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Method for preparing high-purity coenzyme Q10 in large scale

A high-purity, coenzyme technology, applied in quinone separation/purification, organic chemistry, bulk chemical production, etc., can solve the problems of low yield and purity, pending research, high cost, etc., to achieve high product quality, reduce production costs, Effect of production cost reduction

Active Publication Date: 2012-03-28
杭州华东医药集团康润制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above two methods only involve a certain process of separating and purifying coenzyme Q10 rather than a complete extraction and separation method
[0004] CN200710166132.1 relates to a purification method for separating coenzyme Q10. Although a purification method for separating coenzyme Q10 starting with coenzyme Q10 fermentation products is provided, the process is complicated, the yield and purity are low, and the cost is high. industrial application
[0005] Therefore, although coenzyme Q10 is widely used, the method of obtaining high-purity coenzyme Q10 and large-scale production remains to be studied

Method used

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  • Method for preparing high-purity coenzyme Q10 in large scale
  • Method for preparing high-purity coenzyme Q10 in large scale
  • Method for preparing high-purity coenzyme Q10 in large scale

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Coenzyme Q10 dried cells 10kg, content 26.81mg / g, particle size 80-120 mesh, moisture 5.6%. Under the pressure of 24.5Mpa, temperature of 35℃, and the amount of entrainer (n-hexane) 1.3ml / g, the 2 Supercritical extraction was performed for 45 minutes to obtain 2.5L of extract with a content of 106.54 mg / ml. Add 1.5L sodium hydroxide solution with a concentration of 0.35mol / L and stir for 40 min, let it stand for 2.5hr, after the layer is completely separated, let go of the lower layer, then add 2L of purified water and stir for 10 min, let it stand for 30 minutes, and let go of the lower layer , The upper layer is dehydrated by a desiccator (anhydrous sodium sulfate 25g) to obtain 2.3L of upper column liquid with a content of 113.30mg / ml. Apply the upper column liquid to a silica gel chromatography column at (effective amount: filler) 1:10, eluting with 2.5% (V / V) ethyl acetate in n-hexane, and obtain the main eluate by TLC chromatography. At the same time, the eluates ...

Embodiment 2

[0050] Coenzyme Q10 dry cell 100kg, content 30.13mg / g, particle size 130-200 mesh, moisture 5%. Under the pressure of 20.5Mpa, the temperature of 30℃, and the amount of entrainer (ether) 1.5ml / g through CO 2 Supercritical extraction for 30 minutes, 25.76L of extract was obtained, with a content of 115.65 mg / ml. Add 26.25L, 0.2mol / L sodium hydroxide solution and stir for 40 min, and let it stand for 2hr. After the layer is completely separated, let go of the lower layer, then add 20L purified water and stir for 10 min, let it stand for 30 minutes, let go of the lower and upper layers After dehydration in a desiccator (28g anhydrous sodium sulfate), 24.4L of upper column liquid was obtained, with a content of 119.70mg / ml. Put the upper column liquid on the column according to (effective amount: filler) 1:5, eluting with 1.5% (V / V) isopropyl ether in petroleum ether, and obtain the main eluate by TLC chromatography. At the same time, separately collect the eluates from the front ...

Embodiment 3

[0052] The chromatographic column of Example 1 was eluted with 2 to 3 times ethanol, and then equilibrated with 1 to 2 times petroleum ether, and set aside.

[0053] Coenzyme Q10 dried cells 20kg, content 16.50mg / g, particle size 60-100 mesh, moisture 6%. Under the pressure of 27.0Mpa, temperature of 33℃, and the amount of entrainer (petroleum ether) 1.0ml / g 2 Supercritical extraction was performed for 50 minutes to obtain 3.8L extract with a content of 85.79 mg / ml. Add 2.5L of sodium hydroxide solution with a concentration of 0.25mol / L and stir for 40 min, and let it stand for 2.5hr. After the layer is completely separated, let go of the lower layer, then add 2.5L of purified water and stir for 10 min, let it stand for 30 minutes, and let go The lower layer and the upper layer are dehydrated by a desiccator (38g anhydrous sodium sulfate) to obtain 3.7L of upper column liquid with a content of 86.10mg / ml. The upper column liquid is added to the chromatographic column that has be...

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Abstract

The invention relates to a method for preparing a separation coenzyme Q10, and in particular relates to a method for preparing a high-purity coenzyme Q10 in a large scale. The method comprises the following steps of: carrying out supercritical extraction on dry thallus containing the coenzyme Q10 to obtain extract liquor; and carrying out alkali treatment on the extract liquor to obtain a column loading liquid, carrying out column chromatography on the column loading liquid to obtain an eluent, concentrating the eluent, and crystallizing with ethanol to obtain the high-purity coenzyme Q10 with the purity higher than 99.5%. When the method provided by the invention is used for producing the coenzyme Q10, the overall yield is higher than 90%, and cost is low, thus the method provided by theinvention is applicable to industrial production.

Description

technical field [0001] The invention relates to a preparation method for separating coenzyme Q10, in particular to a large-scale preparation method for high-purity coenzyme Q10. Background technique [0002] Coenzyme Q10, also known as vitamin Q, is the main component of proton transfer and electron transfer in the cellular respiratory chain in organisms. It has important physiological and pharmacological effects in the human body, so it is called vitamin Q or vitamin coenzyme Q10. It is in the respiratory chain. A coenzyme that does not bind tightly to proteins. In terms of medicine: it can treat heart disease, scurvy, high blood pressure, duodenal ulcer, gastric ulcer, necrotizing periodontitis, viral hepatitis; it also has anti-tumor, treatment of round alopecia and emphysema. function; it also has certain treatment for hearing impairment; it has a significant auxiliary treatment for AIDS and Parkinson's disease; it can be used in cosmetics and health products: it has an...

Claims

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Application Information

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IPC IPC(8): C07C50/28C07C46/10
CPCY02P20/54
Inventor 周建仁蒋风王维毛海明梅云云
Owner 杭州华东医药集团康润制药有限公司
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