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Preparation method for wall breaking extraction of chrysophanol

A chrysophanol and ultra-high pressure technology, applied in organic chemistry, quinone separation/purification, etc., can solve the problems of time-consuming and low extraction rate

Inactive Publication Date: 2018-09-25
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the extraction of chrysophanol is mostly carried out by water decoction, percolation, etc. The traditional extraction method is time-consuming and has a low extraction rate. Using ultra-high pressure impingement flow technology combined with macroporous resin adsorption purification technology can effectively improve the extraction of chrysophanol rate, and reduce the loss of active ingredients, reduce the content of pesticide residues in medicinal materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The medicinal material of cassia is dried, crushed, passed through a 40-mesh sieve, and the powder is soaked in ethanol. The soaked material is added to an ultra-high pressure extractor, and chrysophanol in cassia is extracted using ultra-high pressure and impinging flow technology. The pressure is 200 MPa and the temperature is normal temperature. , the macroporous adsorption resin AB-8 on the extracted chrysophanol, the mass ratio of the amount of resin to the raw material is 1:2, and the chloroform-methanol solution with a volume ratio of 20:1 is used for elution, and the eluate is collected and decompressed Concentrate to obtain a concentrate, the concentrate is separated and purified by high-speed countercurrent chromatography, using chloroform-methanol-water as a two-phase solvent system, the volume ratio of chloroform-methanol-water is 10:5:6, and the upper phase is used as a stationary phase, The lower phase is the mobile phase, the speed of the main machine is 8...

Embodiment 2

[0018] The medicinal material of cassia seed is dried, crushed, passed through a 40-mesh sieve, the powder is soaked in ethanol, and the soaked material is added to an ultra-high pressure extractor, and the chrysophanol in cassia seed is extracted by using ultra-high pressure and impinging flow technology, the pressure is 300MPa, and the temperature is normal temperature , the macroporous adsorption resin D-101 on the extracted chrysophanol, the mass ratio of the amount of resin to the raw material is 1:2, and the chloroform-methanol solution with a volume ratio of 20:1 is used for elution, and the eluate is collected and decompressed Concentrate to obtain a concentrate, the concentrate is separated and purified by high-speed countercurrent chromatography, using chloroform-methanol-water as a two-phase solvent system, the volume ratio of chloroform-methanol-water is 10:5:6, and the upper phase is used as a stationary phase, The lower phase is the mobile phase, the speed of the ...

Embodiment 3

[0020] The medicinal material of cassia is dried, crushed, passed through a 40-mesh sieve, and the powder is soaked in ethanol. The soaked material is added to an ultra-high pressure extractor, and chrysophanol in cassia is extracted using ultra-high pressure and impinging flow technology. The pressure is 200 MPa and the temperature is normal temperature. , the macroporous adsorption resin DA-201 on the extracted chrysophanol, the mass ratio of the amount of resin to the raw material is 1:2, and the chloroform-methanol solution with a volume ratio of 20:1 is used for elution, and the eluate is collected and decompressed Concentrate to obtain a concentrate, the concentrate is separated and purified by high-speed countercurrent chromatography, using chloroform-methanol-water as a two-phase solvent system, the volume ratio of chloroform-methanol-water is 10:5:6, and the upper phase is used as a stationary phase, The lower phase is the mobile phase, the host speed is 900rpm, and th...

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Abstract

The invention relates to a preparation method for wall breaking extraction of chrysophanol. The preparation method comprises: 1) taking Semen Cassiae, drying, crushing, screening with a 40 mesh sieve,immersing the powder in ethanol, adding the soaked material to an ultrahigh pressure extractor, and extracting the chrysophanol from the Semen Cassiae by using an ultrahigh pressure and impinging stream technology; 2) loading the extracted chrysophanol onto a macroporous adsorption resin, carrying out elution with a chloroform-methanol solution with a volume ratio of 20:1, collecting the eluent,and carrying out pressure reducing concentration to obtain a concentrated product; and 3) separating and purifying the concentrated product by using a high-speed countercurrent chromatography method,collecting the target fraction, recovering the reagent, and drying to obtain the product, wherein chloroform-methanol-water is used as a two-phase solvent system, the upper phase is taken as a stationary phase, the lower phase is taken as a mobile phase, the rotation speed of the main machine is 800-1000 rpm, and the flow rate is 2-3 mL / min. According to the present invention, the preparation method has advantages of less sample loss, good separation effect and low cost, and can obtain chrysophanol with characteristics of high content and good quality.

Description

technical field [0001] The invention relates to a preparation method for extracting chrysophanol by breaking walls, and belongs to the field of extraction of active ingredients of traditional Chinese medicines. Background technique [0002] Semen Cassiae is the dry mature seed of Cassia officinalis and Cassia officinalis of the leguminous plant. It tastes sweet, bitter, salty and slightly cold in nature. Dizziness, dim vision, habitual constipation, etc. [0003] The main active ingredients of Semen Cassiae are free anthraquinones, glycosides, and lactones, which have been widely used clinically for various cardiovascular and cerebrovascular diseases and hyperlipidemia. [0004] At present, the extraction of chrysophanol is mostly carried out by water decoction, percolation, etc. The traditional extraction method is time-consuming and has a low extraction rate. Using ultra-high pressure impingement flow technology combined with macroporous resin adsorption purification tech...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/10C07C50/34
CPCC07C46/10C07C50/34
Inventor 杨成东
Owner NANJING ZELANG AGRI DEV