Method for extracting and separating levorotation-synephrine from green tangerine orange peel

A technology of green bark and extract, which is applied in chemical instruments and methods, medical preparations containing active ingredients, pharmaceutical formulas, etc., and can solve problems such as unrealized separation and identification of synephrinesynephrine

Inactive Publication Date: 2009-04-08
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There have been many reports on the separation and preparation of synephrine, but the limita...

Method used

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  • Method for extracting and separating levorotation-synephrine from green tangerine orange peel
  • Method for extracting and separating levorotation-synephrine from green tangerine orange peel
  • Method for extracting and separating levorotation-synephrine from green tangerine orange peel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Chop green peel, grind into powder, and freeze-dry to get green peel fine powder. Weigh 100g of Qingpi fine powder, add 2L of 15% ethanol solution, extract twice in the extraction reflux device under the condition of 80°C, concentrate the extract under reduced pressure to obtain 14g of extract, add 50mL of water to dissolve the extract, and make the solid content 80-85%, put the sample on a 500mL D101 macroporous resin column, wash it with 2 times the volume of distilled water, and then elute with 4 times the volume of 15% ethanol solution, using a vacuum of 0.06-0.09Mpa and a temperature of 40- The eluate was concentrated under reduced pressure at 50°C, and then spray-dried at a temperature of 50-60°C to obtain 2.8 g of the crude product, which was determined by high-performance liquid chromatography using a ChiralPakAD-H chiral column, wherein the content of (-)-synephrine was 30.3%. Dissolve the crude product in pure ethanol, stir in silica gel of the same quality a...

Embodiment 2

[0022] Weigh 4.5kg of Qingpi fine powder, add 70L of 30% ethanol solution, extract twice in the extraction reflux device at 80°C, concentrate the extract under reduced pressure to obtain 500mL of extract, add 1.5L of water to dissolve the extract, and load it on The 5L D101 macroporous resin column was first washed with 2 times the volume of distilled water, and then eluted with 4 times the volume of 15% ethanol solution. After the eluent was concentrated under reduced pressure, it was spray-dried to obtain 102 g of crude product, wherein the (-)-synephrine content was about was 31.1%. The crude product was dissolved in ethanol, mixed with silica gel of the same quality as the crude product, and the ethanol was evaporated to obtain a silica gel adsorption sample. The silica gel adsorption sample was loaded on a 3L silica gel column, eluted with the eluent prepared by dichloromethane:methanol:ammonia water=8:2:0.1, and the eluted fraction containing synephrine was collected, co...

Embodiment 3

[0024] Weigh 20kg of Qingpi fine powder, add 300L 40% ethanol solution, extract twice in the extraction reflux device at 80°C, concentrate the extract under reduced pressure to obtain 2L of extract, add 3L of water to dissolve the extract, and load it on a 20L container D101 macroporous resin column, rinsed with 2 times volume of distilled water first, then eluted with 4 times volume of 15% ethanol solution, and the eluent was concentrated under reduced pressure and spray-dried to obtain 432g of crude product, wherein the content of (-)-synephrine was about 30.9 %. The crude product was dissolved in ethanol, mixed with silica gel of the same quality as the crude product, and the ethanol was evaporated to obtain a silica gel adsorption sample. Load the silica gel adsorption sample on a 30L silica gel column soaked in dichloromethane, elute and collect with the eluent prepared by dichloromethane: methanol: ammonia water = 9:2:0.1, collect the components containing synephrine, an...

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Abstract

The invention discloses a method for extracting levo-synephrine from green tangerine orange peel. The method comprises the following steps: refluxing and extracting the levo-synephrine in green tangerine orange peel powder twice by 15 to 45 percent alcohol at a temperature of 80 DEG C, decompressing and concentrating the extract to 80 to 85 percent of solid which is placed on a D101 macroporous absorption resin column, and eluting the solid by 15 percent alcohol; decompressing and concentrating the eluant to obtain a crude product of the levo-synephrine after spraying and drying; dissolving the crude product of the levo-synephrine by pure alcohol, adding silica gel with the same mass as the crude product, stirring the mixture evenly, removing the alcohol, preparing a silica-gel adsorption sample, sampling by a dry method, using the eluant prepared by methylene chloride and methanol as well as ammonia water the volume ratio of which are 6-9:2:0.1 to elute and collect the levo-synephrine component; and decompressing and concentrating the levo-synephrine component separated and eluted by the silica gel column, and obtaining the levo-synephrine product after spraying and drying. The content of the synephrine in the product prepared by the method is higher than 90 percent.

Description

technical field [0001] The invention belongs to the technical field of food processing, and relates to a deep processing technology of green skin, in particular to a method for separating and preparing (-)-synephrine from green skin. technical background [0002] A green skin is the immature fruit of tangerine, which is a traditional Chinese medicinal material with a long history and widely used. Synephrine is the main active ingredient, which has the effects of boosting blood pressure, anti-shock, and promoting metabolism. Synephrine is a chiral substance, which mainly exists in the form of (-)-synephrine in natural plants, but racemization easily occurs during the extraction and separation of synephrine, which increases the content of (+)-synephrine. Studies at home and abroad have shown that (-)-synephrine is the effective configuration of synephrine for its pharmacological effect, and (+)-synephrine may produce pharmacodynamic antagonism, and may even be the cause of th...

Claims

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Application Information

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IPC IPC(8): C07C215/30C07C213/10A61K36/752
Inventor 沈莲清张超杜琪珍
Owner ZHEJIANG GONGSHANG UNIVERSITY
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