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Supercritical extraction method for evodiamine

A kind of evodiamine and supercritical technology, applied in the field of technical production of high-purity evodiamine, can solve the problems of pollution, low product purity, low extraction rate, etc.

Inactive Publication Date: 2011-02-16
TIBET JINKE GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is to disclose a production method of evodiamine with supercritical extraction as the main means, so as to overcome the defects of serious pollution, low extraction rate and low product purity in the existing production technology of evodiamine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] Take 100 grams of Evodia, crush it to a 60-mesh sieve, ultrasonically treat it for 180-300s, and dry it at a low temperature of 50-60℃, and place it in an extraction tank; add the entrainer anhydrous ethanol at the ratio of 4.2: 100; under the extraction pressure 19-21MPa, extraction temperature 35-40℃, CO 2 Separation is carried out under the condition of flow rate of 2.0-3.0L / min. After 120-150 minutes of dynamic operation, 4.51g of crude evodialine is obtained, with a crude yield of 4.51%; the entrainer is recovered and the separated CO is clean 2 The fluid is condensed by the condenser and recycled in the device. The extracted evodia base was purified by chromatography, the purification instrument was Agilent 1100, the chromatographic column conditions were: C18 column, mobile phase: acetonitrile-water (42:55); flow rate: 1.0mL·min -1 ; Column temperature: 40°C; detection wavelength 290nm; injection volume: 10μL, the purity of evodia base is greater than 99%.

example 2

[0025] Take 100 grams of Evodia, crushed to 80-mesh sieve, treated with ultrasonic for 180-300s, and dried at 50-60℃ low temperature, placed in the extraction tank; add the entrainer absolute ethanol according to the ratio of 4.2:100; under the extraction pressure 19-21MPa, extraction temperature 30-40℃, CO 2 The separation was carried out under the condition of flow rate of 2.0-3.0L / min. After 120-150 minutes of dynamic operation, 6.10g crude evodialine was obtained, with a crude yield of 6.10%; the entrainer was recovered and the CO was separated after separation. 2 The fluid is condensed by the condenser and recycled in the device. The extracted evodia base was purified by chromatography, the purification instrument was Agilent 1100, the chromatographic column conditions were: C18 column, mobile phase: acetonitrile-water (42:55); flow rate: 1.0mL·min -1 ; Column temperature: 40°C; detection wavelength; 290 nm; injection volume: 10 μL, the purity of evodia base is greater than ...

example 3

[0027] Take 100 grams of Evodia, crush it to a 100-mesh sieve, ultrasonically treat it for 180-300s, and dry it at a low temperature of 50-60℃, and place it in an extraction tank; add the entrainer anhydrous ethanol at a ratio of 4.2: 100; 19-21MPa, extraction temperature 30-40℃, CO 2 The separation was carried out under the condition of a flow rate of 2.5L / min. After 120-150 minutes of dynamic operation, 5.10g crude evocarpine was obtained. The crude product yield was 5.10%. The entrainer was recovered and the separated CO was clean. 2 The fluid is condensed by the condenser and recycled in the device. The extracted evodia base was purified by chromatography, the purification instrument was Agilent 1100, the chromatographic column conditions were: C18 column, mobile phase: acetonitrile-water (42:55); flow rate: 1.0mL·min -1 ; Column temperature: 40°C; detection wavelength; 290 nm; injection volume: 10 μL, the purity of evodia base is greater than 99%.

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Abstract

The invention relates to a method for extracting total alkaloid from rutaceae plant fruit fructus evodiae by adopting a supercritical extraction technology. Raw materials are pretreated in ways of raw material pulverization, screening, ultrasonic assisting, and the like; and effective components of the fructus evodiae are extracted by adopting anhydrous ethanol as an entrainer through applying a supercritical fluid technology. The method is simple and rapid and can be used for effectively extracting the alkaloid in the rutaceae plant fruit. The concrete application condition comprises the extracting pressure of 19-21MPa, the extracting temperature of 30-40 DEG C, the extracting time of 120-150 minutes and the CO2 flow of 2.0-3.0L / minute. The evodiamine is the main alkaloid in the plant and has various pharmacological activities of tumor resistance, nociception resistance, weight loosing, heart protection, blood pressure reduction, and the like.

Description

Technical field [0001] This patent relates to an extraction method of evodialine, specifically a method for producing high-purity evodialine by applying ultrasonic assisted extraction, supercritical extraction and other technologies. Background technique [0002] The molecular formula of evodia is C 19 H 17 N 3 O, molecular weight is 303.36, CAS NO: 518-17-2. Evodia rutaceae Evodia rutacearpa (Juss.)benth., stone tiger Evodiarutacearpa (Juss.)benth.Var.of f icinalis(Dode)Huang or sparse evodia Evodiarutacearpa(Juss.)bentheri.Vardebod Huang's dry and nearly mature fruit has the functions of dispelling cold and relieving pain, reducing adverse effects and relieving vomiting, helping yang and relieving diarrhea. Evodiamine is the main alkaloid in the plant, which has various pharmacological activities such as anti-tumor, anti-nociception, weight loss, heart protection, and blood pressure reduction. [0003] At present, the industry mainly uses plant extraction and semi-synthetic met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/14
CPCY02P20/54
Inventor 张丽云高聚霞
Owner TIBET JINKE GRP
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