Method for separating and purifying pyrroloquinoline quinone disodium salt based on fermentation liquid composite salting-out

A technology for pyrroloquinoline quinone disodium salt and pyrroloquinoline quinone, which is applied in the fields of biochemical industry and separation and purification, can solve the problems of obtaining pyrroloquinoline quinone disodium salt by separation, and does not involve high-purity separation and extraction of fermentation broth. The effect of shortening the process cycle, short production cycle and reducing waste water discharge

Active Publication Date: 2019-01-11
福建康鸿生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The above-mentioned prior art about pyrroloquinoline quinone sodium salt is all about the preparation of sodium salt from pyrroloquinoline quinone, and there is no description related to the high-purity separa

Method used

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Examples

Experimental program
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Example Embodiment

[0073] Example 1

[0074] Preparation of polyvinyl alcohol magnetic microspheres

[0075] Fe 3 O 4 Preparation of magnetic fluid: at 50℃, 0.5mol / L FeCl 2 Solution and 0.5mol / L FeCl 3 The solution was added to a three-necked flask in a volume ratio of 1:2, while stirring in the disperser (14000r / min), a molar ratio of 3mol / L NaOH solution was added dropwise, and the temperature was raised to 80°C and stirred for 40 minutes. After the reaction was completed Separate the precipitate with a magnetic field, repeatedly wash with distilled water until the supernatant is neutral, and dry to obtain black powdery Fe 3 O 4 Magnetic fluid

[0076] Preparation of polyvinyl alcohol magnetic microspheres: Fully swell the PVA with distilled water, stir at 90°C to prepare a 9% PVA aqueous solution, and add an appropriate amount of Fe 3 O 4 Pour the magnetic fluid into the PVA solution, stir and mix, disperse with a cell pulverizer for 20 minutes, then pour into the dispersion medium (oil: Tween: n-bu...

Example Embodiment

[0077] Example 2

[0078] Preparation of pyrroloquinoline quinone disodium salt

[0079] S1: Separate about 21L of pyrroloquinoline quinone fermentation broth through a ceramic ultrafiltration membrane for the first filtration to obtain a pyrroloquinoline quinone primary filtrate, with a filtration yield of 98.2%;

[0080] S2: Take the primary filtrate obtained in the previous step, adjust the concentration of pyrroloquinoline quinone to about 800-850mg / L, adjust the pH to 4.3 with sulfuric acid, stir for 1 hour and then filter. Before filtering, pre-coat a layer of mesopores on the filter membrane Silica (particle size: 600nm, thickness: 0.3mm), filtered to obtain the de-impurity filtrate, the chromatographic purity is 83.6%;

[0081] S3: Sulfuric acid was added dropwise to the impurity removal filtrate obtained in the upper step to make the pH to 2.4, and the polyvinyl alcohol magnetic microspheres prepared in Example 1 were added to 3.5wt%. After the adsorption reaction for 3 hours...

Example Embodiment

[0087] Example 3

[0088] Preparation of pyrroloquinoline quinone disodium salt

[0089] S1: The pyrroloquinoline quinone fermentation broth is filtered once through the ceramic membrane separation technology to obtain the pyrroloquinoline quinone primary filtrate with a filtration yield of 98%;

[0090] S2: Take the primary filtrate obtained in the previous step, adjust the pH to 4.3 with sulfuric acid, remove impurities, stir for 1h and then filter. Before filtering, pre-coat a layer of mesoporous silica (particle size 0.6-0.7um) on the filter membrane , Add mesoporous silica in batches during the filtration process, and add 3 times in total until the filtration is completed (the total amount is the same as in Example 1) to obtain the impurity removal filtrate with a chromatographic purity of 86.1%;

[0091] S3: Add sulfuric acid dropwise to the impurity removal filtrate obtained in the upper step to adjust the pH to 2.4, add 5 wt% of the polyvinyl alcohol magnetic microspheres prep...

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Abstract

The invention discloses a method for separating and purifying pyrroloquinoline quinone disodium salt based on a fermentation raw material liquid. The method comprises: (1) primary filtration, (2) secondary filtration, (3) extraction of pyrroloquinoline quinone, (4) primary salting-out, (5) decolorization with activated carbon, (6) secondary salting-out, and (7) crystallization. The method has simple processes, realizes a low cost, can effectively shorten the product purification cycle, has a high product recovery rate and realizes the product purity of 99.5%.

Description

technical field [0001] The invention belongs to the technical field of biochemical industry and separation and purification, and in particular relates to a separation and purification method for obtaining pyrroloquinoline quinone disodium salt from fermentation liquid. Background technique [0002] The chemical name of pyrroloquinoline quinone (PQQ) is 4,5-dihydro-4,5-dioxide-1-hydropyrrole (2,3f)quinone-2,7,9-tricarboxylic acid, and its structural formula is as follows: It is a crystal at room temperature, but its spectral properties are quite special. The absorption coefficient of PQQ at ultraviolet 249nm wavelength is 18400mol -1 cm -1 . It mainly participates in the redox process catalyzed by the enzyme as an electron acceptor or donor, and the three carboxyl groups of the ortho-quinone in its chemical structure are its important functional groups. [0003] PQQ is a cofactor involved in redox reactions and acts as a coenzyme for many enzymes, such as dehydrogenases, ...

Claims

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Application Information

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IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 张茂华蒋永飞赖庆云赵正国陈亮
Owner 福建康鸿生物科技有限公司
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