Comprehensive recovery method for effective ingredients in 7-amidogen cephalosporins alkanes acid crystallization mother liquor produced through enzymatic hydrolysis method

An aminocephalosporanic acid and recovery method technology, applied in the pharmaceutical field, can solve problems such as high treatment costs, and achieve the effects of reducing emissions, reducing costs, and realizing environmental protection, clean and green production

Active Publication Date: 2015-12-30
SHANXI WEIQIDA PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no effective way to recycle this part of the mother liquor, and it can only be used as high-concentration wastewater for subsequent environmental protection treatment. Manufacturers have paid high treatment costs for this

Method used

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  • Comprehensive recovery method for effective ingredients in 7-amidogen cephalosporins alkanes acid crystallization mother liquor produced through enzymatic hydrolysis method
  • Comprehensive recovery method for effective ingredients in 7-amidogen cephalosporins alkanes acid crystallization mother liquor produced through enzymatic hydrolysis method

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Effect test

preparation example Construction

[0033] In the preparation of the step (4) 7-ACA, the analytical solution obtained in the above step (2) is concentrated by using a nanofiltration membrane with a molecular weight cut-off of 150 to 300 Daltons to obtain a concentrated solution; Add immobilized cephalosporin C acylase, at pH 8.00-8.60, temperature 5-30°C, crack CPC in the concentrated solution; after the cleavage, filter to remove immobilized cephalosporin C acylase , the resulting filtrate was adjusted to pH 3.00-5.50 with acid, and 7-ACA crystals were precipitated to obtain 7-ACA crystals.

[0034] Among them, the concentration of 7-ACA in the analysis solution obtained in the above step (2) is about 5.0 to 10.0 g / L, which does not reach the concentration required for crystallization, and needs to be concentrated to 15.0 to 25.0 g / L through a nanofiltration membrane, preferably 20.0 to 25.0 g / L. g / L; the nanofiltration membrane should choose a nanofiltration membrane with a molecular weight cut-off of 100-300 ...

Embodiment 1

[0039] According to the following steps, the active ingredient in the 7-ACA crystallization mother liquor produced by the enzymatic cleavage method is comprehensively recovered:

[0040] (1) Preparation of 7-ACA mother liquor concentrate

[0041] Take 20.0L of the 7-ACA crystallization mother liquor after 7-ACA crystallization separation, the concentration of 7-ACA in the mother liquor is 1.1g / L, the concentration of D-α-aminoadipic acid is 11.6g / L, the concentration of CPC is 0.3g / L, pH5 .19.

[0042] Slowly adjust the above-mentioned 7-ACA crystallization mother liquor with 15wt% sodium hydroxide solution until the solution is clear, and the pH is adjusted to 7.10, and then use a nanofiltration membrane with a molecular weight cut-off of 160 Daltons to store the 7-ACA crystallization mother liquor at 5-8°C Concentrate to 2.0L, wherein the concentration of 7-ACA is 10.6g / L, the concentration of D-α-aminoadipic acid is 113.3g / L, and the concentration of CPC is 2.9g / L.

[004...

Embodiment 2

[0050] According to the following steps, the active ingredient in the 7-ACA crystallization mother liquor produced by the enzymatic cleavage method is comprehensively recovered:

[0051] (1) Preparation of 7-ACA mother liquor concentrate

[0052] Take the enzymatic cleavage method after 7-ACA crystal separation to produce 20.0L of 7-ACA crystallization mother liquor, the concentration of 7-ACA in the mother liquor is 1.0g / L, the concentration of D-α-aminoadipic acid is 11.2g / L, and the concentration of CPC is 0.5g / L, pH5.16.

[0053] Slowly adjust the above-mentioned 7-ACA crystallization mother liquor with 15wt% sodium hydroxide solution until the solution is clear, and the pH is adjusted to 6.90, and then use a nanofiltration membrane with a molecular weight cut-off of 160 Daltons to store the 7-ACA crystallization mother liquor at 5-8°C Concentrate to 2.5L, in which the concentration of 7-ACA is 7.8g / L, the concentration of D-α-aminoadipic acid is 89.2g / L, and the concent...

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Abstract

The invention belongs to the technical field of pharmacy, and relates to a comprehensive recovery method for effective ingredients in 7-amidogen cephalosporins alkanes acid crystallization mother liquor produced through an enzymatic hydrolysis method. The method comprises the following steps that 1, the 7-ACA mother liquor is prepared; 2, 7-ACA and CPC are adsorbed and decomposed; 3, D-alpha-aminoadipicacid is prepared; 4, 7-ACA is prepared. 7-ACA and D-alpha-aminoadipicacid in the 7-ACA crystallization mother liquor are separated through the specific adsorption effect of macroreticular resin on 7-ACA, appropriate decomposition agents is adopted for decomposing 7-ACA and CPC adsorbed to the resin, then D-alpha-aminoadipicacid and 7-ACA are recovered from adsorption raffinate and decomposition liquid respectively, the quality of the recovered 7-ACA products is superior to that of 7-ACA products obtained through the enzymatic hydrolysis method, and D-alpha-aminoadipicacid can be used for preparing a fermentation medium of CPC. The effective ingredients in the mother liquor are successfully recovered through the brand-new process, the emission of high-concentration waste water is greatly reduced, the cost for treating sewage is reduced, and environment-friendly, clean and green production is achieved.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and relates to a method for comprehensively recovering active ingredients in the mother liquor of 7-aminocephalosporanic acid crystals produced by enzymatic cleavage, more specifically, to the method of enzymatic cleavage to produce 7-amino Comprehensive recovery method for cephalosporanic acid and D-alpha-aminoadipic acid. Background technique [0002] 7-amino-cephalosporanic acid (7-amino-cephalosporanic acid), referred to as 7-ACA, is the most commonly used core in cephalosporins. It has two active groups, namely the 3-position acetoxy group and the 7- The amino group at the position is connected with different side chains on these two active groups to form cephalosporin antibiotics with different properties. This type of antibiotic can effectively inhibit the synthesis of bacterial cell walls, but human cells have no cell walls, so they have excellent selectivity, good safety, and strong ba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/40C07C227/42C07C229/24C07D501/12C07D501/18C12P35/02
Inventor 张俊波刘君臣侯瑞峰王雁安琪郭恒龙
Owner SHANXI WEIQIDA PHARMA IND
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