Method for extracting rhubarb powder dissociated anthraquinone by supercritical acid hydrolysis

A free anthraquinone, supercritical technology, applied in quinone separation/purification, bulk chemical production, organic chemistry and other directions, can solve the problems of high production cost, cumbersome operation, large consumption of organic solvents, etc. Simple process and low solvent consumption

Inactive Publication Date: 2006-07-19
北京盖雅环境科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Generally speaking, these methods consume a lot of organic solvents, the op

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  • Method for extracting rhubarb powder dissociated anthraquinone by supercritical acid hydrolysis
  • Method for extracting rhubarb powder dissociated anthraquinone by supercritical acid hydrolysis

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Example Embodiment

[0028] Example 1

[0029] Take 100 grams of 80 mesh rhubarb powder, add 150ml of 5mol / l concentrated hydrochloric acid and hydrolyze it at 60° for 1.5 hours. After the reaction is complete, add 25 grams of calcium carbonate and mix well to neutralize excess hydrochloric acid until no bubbles are generated. Put the rhubarb powder into the supercritical extraction kettle, while adding 100ml of 99% ethanol, static extraction for 0.5 hours, the extraction pressure is 45MPa, and the extraction temperature is 60°C. After that, add 200ml of 99% concentrated ethanol from the entrainer pump at a rate of 6ml / min, and perform dynamic extraction for 1 hour, maintaining the same extraction pressure and temperature as static extraction. The pressure of the separation vessel is 4MPa, and the average flow rate of carbon dioxide is 0.5l / min. The product from the separation kettle was collected and spray-dried under reduced pressure to obtain 2.65 g of rhubarb free anthraquinone powder. The purity...

Example Embodiment

[0033] Example 2

[0034] Take 300 grams of 80 mesh rhubarb powder, add 300ml of 5mol / l concentrated hydrochloric acid and hydrolyze it at 60° for 1.5 hours. After the reaction is complete, add 75 grams of calcium carbonate and mix well to neutralize excess hydrochloric acid until no bubbles are generated. Put the rhubarb powder into the supercritical kettle of 21, while adding 300ml of 99% ethanol, static extraction for 0.5 hours, the extraction pressure is 45MPa, and the extraction temperature is 60°C. After that, add 600ml of 99% concentrated ethanol from the entrainer pump at a rate of 19ml / min, and perform dynamic extraction for 1.1 hours, maintaining the same extraction pressure and temperature as static extraction. The separation tank pressure is 4MPa, and the average flow rate of carbon dioxide is 0.5l / min. The product from the separation kettle was collected and spray-dried under reduced pressure to obtain 8.05 g of rhubarb free anthraquinone powder. Its purity is greate...

Example Embodiment

[0035] Example 3

[0036] Take 800 g of 80 mesh rhubarb powder, add 800 ml of 5 mol / l concentrated hydrochloric acid and hydrolyze it at 60° for 1.5 hours. After the reaction is complete, add 200 g of calcium carbonate and mix well to neutralize excess hydrochloric acid until no bubbles are generated. Put the rhubarb powder into the supercritical kettle of 21, while adding 800ml of 99% ethanol, static extraction for 0.5 hours, the extraction pressure is 45MPa, and the extraction temperature is 60°C. After that, add 1600ml of 99% concentrated ethanol from the entrainer pump at a rate of 50ml / min, and perform dynamic extraction for 1.1 hours, maintaining the same extraction pressure and temperature as static extraction. The pressure of the separation vessel is 4MPa, and the average flow rate of carbon dioxide is 0.5l / min. The product from the separation kettle was collected and spray-dried under reduced pressure to obtain 22.05 grams of rhubarb free anthraquinone powder. Its purity...

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Abstract

The related extraction method with hypercritical acid hydrolysis for rhubarb anthrone from rhubarb belonged to traditional medicine comprises: acid hydrolyzing the rhubarb powder, and neutralizing with proper alkali; extracting the rhubarb powder for 0.5-1.5h with hypercritical CO2 by 35-60Deg and 25-45MPa as the best time and pressure respectively; combining the static and dynamic extraction, reducing pressure to spray and dry the extracted product, and obtaining the mixture contained five constituents as the rhubarb, chrysophanol, rheinic acid, aloe-emodin and ryeochrysidin total more than 98.5%. This invention has high extraction efficiency with low cost and green feature.

Description

technical field [0001] The invention relates to a method for extracting substances, specifically, a method for extracting rhubarb anthraquinones in rhubarb powder by using supercritical carbon dioxide fluid. Background technique [0002] Rhubarb is one of the most widely used Chinese herbal medicines in Chinese medicine prescriptions in my country. The main components of its extracts are emodin, chrysophanol, aloe-emodin, emodin methyl ether and rhein and other anthraquinone compounds. These components have a wide antibacterial spectrum and strong antibacterial effect, and have strong antibacterial effect on various bacteria and pathogenic fungi. Among them, rhein, emodin, and aloe-emodin have the strongest effects. [0003] The molecular weight range of rhubarb anthraquinone extracts is 256-300. Because the molecule contains hydroxyl and carboxyl groups, the polarity is strong. Therefore, in the process of extracting with supercritical carbon dioxide fluid, an entrainer mu...

Claims

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Application Information

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IPC IPC(8): C07C46/10C07C50/18
CPCY02P20/54
Inventor 未作君林立黄文倪晋仁
Owner 北京盖雅环境科技有限公司
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