Supercritical carbon dioxide method for extracting high purity rhubarb free anthraquinones

A free anthraquinone, supercritical technology, applied in pharmaceutical formulations, medical preparations containing active ingredients, plant raw materials, etc., can solve the problems of long auxiliary time for loading and unloading, hidden dangers in production safety, and limited volume. It is beneficial to large-scale industrial production, preventing equipment corrosion and potential safety hazards, and achieving high product yield and purity.

Inactive Publication Date: 2007-10-17
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this process is that it is difficult to mix calcium carbonate and rhubarb powder evenly when neutralizing excess acid liquid, resulting in high local acidity of rhubarb powder, which will cause serious corrosion to stainless steel extraction kettle at high temperature and high pressure and shorten the life of supercritical fluid extraction equipment , and bring potential safety hazards to production
Chinese patent application 200610057160.5 also treats rhubarb powder with hydrochloric acid solution and infiltrates it with ethanol, then puts it into a supercritical carbon dioxide extraction kettle for extraction to obtain free anthraquinone. In this process, hydrochloric acid directly enters the extraction kettle without neutralization, which will cause corrosion to equipment. more serious
In addition, this type of extraction method needs to put rhubarb powder into the extraction tank, and the volume of the supercritical extraction tank is limited, so the single-batch extraction yield is low; and the auxiliary time for loading and unloading is long, which limits the industrialization of the process

Method used

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  • Supercritical carbon dioxide method for extracting high purity rhubarb free anthraquinones

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Referring to accompanying drawing 1, when supercritical carbon dioxide fluid continuously extracts rhubarb free anthraquinone, at first raw material powder is leached with organic solvent to obtain rhubarb leaching liquid; Neutralization with base follows. Heat the extraction kettle 8 and the separation kettle 9 to the set temperature, and simultaneously open the booster plunger pump 6a to pressurize the extraction kettle 8 to the set pressure (close the front valve 11 of the separation kettle 9 at this time). Pour the rhubarb leaching solution treated by acid hydrolysis and alkali neutralization into the entrainer tank 3, and continuously pump it into the extraction tank 8 at a certain flow rate by the entrainer pump 6b. Now open the front valve 11 of the separation kettle 9 to control the flow of circulating carbon dioxide, so that rhubarb anthraquinone and the organic solvent continuously flow into the separation kettle 9 from the extraction kettle 8 at a certain rat...

Embodiment 2

[0033] According to the technical process of Example 1, take 250 grams of 80-100 mesh rhubarb crude drug powder (2.81 g of rhubarb total anthraquinones / 100 g of rhubarb powder), and add it to a percolation bed of φ4×80 cm. Percolation leaching was carried out with ethanol at 60°C. The amount of ethanol is 2000mL, the flow rate is 1.2L h -1 , after about 1.67h, the leaching was finished, and 1770mL of ethanol leaching solution was collected;

[0034] Add 20 mL of concentrated hydrochloric acid (36%, w / w) to the ethanol leaching solution, mix well, and hydrolyze at 70° C. for 2 hours. It is detected that rhubarb-bound anthraquinone is completely converted into free form. Finish the reaction, add 25 grams of calcium carbonate powder in the reaction solution, and adjust the pH of the reaction solution to be 6.6.

[0035] Adjust the temperature of the extraction tank of the supercritical carbon dioxide fluid extraction equipment to 50°C, the pressure to 25MPa, the temperature of ...

Embodiment 3

[0037] According to the technical process of Example 1, take 250 grams of 80-100 mesh rhubarb crude drug powder (2.81 g of rhubarb total anthraquinones / 100 g of rhubarb powder), and add it to a percolation bed of φ4×80 cm. Percolation leaching was carried out with ethanol at 40°C. The amount of ethanol is 2000mL, the flow rate is 1.0L·h -1 , after about 2 hours, the leaching was finished, and 1800 mL of ethanol leaching solution was collected;

[0038] Add 20 mL of concentrated hydrochloric acid (36%, w / w) to the ethanol leaching solution, mix well, and hydrolyze at 50° C. for 2 hours. It is detected that rhubarb-bound anthraquinone is completely converted into free form. Finish the reaction, add 25 grams of calcium carbonate powder in the reaction solution, and adjust the pH of the reaction solution to be 6.8.

[0039] Adjust the temperature of the extraction tank of the supercritical carbon dioxide fluid extraction equipment to 50°C, the pressure to 15MPa, the temperature ...

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Abstract

The invention discloses a method for extracting highly purified rhubarb dissociated anthraquinone by a hypercritical CO2 extraction method, including leaching the material with organic solvent to get leaching liquid, hydrolyzing the combined anthraquinone, balancing out the superfluous acid with inorganic alkali or acid after hydrolytic reaction, getting hydrolytic leaching liquid; injecting the hydrolytic leaching liquid into the extraction vessel for a hypercritical CO2 extraction, entering to the separation vessel after the extraction; recycling separated CO2, collecting discharging rhubarb dissociated anthraquinone and organic solvent, steaming out the organic solvent decompressly, obtaining the rhubarb dissociated anthraquinone powder. The invention adopts the liquid feed to effectively control the material liquid acidity in the extraction vessel and prevent the equipment corrosion and potential safety problems; meanwhile, it does not need install and detach the extraction vessel by entrainer pump liquid feed so that the extraction is processed continuously and greatly saves the extraction time and improve the output in unit time.

Description

technical field [0001] The invention relates to the field of supercritical carbon dioxide extraction, in particular to a method for extracting rhubarb powder with supercritical carbon dioxide fluid to obtain high-purity rhubarb free anthraquinones. Background technique [0002] Rhubarb is the dry root and rhizome of Rheum palmatum L., Rheumtanguticum Maxim.ex Balf., or Rheum officinale Baill. of the Polygonaceae plant. It is one of the most widely used Chinese herbal medicines in Chinese medicine prescriptions. The main active ingredients are emodin, chrysophanol, aloe-emodin, emodin methyl ether and rhein and other anthraquinone compounds and their glycosides. These components have a wide antibacterial spectrum and strong antibacterial effect, and have strong antibacterial effect on various bacteria and pathogenic fungi. Among them, free aglycones such as rhein, emodin, and aloe-emodin have the strongest antibacterial effect. [0003] Solvent extraction is generally used ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/708A61P31/04
Inventor 魏作君刘迎新任其龙
Owner ZHEJIANG UNIV
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