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Method for extracting, separating and purifying scopoletin from erycibe schmidtii craib

A technology for separation and purification of Radix chinensis, applied in the direction of organic chemistry and the like, to achieve the effects of low cost, wide distribution and simple process

Inactive Publication Date: 2018-04-06
CHENGDU MEDICAL COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are few studies on the extraction of scopolamine from Dinggong glabra with strong specificity, and there is an urgent need for a simple, low-cost, environmentally friendly and efficient method to extract scopolamine from Dinggong glabra

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 1 kg of Dinggong glabra cane, crush it, add industrial ethanol with a material-to-liquid ratio of 1:5 kg / L, and reflux extract 3 times, each time for 2 hours, combine the extracts, and recover ethanol under reduced pressure to obtain 175 g of extract. Add 0.2% hydrochloric acid aqueous solution to the extract and soak for 3 times, stir thoroughly, combine the acidic water layer, let it stand overnight, and separate to obtain 20g of precipitate. Dissolve the precipitate with 200mL70% ethanol and put it on a 2L macroporous resin column (the model of the macroporous resin is D-101), elute with 6L water to remove impurities, and then use 6L 30%, 45%, and 60% ethanol aqueous solution to elute successively, Scopolamine was eluted at 45%, and scopolamine was eluted with 60% ethanol. The fraction eluted with 45–60% ethanol was concentrated and evaporated to dryness to obtain a crude product. The crude product was dissolved by heating with 90% ethanol and recrystallized at 4...

Embodiment 2

[0024] Take 1 kg of Dinggong glabra cane, crush it, add industrial ethanol with a material-to-liquid ratio of 1:6 kg / L, and reflux extract for 3 times, each time for 2 hours, combine the extracts, and recover ethanol under reduced pressure to obtain 180 g of extract. Add 0.2% sulfuric acid aqueous solution to the extract and soak for 3 times, stir thoroughly, combine the acidic water layer, let it stand overnight, and separate to obtain 21g of precipitate. Dissolve the precipitate with 200mL70% ethanol and put it on a 2L macroporous resin column (the model of the macroporous resin is D-101), elute with 6L water to remove impurities, and then use 6L 30%, 45%, and 60% ethanol aqueous solution to elute successively, Scopolamine was eluted at 45%, and scopolamine was eluted with 60% ethanol. The fraction eluted with 45–60% ethanol was concentrated and evaporated to dryness to obtain a crude product. The crude product was dissolved by heating with 85% ethanol and recrystallized at 4...

Embodiment 3

[0026] Take 1kg of Dinggong glabra cane, crush it, add industrial ethanol with a material-to-liquid ratio of 1:7kg / L, and reflux extract twice, each time for 3 hours, combine the extracts, and recover the ethanol under reduced pressure to obtain 181g of extract. Add 0.2% phosphoric acid aqueous solution to the extract and soak for 3 times, stir thoroughly, combine the acidic water layer, let it stand overnight, and separate to obtain 22g of precipitate. Dissolve the precipitate with 200mL60% ethanol and put it on a 2L macroporous resin column (the model of the macroporous resin is D-101), elute with 6L water to remove impurities, and then use 6L 30%, 50%, and 60% ethanol aqueous solution to elute successively, Scopoletin was eluted at 50%, and scopolamine was eluted with 60% ethanol. The fraction eluted with 50–60% ethanol was concentrated and evaporated to dryness to obtain a crude product. The crude product was heated and dissolved with 80% ethanol, and recrystallized at a lo...

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PUM

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Abstract

The invention discloses a method for extracting, separating and purifying scopoletin from erycibe schmidtii craib. The method comprises the following steps: (1) grinding erycibe schmidtii craib stemsto obtain erycibe schmidtii craib stem powder; (2) uniformly mixing the erycibe schmidtii craib stem powder and ethanol, performing reflux extraction at the temperature of 50-60 DEG C so as to obtainan extracting solution, wherein a solid-liquid ratio is 1:(5-8)kg / L, and recovering the solvent so as to obtain extract A; (3) adding an acid aqueous solution into the extract A for soaking for threetimes, and separating to obtain a precipitate B; (4) dissolving the precipitate B into 60-70% of ethanol, loading onto a macroporous resin column, eluting with water and different ratios of ethanol water in sequence so as to obtain an eluent, and concentrating to obtain crude scopoletin; and (5) dissolving the crude scopoletin into 80-90% of ethanol, and recrystallizing, thereby obtaining the scopoletin. The raw materials selected by the method are wide in distribution. Moreover, according to the method, the process is simple, the cost is low, the environmental-friendly and high-efficiency effects are achieved, the product yield is high and the method is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for extracting, separating and purifying scopoletin from Dinggong glabrata. Background technique [0002] Erycibe schmidtii Craib is a plant of the genus Erycibe in the family Convolvulaceae. Distributed in Yunnan, Guangxi, Guangdong and other places, it grows in areas with an altitude of 250 meters to 1200 meters, and mostly grows in dense forests and sparse forests in valleys. Its cane part is one of the sources of traditional Chinese medicine Dinggongteng, which has the effects of expelling wind and dampness, reducing swelling and relieving pain, and is used to treat rheumatic arthralgia, hemiplegia, and swelling and pain. [0003] Scopoletin, also known as scopoletin, scopoletin, scopoletin, and scopolamine, belongs to coumarin compounds. Its chemical name is 6-methoxy-7-hydroxycoumarin, and its molecular formula is C 10 h 8 o 4 , molecular weight 192. Studies have shown that scopoletin is one of the active in...

Claims

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Application Information

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IPC IPC(8): C07D311/16
CPCC07D311/16
Inventor 李丽梅周岳任望曾婷吴秀银邹强刘阳阳泰王衍堂李敏惠杨淑霞
Owner CHENGDU MEDICAL COLLEGE
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