermentation production process, in addition to the main production of lincomycin A component, a small amount of lincomycin hydrochloride is semi-produced. components such as mycin B and trace amounts of lincomycin E. Compared with lincomycin A component, lincomycin B component has low antibacterial activity and relatively large toxin. Therefore, the content of B component in li...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/16C07H1/06
CPCC07H1/06C07H15/16
Inventor 左飞鸿钟承赞葛友群余承祥丁永绥秦义平李进进潘磊
Owner JIANGXI GUOYAO PHARMA LLC
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