Method for quickly separating and preparing high-purity deoxyrhapontin and rhapontin

A technology for deoxygenating rhubarb and rhubarb, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve problems such as hidden dangers of resin raw material safety, low product purity, complicated operation, etc., and achieve Conducive to quality control, high purity, high preparation effect

Active Publication Date: 2012-10-03
PUREDIA LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to problems such as unavoidable resin residues and potential safety hazards of resin raw materials, the State Food and Drug Administration has made corresponding restrictions and regulations on the production process of using adsorption resin separation and purification for health food (National Food and Drug Administration Note [2005] No. 202)
Therefore, methods such as traditional column chromatography in the above-mentioned patent method and literature have certain limitations in the actual production and application of medicine and health food industry; Low, complex operation, low product purity and many other defects

Method used

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  • Method for quickly separating and preparing high-purity deoxyrhapontin and rhapontin
  • Method for quickly separating and preparing high-purity deoxyrhapontin and rhapontin
  • Method for quickly separating and preparing high-purity deoxyrhapontin and rhapontin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 A method for rapidly separating and preparing high-purity deoxyrhein and erinacein, comprising the following steps:

[0035] (1) Weigh 50 g of the dried root of the cultivated rhubarb, cut it into 5 mm slices, and obtain the raw material for extraction.

[0036](2) Add 250mL of ethanol solution with a mass concentration of 80% to the extraction raw materials, and place it in a HH-4 constant temperature water bath produced by Guohua Electric Appliance Co., Ltd., heat and reflux at 40°C for 4 hours, and the extraction times are 2 times. The combined extracts were collected to obtain a crude extract; the crude extract was concentrated and dried under reduced pressure at 50°C and vacuumed to a negative pressure of 0.01 MPa using an R-114 rotary evaporator produced by Buchi BUCHI Laboratory Technology Co., Ltd., Switzerland. Constant weight yielded 16 g of extract.

[0037] (3) Mix the four solvents of methanol, water, n-butanol and chloroform according to the v...

Embodiment 2

[0043] Example 2 A method for rapidly separating and preparing high-purity deoxyrhein and erinacein, comprising the following steps:

[0044] (1) Weigh 50 g of the dried root of rhubarb cultivated in Hetao, and use a high-speed universal pulverizer produced by Beijing Kewei Yongxing Instrument Co., Ltd. to pulverize it into 80-mesh powder to obtain the raw material for extraction.

[0045] (2) Add 750mL of ethanol solution with a mass concentration of 40% to the extracted raw materials, and place it in a HYR automatic decoction machine produced by Tianjin Huayanyuan Machinery Co., Ltd., heat and reflux at 90°C for 3 hours, and the number of extractions is 3 times , collect and combine the extracts to obtain the crude extract; the crude extract is concentrated and dried under reduced pressure at 30°C and vacuumed to a negative pressure of 0.1MPa using the R-114 rotary evaporator produced by Buchi BUCHI Laboratory Technology Co., Ltd. To constant weight, 21 g of extract were o...

Embodiment 3

[0052] Example 3 A method for rapidly separating and preparing high-purity deoxyrhein and erinacein, comprising the following steps:

[0053] (1) Weigh 50 g of the dried root of wild rhubarb rhubarb, and use a high-speed universal pulverizer produced by Beijing Kewei Yongxing Instrument Co., Ltd. to pulverize it into a 10-mesh powder to obtain the raw material for extraction.

[0054] (2) Add 550mL of ethanol solution with a mass concentration of 50% to the extracted raw materials, and place it in a HYR automatic decoction machine produced by Tianjin Huayanyuan Machinery Co., Ltd., heat and reflux at 70°C for 0.5 hours, and the number of extractions is 4 times , collect and combine the extracts to obtain the crude extract; the crude extract is concentrated and dried under reduced pressure at 45°C and vacuumed to a negative pressure of 0.05MPa using the R-114 rotary evaporator produced by Buchi BUCHI Laboratory Technology Co., Ltd. To constant weight, 20 g of extract was obta...

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Abstract

The invention relates to a method for quickly separating and preparing high-purity deoxyrhapontin and rhapontin. The method comprises the following steps of: (1) cutting or grinding the dry root or rhizome of the wild or cultivated rhubarb plant to obtain the extraction raw material; (2) performing alcohol extraction and drying of the extraction raw material to obtain an extract; (3) mixing four solvents of methanol, water, n-butyl alcohol and chloroform; shaking, standing for layering and collecting the upper-phase solvent and the lower-phase solvent; and performing ultrasonic treatment of the upper-phase solvent and the lower-phase solvent to obtain a stationary phase and a mobile phase; (4) dissolving the extract in the mobile phase to obtain a sample injection solution; (5) sequentially pumping the stationary phase and the mobile phase into a separation tube of a high-speed counter-current chromatographic apparatus, and injecting the sample injection solution into a sample injection ring of the high-speed counter-current chromatographic apparatus; (6) collecting the effluent liquid A in the time range from 70min to 100min, and drying the effluent liquid A to obtain deoxyrhapontin; (7) reversely rotating the separation tube; and (8) collecting the effluent liquid B in the time range from 400min to 450min, and drying the effluent liquid B to obtain rhapontin. The method provided by the invention is simple to operate and facilitates the industrial production.

Description

technical field [0001] The invention relates to a method for separating and preparing high-purity medical active ingredients from plants, in particular to a method for rapidly separating and preparing high-purity deoxyrheidin and terrain. Background technique [0002] Rhubarb is a well-known traditional Chinese medicinal material in my country. Its medicinal records first appeared in "Shen Nong's Materia Medica", and it is listed as inferior. It has the effect of "relieving diarrhea and breaking stagnation". In the application of traditional Chinese medicine, the medicinal scope of the rhubarb plant is very single, mainly focusing on its purgative effect. Modern research has proved that the main material base component of rhubarb's purging effect is anthraquinones. Therefore, anthraquinone compounds are identified as traditional medicinal compounds of rhubarb medicinal materials, and are the main indicators used by countries all over the world to evaluate the quality of rhu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08
Inventor 王小艳袁木荣
Owner PUREDIA LTD
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