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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally speaking, these methods consume a lot of organic solvents, the operation is extremely cumbersome, and the production cost is relatively high.

Method used

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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

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Take 100 grams of 80 mesh rhubarb crude drug 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 to neutralize the excess hydrochloric acid until no bubbles are generated. Put the rhubarb powder into a supercritical extraction kettle, add 100ml of 99% ethanol at the same time, and extract statically 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, keeping 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. Collect the product from the separation tank and spray dry under reduced pressure to obtain 2.65 grams of rhubarb free anthraquinone powder. Its purity is 98.8% as...

Embodiment 2

[0034] Take 300 grams of 80 mesh rhubarb crude drug 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 to neutralize the excess hydrochloric acid until no bubbles are generated. Put the rhubarb powder in a 21-degree supercritical kettle, add 300ml of 99% ethanol at the same time, and extract it statically for 0.5 hour, the extraction pressure is 45MPa, and the extraction temperature is 60°C. Afterwards, add 99% concentrated ethanol 600ml from the entrainer pump at a rate of 19ml / min, and extract dynamically for 1.1 hours, keep the same extraction pressure and temperature as the static extraction, the separation tank pressure is 4MPa, and the average flow rate of carbon dioxide is 0.5l / min. Collect the product from the separation tank and spray dry it under reduced pressure to obtain 8.05 grams of rhubarb free anthraquinone powder. Its purity is greater tha...

Embodiment 3

[0036] Take 800 grams of 80 mesh rhubarb crude drug powder, add 800ml of 5mol / l concentrated hydrochloric acid and hydrolyze it at 60° for 1.5 hours, after the reaction is complete, add 200 grams of calcium carbonate and mix to neutralize the excess hydrochloric acid until no bubbles are produced. Put the rhubarb powder in a 21-degree supercritical kettle, add 800ml of 99% ethanol at the same time, and extract it statically for 0.5 hour, the extraction pressure is 45MPa, and the extraction temperature is 60°C. Afterwards, add 99% concentrated ethanol 1600ml from the entrainer pump at a rate of 50ml / min, and extract dynamically for 1.1 hours, keep the same extraction pressure and temperature as the static extraction, the separation tank pressure is 4MPa, and the average flow rate of carbon dioxide is 0.5l / min. Collect the product from the separation tank and spray dry it under reduced pressure to obtain 22.05 grams of rhubarb free anthraquinone powder. Its purity is greater t...

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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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