Extraction and purification method of sesquiterpenes coumarin ether and use thereof

The technology of a terpene coumarin ether and a purification method is applied in the field of extraction and purification of a sesquiterpene coumarin ether, which can solve the problems of high solvent consumption, long separation time, and low separation efficiency, and achieves simple preparation methods and easy raw materials. The effect of obtaining and improving the separation efficiency

Inactive Publication Date: 2008-12-17
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] After searching the prior art, it was found that in the journal Journal of Natural Products, Volume 45, No. 4, New sesquiterpene-courmain from Achillea and Artemisia species, it was reported that from Northwest Artemisia, Iran Artemisia, Old Man Artemisia, Yarrow and Artemisia species The example of sesquiterpene coumarin ether is isolated, but the method in this document adopts the method of petroleum ether cold immersion extraction, this method has long separation time, low separation efficiency, and consumes more solvents

Method used

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  • Extraction and purification method of sesquiterpenes coumarin ether and use thereof
  • Extraction and purification method of sesquiterpenes coumarin ether and use thereof
  • Extraction and purification method of sesquiterpenes coumarin ether and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of Sesquiterpene Coumarin Ether

[0026] 1. Cultivate the hair roots induced by Artemisia annua of the genus Artemisia annua in Compositae. The culture conditions are: basic MS medium + 30g / L sucrose, photoperiod: light 16h / dark 8h, 25°C, shaker speed 110r / min ; Obtain the roots of Artemisia annua growing to the stable stage;

[0027] 2. Take out 200g of Artemisia annua hair roots that have grown to the stable stage and dry them in the sun, then pulverize them with a pulverizer, and all pulverized samples need to pass through a 60-mesh sieve. The part that failed to pass the sieve was crushed again or sieved after being ground in the mortar until all the samples were sieved;

[0028] 3. Soak the sample powder in 2L of methanol, ultrasonicate twice, 30min each time, shake well in the middle, with an interval of 10min, and pay attention to control the water temperature not to exceed 50°C. After the extraction is complete, filter, take the filtrate, and conce...

Embodiment 2

[0034] Column Chromatographic Separation of Sesquiterpene Coumarin Ether Drimartol A

[0035] 1. Take out 200g of Artemisia annua roots that have grown to the stable stage (14-18 days) and dry them in the sun, then pulverize them with a pulverizer, and all pulverized samples need to pass through a 60-mesh sieve. The parts that failed to pass the sieve were crushed again or sieved after being ground in a mortar until all the samples were sieved.

[0036] 2. Soak the sample powder in 2L of methanol, ultrasonicate five times, 30min each time, pay attention to control the water temperature not to exceed 50°C. After the extraction is completed, filter, take the filtrate, concentrate after rotary evaporation to obtain a brown extract (about 17.3g), and directly disperse the obtained extract with petroleum ether: ethyl acetate (volume ratio 1:3) 50mL, which can be assisted by ultrasound for 5~10min , then filtered, and the filtrate was applied to a silica gel column for column chrom...

Embodiment 3

[0039] Preparation of Sesquiterpene Coumarin Ether drimartolA by Liquid Phase Separation

[0040] 1. Take out 200g of Artemisia annua roots that have grown to the stable stage (14-18 days) and dry them in the sun, then pulverize them with a pulverizer, and all pulverized samples need to pass through a 60-mesh sieve. The parts that failed to pass the sieve were crushed again or sieved after being ground in a mortar until all the samples were sieved.

[0041]2. Soak the sample powder in 2L of methanol, overnight, ultrasonic three times, 30min each time, shake well in the middle, with an interval of 5~10min, pay attention to control the water temperature not to exceed 50℃. After the extraction is complete, filter, take the filtrate, concentrate after rotary evaporation to obtain a brown extract (about 15.8 g), then use 1 L of ethyl acetate and water (volume ratio 1:1) for dual-phase extraction, take the upper ethyl acetate organic phase, Concentrate the organic phase into an ext...

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Abstract

The invention relates to a method for extracting and purifying sesquiterpene coumarin aether in the field of chemical technology, which comprises the steps as follows: step 1: southernwood roots are smashed and ultrasonically extracted with methanol; the extracting solution is rotary-evaporated and condensed to obtain extract which is then delaminated by adopting acetic ether and water double-phase dispersion and extraction; the acetic ether organic phase of an upper layer is taken as an extracting concentrate; step 2: column chromatography is carried out after the extracting concentrate is added with an adsorbent; elution is carried out by using petroleum ether and acetic ether mixed eluant, and then thin-layer chromatography is carried out to collect components containing the sesquiterpene coumarin aether; step 3: the concentrate is furthered condensed to the extract which is then dispersed with methanol of same volume and then filtered with a nylon membrane, purified with the reversed-phase column of a preparative liquid phase ODS RP-C18 and eluted with mixture solution of methanol and water; and finally, the corresponding components are condensed. The invention has simple preparation method and easily available raw materials for preparation and can be applied to chemoprophylaxis and cure of tumors and development of relevant antitumor drugs.

Description

technical field [0001] The present invention relates to a method in the technical field of chemical industry, more specifically, to a method for extracting and purifying sesquiterpene coumarin ether and its application. Background technique [0002] Artemisia annua is a well-known traditional Chinese herbal medicine in my country. It has the functions of clearing heat, relieving heat, and removing steam; treating febrile diseases, summer heat, bone steaming and labor fever, malaria, dysentery, jaundice, scabies, and itching. Artemisia annua root can treat hot bone steaming, joint pain, and blood in stool; fruit (artemisia annua) can clear away heat, tear eyes, improve eyesight, and kill insects. The antimalarial sesquiterpene artemisinin produced by it is recognized by the World Health Organization as the most effective antimicrobial malaria drug to replace quinine in the 21st century. Secondary development of Artemisia annua resources to produce new biologically active sub...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/16A61K31/37A61P35/00A61K36/282
Inventor 钟建江翟丹丹
Owner SHANGHAI JIAO TONG UNIV
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