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Purification process for preparing high-purity coenzyme Q10

A high-purity, coenzyme technology, used in quinone separation/purification, organic chemistry, etc., can solve the problems of rising industrial application costs, low reuse times of silica gel, harsh industrial operating environment, etc., achieve good purification effect, reduce silica gel purification pressure , the effect of high number of reuse

Active Publication Date: 2013-06-12
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current method has the following disadvantages: the high cost of activated alumina increases the cost of industrial application; the number of times of silica gel reuse is low; resulting in harsh industrial operating environment, easy to cause environmental pollution, and increase follow-up costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh 1g of coenzyme Q10 crude extract and dissolve it in 300ml ethanol, fill the separation column with HZ816 resin, load the sample at 2 times the column volume per hour, elute with ethanol solution for 5 times the column volume after loading, and remove most of the impurities Use acetone solution to elute 2 times the column volume. Concentrate the obtained eluent under reduced pressure, dissolve the obtained concentrate with 100ml of ethanol, let it stand at 0°C for 12 hours, and recrystallize twice to obtain 93.4% coenzyme Q10 crystals. Load the obtained coenzyme Q10 crystals: chromatographic silica gel = 1:25, use n-hexane: ethyl acetate = 20:1 as the eluent, collect the coenzyme Q10, and concentrate and dry the obtained coenzyme Q10 solution under reduced pressure to obtain a purity of ≥98%. crystals.

Embodiment 2

[0038] Weigh 1 g of the crude coenzyme Q10 extract and dissolve it in 300 ml of acetone: water = 8:1. Fill the separation column with HZ820 resin, load the sample at 3 times column volume / hour, elute 5 times the volume with acetone: water = 6:1 solution after loading, remove most of the impurities and use ethyl acetate solution to elute 2 times the column volume. Concentrate the obtained eluent under reduced pressure, dissolve the obtained concentrate with 50 ml of acetone solution, let it stand at 0° C. for 12 hours, and recrystallize twice to obtain 92.5% coenzyme Q10 crystals. The resulting coenzyme Q10 crystals: chromatographic silica gel mass ratio 1:25 is loaded on the sample, and the coenzyme Q10 is collected by using n-hexane: ethyl acetate volume ratio 30:1 as the eluent, and the obtained coenzyme Q10 solution is concentrated and dried under reduced pressure to obtain a purity ≥ 98% crystalline.

Embodiment 3

[0040] Weigh 1 g of coenzyme Q10 crude extract and dissolve it in 300 ml of acetone:water mixed solution with a volume ratio of 20:1. Fill the separation column with HZ830 resin, load the sample at 3 times the column volume / hour, and elute 5 times the volume with a solution of acetone:water with a volume ratio of 7:1 after loading the sample. After removing most of the impurities, use acetone solution to elute 2 times the column volume. The obtained eluate was concentrated under reduced pressure, and the obtained concentrate was dissolved in 30 ml of ethyl acetate, left to stand at 0° C. for 12 hours, and recrystallized twice to obtain 91.4% coenzyme Q10 crystals. The obtained coenzyme Q10 crystals: chromatographic silica gel mass ratio 1:25 is loaded on the sample, and petroleum ether: ether volume ratio 25:1 is used as the eluent to collect coenzyme Q10. The obtained coenzyme Q10 solution is concentrated and dried under reduced pressure to obtain a purity of ≥98%. crystals....

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Abstract

The invention relates to a purification process for preparing high-purity coenzyme Q10 from crude coenzyme Q10 extracts obtained from thallus fermentation, which belongs to the technical field of compound separation purification. The purification process is characterized by sequentially comprising the following steps of: carrying out adsorbent resin adsorption, elution, concentration, crystallization and recrystallization on the crude coenzyme Q10 extracts; then, carrying out chromatography on a silicagel column; and purifying and refining by using a petroleum ether -aether or normal hexane-ethyl acetate mixed solvents as eluant. The invention has the following advantages that by adopting an adsorbent resin, good adsorption performance can be exerted on the coenzyme Q10, the desorption operation is simple, the stability is good, and the adsorbent resin can be reused many times; and by combining the adsorbent resin with the silica gel chromatography method, the silica gel utilization rate is high, the required silica gel is low quantity and can maintain good purification effect after being reused more than 10 times, the waste quantity of the silica gel is small, and the solvents can be recycled so that the purpose of environment protection is achieved. The production operation is simple and convenient, and the purity of the obtained coenzyme Q10 is higher than or equal to 98 percent.

Description

technical field [0001] The invention belongs to the technical field of compound separation and purification, and relates to a purification process of biomedical product coenzyme Q10, in particular to a process for separating and purifying coenzyme Q10 from a coenzyme Q10 crude extract obtained from bacterial fermentation. Background technique [0002] Coenzyme Q10 (coenzyme Q10), also known as ubiquinone, is a fat-soluble quinone compound with a structure similar to vitamin K. It is widely distributed in nature and mainly exists in yeast, plant leaves, seeds and cells of heart, liver and kidney of animals. [0003] American scholar Frederick first isolated coenzyme Q10 from bovine myocardium in 1957. It combines with the inner membrane of mitochondria and participates in the process of cellular oxidative phosphorylation and ATP generation. Recent studies have found that coenzyme Q10 also has preventive and therapeutic effects on various diseases such as cancer, cardiovascul...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C50/28C07C46/10
Inventor 徐环昕洪晨江江邦和宁方红刘坐镇
Owner EAST CHINA UNIV OF SCI & TECH
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