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Pyrroloquinoline quinone disodium salt crystal and preparation method thereof

A technology of pyrroloquinoline quinone disodium salt and pyrroloquinoline quinone, which is applied in the field of pyrroloquinoline quinone disodium salt crystal and its preparation, can solve the problems that affect the popularization and use of PQQ, easy moisture absorption, poor stability, etc., and achieve Regular crystal shape, good stability and good reproducibility

Active Publication Date: 2019-01-04
SHANDONG JINCHENG BIO PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the report of the above-mentioned literature and the inventor’s research on the above-mentioned crystal, it is found that the existing PQQ disodium salt crystal is easy to absorb moisture, has poor stability, and is not suitable for development, which affects the popularization and use of PQQ

Method used

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  • Pyrroloquinoline quinone disodium salt crystal and preparation method thereof
  • Pyrroloquinoline quinone disodium salt crystal and preparation method thereof
  • Pyrroloquinoline quinone disodium salt crystal and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0055]Add 100 g of pyrroloquinoline quinone acid in free form to 10 L of water, stir to form a suspension, add sodium hydroxide to adjust the pH to 8.5, and stir for 15 minutes to completely dissolve; filter to obtain the filtrate, slowly add hydrochloric acid under stirring to adjust the pH to 3.5; Nanofiltration desalination of nanofiltration membrane with a molecular weight of 150-300D, washing with purified water until the conductivity of the permeate is ≤50μS / cm, and ending; vacuum concentration and crystallization, the internal temperature of the feed liquid during the concentration process is 25-35°C; suction filtration, washing wet The product was vacuum-dried at 50°C for 6 hours to obtain 109.5 g of crystals. The obtained crystal is detected, and its purity measured by HPLC is 99.7%; the Na ion content is detected by cation chromatography, and the PQQ content is recorded in conjunction with the HPLC external standard method, and the mass ratio of PQQ and Na contained i...

Embodiment 2

[0057] Add 100 g of pyrroloquinoline quinone monosodium salt into 10 L of water, stir to form a suspension, add sodium hydroxide to adjust the pH to 7.5, and stir for 15 minutes to completely dissolve; filter to obtain the filtrate, slowly add hydrochloric acid to adjust the pH to 3.2 while stirring; Nanofiltration desalination of nanofiltration membrane with a molecular weight cut-off of 150-300D, washing with purified water until the conductivity of the permeate is ≤50μS / cm, and ending; vacuum concentration and crystallization, the internal temperature of the feed liquid during the concentration process is 25-35°C; suction filtration, washing The wet product was vacuum-dried at 60°C for 5 hours to obtain 96.8 g of crystals. The obtained crystal is detected, and its purity measured by HPLC is 99.8%; the Na ion content is detected by cation chromatography, and the PQQ content is recorded in conjunction with the HPLC external standard method, and the mass ratio of PQQ and Na con...

Embodiment 3

[0059] Add 100 g of pyrroloquinoline quinone trisodium salt into 10 L of water, stir to form a suspension, add sodium hydroxide to adjust the pH to 8.0, and stir for 15 minutes to completely dissolve; filter to obtain the filtrate, slowly add sulfuric acid under stirring to adjust the pH to 3.7; Nanofiltration desalination of nanofiltration membrane with a molecular weight cut-off of 150-300D, washing with purified water until the conductivity of the permeate is ≤50μS / cm, and ending; vacuum concentration and crystallization, the internal temperature of the feed liquid during the concentration process is 25-35°C; suction filtration, washing The wet product was vacuum-dried at 40°C for 10 hours to obtain 78.3 g of crystals. The obtained crystal is detected, and its purity measured by HPLC is 99.7%; the Na ion content is detected by cation chromatography, and the PQQ content is recorded in conjunction with the HPLC external standard method, and the mass ratio of PQQ and Na contain...

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Abstract

The purpose of the invention is to provide a pyrroloquinoline quinone disodium salt crystal which is simple and suitable for large-scale production and a preparation method thereof, wherein the preparation method of the pyrroloquinoline quinone disodium salt crystal comprises the following steps: the pH of an aqueous solution containing a pyrroloquinoline quinone disodium salt or an alkali metal salt thereof is adjusted to 7.5-8.5, then the acid is added to adjust the pH to 3.0-4.0, the pyrroloquinoline quinone disodium salt crystal is obtained by desalting, crystallizing and drying. The preparation method has the advantages of simple and easy to control, and the obtained pyrroloquinoline quinone disodium salt crystal is almost free of moisture absorption.

Description

technical field [0001] The invention relates to a pyrroloquinoline quinone disodium salt crystal and a preparation method thereof. Background technique [0002] Current studies have shown that pyrroloquinolinequinone (hereinafter referred to as PQQ) is the third coenzyme of oxidoreductases discovered after nicotinamide and flavin nucleotides. It is a small molecule compound found in microorganisms and is widely distributed in Among the various tissues and organs of the human body, it is called the fourteenth vitamin. PQQ has a variety of physiological functions, and has broad application prospects in food, medicine, cosmetics and other industries. The molecular weight of PQQ is 330.2, and its chemical name is: 4,5-Dihydro-4,5-dioxo-1H-pyrrolo[2,3-f]quinoline-2,7,9-tricarboxylic Acid, and its structural formula is as follows: [0003] [0004] PQQ widely exists in prokaryotic cells and eukaryotic tissues, such as Klebsiella pneumoniae (Klebsiellapneumoniae), Methylobacte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04
CPCC07B2200/13C07D471/04
Inventor 杨修亮李江涛孙国祥荣金雷徐克张成国
Owner SHANDONG JINCHENG BIO PHARMA CO LTD
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