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Method for separating and purifying pyrroloquinoline quinone

A technology for separation and purification of pyrroloquinoline quinone, which is applied in the field of separation and purification of pyrroloquinoline quinone, can solve problems such as lack of attention and influence on product yield, achieve the effect of improving purity and yield, and reducing subsequent processing steps

Inactive Publication Date: 2021-01-08
内蒙古拜克生物有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is proved by experiments that the method of the invention has the characteristics of simple process operation, high degree of cohesion, high product recovery and high purity, but according to the records of this application, it can be known that it does not pay attention to the yield of the final product pyrroloquinoline quinone, and its The use of macroporous resins followed by purification with hydrophilic silica gel fillers will affect the yield of the product

Method used

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  • Method for separating and purifying pyrroloquinoline quinone

Examples

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Embodiment 1

[0051] Embodiment 1 A method for separating and purifying pyrroloquinoline quinone, comprising the following steps:

[0052] (1) Adjust the pH of 30L of fermented broth containing pyrroloquinoline quinone to 2.0, then add 150g of water-soluble starch and alginic acid with a mass ratio of 2:1, let stand at 30°C for 10 minutes, and then add diatomaceous earth 150g carries out plate and frame filtration, obtains filtrate;

[0053] (2) Concentrate the filtrate obtained in step (1), enrich it through XDA-7 and XDA-1 mixed macroporous resin with a volume ratio of 1:2, and then use water for elution at a rate of 2.5BV / h , to obtain the eluate;

[0054] (3) Concentrating the eluent obtained in step (2) and adding acid to adjust the pH value to 3.0, so that pyrroloquinoline quinone is crystallized from the eluent to obtain coarse crystals of pyrroloquinoline quinone;

[0055] (4) Recrystallize the crude pyrroloquinoline quinone crystals obtained in step (3) to obtain pyrroloquinoline...

Embodiment 2

[0058] Embodiment 2 A method for separation and purification of pyrroloquinoline quinone, comprising the following steps:

[0059] (1) Adjust the pH of 30L of fermented broth containing pyrroloquinoline quinone to 3.0, then add 300g of water-soluble starch and alginic acid with a mass ratio of 5:1, let stand at 30°C for 20 minutes, and then add diatomaceous earth 150g carries out plate and frame filtration, obtains filtrate;

[0060] (2) Concentrate the filtrate obtained in step (1), enrich it with XDA-7 and XDA-1 mixed macroporous resin with a volume ratio of 1:3, and then use water for elution with an elution rate of 3BV / h, get eluent;

[0061] (3) Concentrating the eluent obtained in step (2) and adding acid to adjust the pH value to 3.2, so that pyrroloquinoline quinone is crystallized from the eluent to obtain coarse crystals of pyrroloquinoline quinone;

[0062] (4) Recrystallize the crude pyrroloquinoline quinone crystals obtained in step (3) to obtain pyrroloquinolin...

Embodiment 3

[0065] Embodiment 3 A method for separation and purification of pyrroloquinoline quinone, comprising the following steps:

[0066] (1) Adjust the pH of 30L of fermented broth containing pyrroloquinoline quinone to 2.5, then add 240g of water-soluble starch and alginic acid with a mass ratio of 4:1, let it stand at 30°C for 10-20 minutes, and then add silicon Alginate 120g carries out plate and frame filtration, obtains filtrate;

[0067] (2) Concentrate the filtrate obtained in step (1), enrich it with XDA-7 and XDA-1 mixed macroporous resin with a volume ratio of 1:2-3, and then use water to elute with an elution rate of 2.5- 3BV / h, get the eluate;

[0068] (3) Concentrating the eluent obtained in step (2) and adding acid to adjust the pH value to 3.0-3.2, so that pyrroloquinoline quinone is crystallized from the eluent to obtain coarse crystals of pyrroloquinoline quinone;

[0069] (4) Recrystallize the crude pyrroloquinoline quinone crystals obtained in step (3) to obtain...

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Abstract

The invention provides a method for separating and purifying pyrroloquinoline quinone, and belongs to the field of biochemical engineering. In the implementation process, a mixture of a nonionic flocculating agent and an anionic flocculating agent is added into fermentation liquor containing pyrroloquinoline quinone to serve as the flocculating agent, impurities can be better agglutinated, specifically, a mixture of water-soluble starch and alginic acid with the mass ratio of 2-5: 1 is used as the flocculating agent, protein impurities and metal ion impurities are deposited, and removed preferably; mixed macroporous resin of XDA-7 and XDA-1 with the volume ratio of 1: 2-3 is used in the purification process, pigment impurities can be removed, pyrroloquinoline quinone can be better purified, high-purity pyrroloquinoline quinone can be obtained only through elution with pure water, recrystallization is carried out subsequently, and a pyrroloquinoline quinone pure product can be obtained;the method is simple to operate and low in cost.

Description

technical field [0001] The invention belongs to the field of biochemical industry, and in particular relates to a method for separating and purifying pyrroloquinoline quinone. Background technique [0002] Pyrroloquinoline quinone (PQQ) is a water-soluble quinone compound widely found in food and animals. It is the coenzyme of glucose dehydrogenase and alcohol dehydrogenase. The chemical name is 4,5-dihydro-4,5 -dioxide-1-hydropyrrole(2,3f)quinone-2,7,9-tricarboxylic acid. PQQ has been proven to have very important physiological functions and is considered a new B vitamin. Studies have shown that PQQ can be used to treat neurological and mental disorders, because PQQ can prevent the formation of amyloid, Inhibition of cytotoxicity of C-terminally shortened variant synuclein. Moreover, PQQ can effectively prevent neurodegeneration caused by oxidative stress. In short, PQQ has the following four functions related to the nervous system: (1) anti-oxidation and scavenging free...

Claims

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Application Information

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IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 侯争平陈锋吉毅楠刘培
Owner 内蒙古拜克生物有限公司
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