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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 the problems of complex process and high cost, and achieve the effect of simple process, low cost, and improved purity and yield

Active Publication Date: 2020-09-08
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a method for separation and purification of pyrroloquinoline quinone, so as to at least overcome the defects of complex process and high cost in the prior art

Method used

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  • Method for separating and purifying pyrroloquinoline quinone
  • Method for separating and purifying pyrroloquinoline quinone
  • Method for separating and purifying pyrroloquinoline quinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The buffer used in this embodiment (8%NaCl-1%NH 4 Ac-PH2.0) is prepared according to the following process: water, sodium chloride and ammonium acetate are mixed into a mixed solution, and its pH is adjusted to 2.0 with hydrochloric acid to obtain a buffer solution; wherein, the mass concentration of sodium chloride is 8%, and the acetic acid The mass concentration of ammonium is 1%.

[0035] Get 10 liters of plate and frame filtrate, add 0.05 gram of sodium chloride therein, adjust pH to carry out precipitation 1 hour after being 3.5, filter and remove precipitate, obtain filtrate (about 10.3 liters, be recorded as filtrate after precipitation); After the ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 5000Da, it is concentrated to a volume of 5 liters of concentrate (the content of pyrroloquinoline quinone in the concentrate is about 6 ~ 7 grams);

[0036] Add 15 grams of oxalic acid to the above concentrated solution, adjust the pH to 2....

Embodiment 2

[0043] Get 10 liters of plate and frame filtrate, add 0.05 gram of sodium chloride therein, adjust the pH to 4.0 and carry out precipitation for 1 hour (to separate out the protein), filter to remove the precipitate, and obtain the filtrate (about 10.5 liters, which is recorded as the filtrate after precipitation); This filtrate is after the ultrafiltration membrane ultrafiltration that is 5000Da through molecular weight cut off, is the nanofiltration membrane nanofiltration that is 100-200Da through molecular weight cut off and concentrates to the concentrated solution that volume is 4.22 liters (the content of PQQ in the concentrated solution is about 6- 7 grams);

[0044] Add 8.4 oxalic acid to the concentrated solution to adjust the pH to 2.0, then add 5 liters of n-butanol for extraction to obtain an extract; add 8% NaCl-1% NH to the extract 4 Ac-PH2.0 back extraction 2 times, the addition amount of each buffer solution is 5 liters, obtains back extraction liquid (about 1...

Embodiment 3

[0051] The present embodiment carries out following stripping comparative verification experiment:

[0052] Take 10 liters of plate and frame filtrate, add 0.05 gram of sodium chloride therein, adjust the pH to be 3.5, carry out precipitation for 1 hour, filter and remove the precipitate, obtain filtrate (about 10.3 liters); After membrane ultrafiltration, it is concentrated to a volume of 5.2 liters of concentrated solution (the content of PQQ in the concentrated solution is about 6-7g) through nanofiltration membrane nanofiltration with a molecular weight cut-off of 100-200Da; add 15g oxalic acid in the concentrated solution After adjusting the pH to 2.0, add 5 liters of n-butanol for extraction to obtain an extract;

[0053] Take 4 liters of the above extract, divide it equally into 2 parts, numbered A and B, and carry out test 1 and test 2 respectively:

[0054] Test 1: Buffer used (1% NH 4 AC-PH is 4.0) prepared according to the following process: dissolving ammonium ac...

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Abstract

The invention provides a pyrroloquinoline quinone separation and purification method, which comprises: (1) pretreatment: removing proteins from a filtrate obtained by filtering a pyrroloquinoline quinone-containing fermentation broth under an acidic condition, and carrying out ultrafiltration and nanofiltration concentration to obtain a pyrroloquinoline quinone concentrated solution; (2) extraction-back extraction: adding oxalic acid to the concentrated solution, controlling the pH value of the system to be 2.0-3.0, extracting with an organic solvent to obtain an extraction solution, and carrying out back extraction on the extraction solution by using a buffer solution with the pH value of 2.0 to 3.0 to obtain a back extraction solution, wherein the ratio of the addition amount of oxalicacid to the mass volume of the concentrated solution is (0.1-1 g):100 mL; and (3) crystallization-decolorization-recrystallization: crystallizing the back extraction solution to obtain a crude crystal, and carrying out decoloration treatment and recrystallization on the crude crystal to obtain a pyrroloquinoline quinone product. The method can be used for efficiently extracting pyrroloquinoline quinone and has the advantages of simple process, low cost and the like.

Description

technical field [0001] The invention relates to a method for separating and purifying pyrroloquinoline quinone, which belongs to the field of microbial fermentation and pharmacy. Background technique [0002] Pyrroloquinoline quinone (Pyrroloquinoline quinone, PQQ), chemical name is 4,5-dihydro-4,5-dioxide-1-hydropyrrole (2,3f) quinone-2,7,9-tricarboxylic acid, alias Methaxatin, is a new coenzyme. In 1979, Salisbury et al. first isolated it from methylotrophic bacteria and identified it as a redox cofactor of membrane-bound dehydrogenase in bacterial cells. It transports electrons with the respiratory chain and is also a new B vitamin. . Some recent studies have found that PQQ has an abnormally high redox cycle ability, and has great application potential in anti-aging of nerve cells and anti-cancer. Meanwhile, in 2008, the U.S. Food and Drug Administration (FDA) approved cognitive function food with PQQ as the main ingredient. Therefore, PQQ has a good application prosp...

Claims

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Application Information

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IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 赵燕张葵
Owner NEW FOUNDER HLDG DEV LLC
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