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Comprehensive recovery method of effective components in enzymatic synthesized ampicillin crystal mother liquor

A technology for ampicillin and crystallization mother liquor, which is applied in the field of comprehensive recovery of active ingredients in enzymatic synthesis of ampicillin crystallization mother liquor, can solve problems such as waste of 6-APA, and achieve the effects of reducing discharge, efficient concentration, and realizing environmental protection, clean and green production.

Active Publication Date: 2018-02-16
SHANXI WEIQIDA PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Use the above method to reclaim D-phenylglycine from the mother liquor. Although ampicillin and D-phenylglycine methyl ester are hydrolyzed by enzymatic cleavage, ampicillin and D-phenylglycine methyl ester still remain in the mother liquor, and the mother liquor Medium 6-APA is wasted a lot

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Comprehensively recover the active ingredient in the ampicillin crystallization mother liquor according to the following steps:

[0038] (1) Adsorption and analysis of ampicillin, 6-APA and D-phenylglycine methyl ester

[0039] Get the enzymatic ampicillin crystallization mother liquor after ampicillin crystallization separation, wherein, D-phenylglycine concentration is 2.67g / L, and 6-APA concentration is 1.44g / L, and D-phenylglycine methyl ester concentration is 0.89g / L, Ampicillin concentration is 4.08g / L, pH value is 4.95. This mother liquor passes through macroporous adsorption resin column bed (resin model is XAD-6, loading capacity 2L, aspect ratio is 4) with the flow velocity of per hour 4L, ampicillin, 6-APA and D-phenylglycine methyl ester are adsorbed on On the resin, while D-phenylglycine is not adsorbed by the resin, it flows through the resin with the mother liquor and is collected as the adsorption residue. When one of ampicillin, 6-APA and D-phenylglyc...

Embodiment 2

[0047] Comprehensively recover the active ingredient in the ampicillin crystallization mother liquor according to the following steps:

[0048] (1) Adsorption and analysis of ampicillin, 6-APA and D-phenylglycine methyl ester

[0049] Get the enzymatic ampicillin crystallization mother liquor after ampicillin crystallization separation, wherein, D-phenylglycine concentration is 3.11g / L, and 6-APA concentration is 1.55g / L, and D-phenylglycine methyl ester concentration is 0.96g / L, Ampicillin concentration is 4.15g / L, pH value is 5.05. This mother liquor passes through macroporous adsorption resin column bed (resin model is XAD-8, loading capacity 2L, aspect ratio is 8) with the flow velocity of per hour 4L, and ampicillin, 6-APA and D-phenylglycine methyl ester are adsorbed on On the resin, while D-phenylglycine is not adsorbed by the resin, it flows through the resin with the mother liquor and is collected as the adsorption residue. When one of ampicillin, 6-APA and D-phenyl...

Embodiment 3

[0057] Comprehensively recover the active ingredient in the ampicillin crystallization mother liquor according to the following steps:

[0058] (1) Adsorption and analysis of ampicillin, 6-APA and D-phenylglycine methyl ester

[0059] Get the enzymatic ampicillin crystallization mother liquor after ampicillin crystallization separation, wherein, D-phenylglycine concentration is 3.45g / L, 6-APA concentration is 1.55g / L, D-phenylglycine methyl ester concentration is 0.97g / L, Ampicillin concentration is 3.24g / L, pH value is 4.99. This mother liquor passes through macroporous adsorption resin column bed (resin model is XAD-6, loading capacity 2L, aspect ratio is 8) with the flow rate of per hour 4L, ampicillin, 6-APA and D-phenylglycine methyl ester are adsorbed on On the resin, while D-phenylglycine is not adsorbed by the resin, it flows through the resin with the mother liquor and is collected as the adsorption residue. When one of ampicillin, 6-APA and D-phenylglycine methyl e...

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Abstract

The invention belongs to the pharmaceutical technical field, and relates to a comprehensive recovery method of effective components in enzymatic synthesized ampicillin crystal mother liquor. D-phenylglycine is separated with ampicillin, 6-APA and D-phenylglycine methyl ester by a separation method of macroporous adsorption resin, D-phenylglycine is not adsorbed by the resin and enters an adsorption residual liquid, the adsorption residual liquid is subjected to electrodialysis, reverse osmosis concentration and crystallization, and then high-quality D-phenyglycine is recycled; ampicillin, 6-APA and D-phenylglycine methyl ester adsorbed on the resin are desorbed and are subjected to nanofiltration concentration, the obtained nanofiltration concentrate can be directly used as reaction bottomwater in an ampicillin enzymatic synthesis process so as to be recycled and reused. The effective components of D-phenylglycine, ampicillin, 6-APA and D-phenylglycine methyl ester in the enzymatic ampicillin crystal mother liquor are comprehensively recycled, economic benefits are created, at the same time, the discharge of high-concentration wastewater is reduced, and the environmental-protection, clean and green production is realized.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and relates to a method for comprehensively recovering active ingredients in ampicillin crystallization mother liquor synthesized by enzymatic method. Background technique [0002] Ampicillin, chemical name (2S,5R,6R)-3,3-dimethyl-6-[(R)-2-amino-2-phenylacetamido]-7-oxo-4-thia- 1-Azabicyclo[3.2.0]heptane-2-carboxylic acid, its free acid contains three molecules of crystal water, it is a commonly used penicillin broad-spectrum β-lactam antibiotics. [0003] Ampicillin has a strong bactericidal effect and the ability to penetrate the cell wall, and is one of the most widely used oral penicillins at present. The preparation method of ampicillin has two kinds of chemical synthesis method and enzymatic method, chemical method is because of its complex reaction steps, harsh synthesis conditions, and the whole reaction process needs to use various organic chemical raw materials, produces a large amoun...

Claims

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Application Information

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IPC IPC(8): C07D499/68C07D499/42C07C227/40C07C229/36
Inventor 袁智灏安雪飞李树有刁夏刘君臣
Owner SHANXI WEIQIDA PHARMA IND
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