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Method for extracting high-purity sinensetin from clerodendranthus spicathus (thunb) C.Y.Wu

A cat's whisker, high-purity technology, applied in the field of extracting high-purity auranone, can solve the problems of poor alumina chromatographic separation and purification effect, poor production continuity, and research on the purification and separation of auranone, and achieves low cost and guaranteed continuity. , the effect of processing batch reduction

Inactive Publication Date: 2017-07-14
HUNAN HUACHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses a flash extractor, which has the advantages of short extraction time and high extraction rate, but has the disadvantage of poor production continuity, and the use of 85-95% high-concentration ethanol will extract a large amount of fat-soluble impurities, such as chlorophyll and volatile oil. etc. After the solvent is recovered, a large amount of precipitation will be produced, resulting in poor separation and purification effect of subsequent alumina chromatography
[0012] In summary, the prior art is mainly aimed at the separation and purification of total phenolic acids and total flavonoids in Cat's Whiskers, and no research has been done on the purification and separation of aurinoids in Cat's Whiskers. All have a content requirement of 0.2 to 98% for orange flavonoids. The demand is large and the market prospect is broad. It is urgent to find a method for extracting high-purity orange flavonoids from cat's whiskers

Method used

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  • Method for extracting high-purity sinensetin from clerodendranthus spicathus (thunb) C.Y.Wu

Examples

Experimental program
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Effect test

reference example 1

[0054] Alumina pretreatment: First, activate commercially available 100-200-mesh neutral alumina at a high temperature of 550°C for 18 hours, and then wash it with 95% ethanol until the effluent is colorless and transparent, and removes the ethanol smell. Until there is no other smell outside, finally wash with water until there is no ethanol smell.

Embodiment 1

[0056] (1) Extraction, concentration, and filtration: crush 100kg of cat's whiskers (the mass content of orange flavonoids is 0.0615%), pass through a 20-mesh sieve, put it in 1000L of methanol aqueous solution with a volume fraction of 30%, and use 2 sets of continuous countercurrent in series Extraction equipment, continuous countercurrent extraction at 50°C for 2 hours, cooling with a plate heat exchanger, first filtering with a 200-mesh filter, and then using a single-effect concentrator to recover the filtrate in vacuum at 60°C and a vacuum of -0.09MPa methanol in the concentrated liquid until the solid content of the concentrated liquid is 5%, and then filter with a ceramic membrane with a pore size of 0.5 μm at a membrane pressure of 3 MPa and 35°C to obtain a concentrated liquid;

[0057] (2) Separation and purification by alumina column chromatography: apply the concentrated solution obtained in step (1) to alumina column chromatography (using neutral alumina activated...

Embodiment 2

[0062] (1) Extraction, concentration, and filtration: crush 100kg of cat's whiskers (the mass content of orange flavonoids is 0.0736%), pass through a 40-mesh sieve, put it in 1500L of ethanol aqueous solution with a volume fraction of 50%, and use 2 sets of continuous countercurrent in series Extraction equipment, continuous countercurrent extraction at 60°C for 3 hours, cooling with a plate heat exchanger, first filtering with a 300-mesh filter, and then using a three-effect concentrator, at 70°C, vacuum degree -0.09MPa, vacuum recovery filtrate the ethanol in the concentrated liquid until the solid content of the concentrated liquid is 7%, and then use a ceramic membrane with a pore size of 0.5 μm to filter at a membrane pressure of 4 MPa and 40°C to obtain a concentrated liquid;

[0063] (2) Separation and purification by alumina column chromatography: apply the concentrated solution obtained in step (1) to alumina column chromatography (using neutral alumina activated in R...

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Abstract

The invention provides a method for extracting high-purity sinensetin from clerodendranthus spicathus (thunb) C.Y.Wu. The method comprises the following steps: (1) crushing the clerodendranthus spicathus (thunb) C.Y.Wu, sieving, extracting, cooling, filtering, recycling a solvent and filtering to obtain a concentrated solution; (2) carrying out aluminum oxide column chromatography on the concentrated solution; washing with water; eluting with a low-degree alcohol water solution and a high-degree alcohol water solution in sequence; collecting eluting solutions respectively and recycling alcohol to obtain flavone extract and phenolic acid extract; (3) carrying out overcritical CO2 extraction on the flavone extract to obtain extracted extract; (4) preparing a liquid chromatography and separating and purifying: dissolving the extracted extract with methanol; feeding a sample and eluting; collecting a target eluting solution and concentrating and drying to obtain a high-purity sinensetin product. According to the method provided by the invention, an aluminum oxide column chromatography technology, an overcritical CO2 extraction technology and a liquid chromatography preparation technology are organically combined; the extracted sinensetin product is pure white, the purity is more than or equal to 98.5 percent and the yield is more than or equal to 91 percent; the method provided by the invention is low in cost, good in selectivity and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for extracting high-purity aurantrone, in particular to a method for extracting a product with arurinone content ≥ 98% from cat's whiskers. Background technique [0002] Clerodendranthus spicathus (Thunb.) C.Y.Wu belongs to Labiatae and belongs to the genus Kidney Tea. Cat's whiskers is a perennial herb that grows in cool and humid places under the forest. It is mainly distributed in Southeast Asia such as Indonesia and Malaysia. It is mainly produced in Guangdong, Guangxi, Yunnan, Fujian and Taiwan in China. Cat's Whiskers is a kind of medicinal and edible plant, cool in nature, bitter in taste, and fragrant in breath. [0003] Cat's Whiskers has significant pharmacological effects. Modern pharmacological research has proved that the pharmacological functions of Cat's Whiskers are mainly reflected in the following aspects: diuretic and stone removal, cooling blood, anti-inflammation; improvement of kidney function; a...

Claims

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Application Information

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IPC IPC(8): C07D311/30C07D311/40
CPCC07D311/30C07D311/40Y02P20/54
Inventor 陈钱龙伟岸黄华学
Owner HUNAN HUACHENG BIOTECH
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