Method for preparing pyrroloquinoline quinone by using 2-keto-L gulonic acid crystallization mother liquor

A technology of pyrroloquinoline quinone and crystallization mother liquor, applied in the direction of fermentation and the like, can solve the problems of low PQQ fermentation yield, failure to meet production requirements, large environmental damage, etc., and achieves good antioxidant effect, high antioxidant activity, and simple steps. Effect

Active Publication Date: 2019-06-28
新拓洋生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reported PQQ chemical synthesis method requires more than ten steps of reaction to obtain, the yield is low, and a large amount of toxic reagents and heavy metal catalysts are required, which is relatively harmful to the environment
The main problem of preparing PQQ by microbial fermentation is that the yield of PQQ fermentation is very low (reported only one hundred micrograms per liter), far from reaching the production requirements

Method used

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  • Method for preparing pyrroloquinoline quinone by using 2-keto-L gulonic acid crystallization mother liquor
  • Method for preparing pyrroloquinoline quinone by using 2-keto-L gulonic acid crystallization mother liquor
  • Method for preparing pyrroloquinoline quinone by using 2-keto-L gulonic acid crystallization mother liquor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1, the preparation of 2-keto-L-gulonic acid crystallization mother liquor

[0028] D-Sorbitol produces sodium 2-keto-L-gluconate mash through a two-step fermentation process. The 2-keto-L-gulonic acid sodium mash is filtered by ultrafiltration to remove impurities such as protein and hyphae, and then passed through a resin column for resin exchange to produce a 2-keto-L-gulonic acid resin exchange solution. Measure 1L of 2-keto-L-gulonic acid resin exchange solution, and concentrate under reduced pressure (temperature 55-80°C, vacuum degree -0.055--0.09MPa), wherein the content of 2-keto-L-gulonic acid is 123mg / mL, then cooled to 4°C to crystallize, and centrifuged to obtain 70mL of 2-keto-L-gulonic acid primary mother liquor. The primary mother liquor of 2-keto-L-gulonic acid is concentrated under reduced pressure (temperature 50-70°C, vacuum degree -0.065--0.1MPa), then cooled to 4°C to crystallize and centrifuged to obtain 2-keto-L-gulone Acid secondary ...

Embodiment 2

[0031] Utilize the method for preparing PQQ from 10L scale 2-keto-L-gulonic acid crystallization mother liquor, comprising the following steps:

[0032] 1. Precipitation and impurity removal

[0033] Use the iron and calcium salt precipitation method to remove impurities, and 1L of divalent metal ions with a total concentration of 1mol / L CaCl 2 and FeCl 2 Add the solution to 10L 2-keto-L-gulonic acid crystallization mother liquor, then add 200g Ca(OH) 2 Adjust the pH, stir for 1 h, and separate by filtration to obtain a precipitate and a supernatant.

[0034] 2. Extraction and enrichment

[0035]Add extract in supernatant, carry out organic solvent ion-pair complex extraction and enrichment, the volume ratio of extract and supernatant is 1:1, and extract comprises extraction agent (trioctylamine, ammoniacal liquor (mass fraction 31.2%) )) and diluent (n-butanol, tert-butanol, n-octanol), its volume ratio is n-butanol: tert-butanol: n-octanol: trioctylamine: ammoniacal liqu...

Embodiment 3

[0044] Utilize the method for preparing PQQ from 10L scale 2-keto-L-gulonic acid crystallization mother liquor, comprising the following steps:

[0045] 1. Precipitation and impurity removal

[0046] Use zinc and manganese salt precipitation to remove impurities, and 2L of ZnCl with a total concentration of divalent metal ions of 3mol / L 2 and MnCl 2 Add the solution to 10L 2-keto-L-gulonic acid crystallization mother liquor, then add 100g Ca(OH) 2 Adjust the pH, stir for 1 h, and separate by filtration to obtain a precipitate and a supernatant.

[0047] 2. Extraction and enrichment

[0048] Add extract to supernatant, carry out organic solvent ion-pair complexation extraction and enrichment, the volume ratio of extract and supernatant is 3:1, and extract includes extraction agent (trioctylamine, ethylenediamine) and dilution Agent (n-butanol, n-propanol, isoamyl alcohol), its volume ratio is n-butanol: n-propanol: isoamyl alcohol: trioctylamine: ethylenediamine=6:2:2:2:0.5...

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Abstract

The invention discloses a method for preparing pyrroloquinoline quinone by using a 2-keto-L-gulonic acid crystallization mother liquid, which is prepared by using the 2-keto-L-gulonic acid crystallization mother liquid as the raw material liquid to extract 4,5-dihydro-4,5-dioxo-1H-pyrrolo[2,3-f]quinoline-2,7,9-tricarboxylic acid. The method for preparing 4,5-dihydro-4,5-dioxo- 1H-pyrrolo[2,3-f]quinolone-2,7,9-tricarboxylic acid by using the 2-keto-L-gulonic acid crystallization mother liquid does not need to undergo fermentation, ion exchange, concentration and other processes, and the steps are simple, a large amount of cost is saved, waste is changed into treasure, resources are fully utilized, and the method is environment-friendly. Moreover, the product pyrroloquinoline quinone prepared by using the 2-keto-L-gulonic acid crystallization mother liquid has a reduced state and has better antioxidant effect. The method for preparing pyrroloquinoline quinone by using the 2-keto-L-gulonic acid crystallization mother liquid has the advantages of simple steps, high separation efficiency and environmental protection.

Description

technical field [0001] The invention relates to a method for preparing pyrroloquinoline quinone, in particular to a method for preparing 4,5-dihydro-4,5-dioxo-1H-pyrrolo[ 2,3-f] quinoline-2,7,9-tricarboxylic acid method. Background technique [0002] Pyrroloquinoline quinone (Pyrroloquinoline quinone, PQQ, also known as 4,5-dihydro-4,5-dioxo-1H-pyrrolo[2,3-f]quinoline-2,7,9-tricarboxylic acid ) includes oxidized and reduced forms. It is the third type of coenzyme found after riboflavin and nicotinamide. It is a member of B vitamins. As a prosthetic group of various enzymes, it has important physiological activities for living organisms. Studies have found that mice lacking PQQ grow slowly, have fragile skin, osteoporosis, abnormal bones, low immune response, poor reproductive ability, and are prone to joint inflammation. It is worth noting that PQQ cannot be synthesized in mammals and must be ingested from the outside to meet the needs of life activities. Therefore, PQQ ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P7/66
Inventor 马科秦天苍钟桂芳苏筱渲叶建斌代军帅勾丽莉
Owner 新拓洋生物工程有限公司
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