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A kind of extraction recovery method of penicillin sulfoxide

A technology of penicillin sulfoxide and medium penicillin is applied in the field of extraction and recovery of penicillin sulfoxide, which can solve the problems of restricting yield improvement and environmental damage.

Active Publication Date: 2018-02-23
NORTH CHINA PHARMA COMPANY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, various crystallization mother liquors discharged in different processes still restrict the improvement of yield and cause damage to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Adjust the pH of the penicillin sulfoxide solution with a concentration of 10mg / ml to 2.5, at 15°C at 30m 3 The flow rate of / h is equipped with 10m 3 Resin column of macroporous adsorption resin, 100 m into penicillin sulfoxide solution 3 , and then at 25°C with methanol (adjusted to pH 7) with 20m 3 The flow rate of / h is desorbed through the resin column, and 20 m of methanol is introduced 3 , collecting the desorption solution for 20 m 3 . Cool the desorption solution to 20°C, adjust the pH to 1.5 with 20% sulfuric acid, grow crystals, filter, wash, and dry to obtain 800 kg (pure) of penicillin sulfoxide.

Embodiment 2

[0050] Adjust the pH of the penicillin sulfoxide crystallization mother liquor with a concentration of 1mg / ml to 2.5, 3 The flow rate of / h is equipped with 10m 3 Resin column of macroporous adsorption resin, 200 m of penicillin sulfoxide crystallization mother liquor 3 , and then at 25°C with methanol (adjusted to pH 7) with 10m 3 The flow rate of / h is desorbed through the resin column, and 20 m of methanol is introduced 3 , collecting the desorption solution for 20 m 3 . The desorption solution was evaporated and concentrated to 2m at a vacuum of 0.08Mpa and 40°C 3 , the temperature of the desorption solution was lowered to 20°C, the pH was adjusted to 1.5 with 20% sulfuric acid, the crystal was grown, filtered, washed, and dried to obtain 156 kg (pure) of penicillin sulfoxide.

Embodiment 3

[0052] Adjust the pH of the penicillin sulfoxide methanol crystallization mother liquor with a concentration of 5mg / ml to 2.5, 3 The flow rate of / h is equipped with 10m 3 The resin column of macroporous adsorption resin is passed into the crystallization mother liquor of penicillin sulfoxide and methanol for 120 m 3 , and then at 25°C with methanol (adjusted to pH 7) with 15m 3 The flow rate of / h is desorbed through the resin column, and 20 m of methanol is introduced 3 , collecting the desorption solution for 20 m 3 . The desorption solution was concentrated to 2m by nanofiltration membrane 3 , the temperature of the desorption solution was lowered to 20°C, the pH was adjusted to 1.5 with 20% sulfuric acid, the crystal was grown, filtered, washed, and dried to obtain 492 kg of penicillin sulfoxide (pure).

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PUM

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Abstract

The invention discloses a method for extracting and recycling penicillin sulfoxide. The method comprises the following steps that a, a penicillin sulfoxide solution is subjected to impurity separation through resin absorption; b, a penicillin sulfoxide desorption solution is obtained through resin desorption; c, a penicillin sulfoxide crystallization solution is obtained through the mechanical application of dissolution penicillin sulfoxide to the penicillin sulfoxide desorption solution or concentration of the penicillin sulfoxide desorption solution; d, the pH of the crystallization solution is adjusted with acid for crystallization, and the penicillin sulfoxide is obtained through filtration, washing and drying. The method can be used for extracting and recycling the penicillin sulfoxide from the low concentration penicillin sulfoxide solution, and therefore the yield of the penicillin sulfoxide is increased, the production cost is reduced, and environmental pollution is reduced. The quality of subsequent products like 7ADCA, cefradine, cefalexin and cefadroxil prepared from the penicillin sulfoxide produced through the technology is improved. Pharmaceutical compositions formed by cefradine, cefalexin, cefadroxil and a medically acceptable carrier can be utilized for treating respiratory tract infection like acute tonsillitis, angina, tympanitis, nasosinusitis, bronchitis and pneumonia, urinary tract infection, skin soft-tissue infection and the like caused by sensitive bacteria.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, in particular to a method for extracting and recovering penicillin sulfoxide. Background technique [0002] Penicillin sulfoxide is an important intermediate for the preparation of 7-amino-desacetoxycephalosporanic acid (7-ADCA), which is one of the two major nuclei of cephalosporin antibiotics , is an important precursor for the production of cephalosporins such as cephalexin, cefadroxil, and cephradine. Therefore, the production quality and yield of penicillin sulfoxide directly affect the production of cephalosporin antibiotics. [0003] The preparation method of penicillin sulfoxide has following several at present: [0004] 1. Penicillin industrial salt method: [0005] a. The penicillin fermentation liquid is filtered and acidified and then extracted with butyl ester to obtain penicillin butyl ester extract (abbreviated as BA); [0006] b. Alkalinization and back-extraction...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D499/46C07D499/18C12P35/00A61K31/545A61P31/04A61P11/02A61P11/04A61P11/00A61P17/00A61P15/00
CPCC07D499/18C07D499/46C12P35/00
Inventor 闫峰周志茂赵伟张伟张桂华周玉段志钢张锁庆孙燕魏青杰
Owner NORTH CHINA PHARMA COMPANY
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