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Method for extracting and purifying gericudranin A

A technology of ezetin and Geely, applied in the field of extracting and purifying Geely zerein A, can solve the problems such as no extraction and purification method of Geely zerein A, and achieve the effects of low cost, high extraction efficiency and good separation effect.

Inactive Publication Date: 2012-12-19
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] After literature search, there is no report on the extraction and purification method suitable for high-purity Gelicin A

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 500g of the coarse powder of the stem bark of Zheshu, and use the supercritical carbon dioxide technology to extract the oily substances in the bark of Zheshu. % acetone solution for ultrasonic cycle extraction once, each time for 1h, the combined extracts were concentrated and then applied to a polyamide resin column. Deliquified, concentrated, mixed with 100-200 mesh silica gel at a weight ratio of 1:1, dried in the shade, placed on a short and thick silica gel column with a diameter-to-height ratio of 1:5, and a mixed solution of ethyl acetate-acetone as the eluent. Carry out elution in sequence according to the volume ratio of 1:5, 1:10, and 1:15, collect the eluate containing Geelysin A, recover the reagent, and place the obtained Geelysin A concentrated solution in a crystallization tank to stand still Make it crystallize for 20 hours, filter, separate out the crystals, recrystallize with acetone-n-hexane (1.5:1) mixed solvent, filter out the crystals, and fr...

Embodiment 2

[0025] Take 500g of the coarse powder of the stem bark of Zheshu, and use supercritical carbon dioxide technology to extract the oily substances in the bark of Zheshu. The extraction temperature is 40°C, the pressure is 25MPa, the extraction time is 0.5h, and the residue is increased by 7 times (V / W) 80% acetone solution was subjected to ultrasonic circulation extraction twice, each time for 1 hour, the combined extracts were concentrated and then applied to a polyamide resin column, first eluted with water and 35% ethanol solution, then eluted with 75% ethanol solution, and collected 75% ethanol Concentrate the eluent, mix well with 100-200 mesh silica gel at a weight ratio of 1:1, dry in the shade, put on a short and thick silica gel column with a diameter-to-height ratio of 1:5, and use ethyl acetate-acetone mixed solution as eluent , sequentially eluted according to the volume ratio of 1:5, 1:9, and 1:13, collected the eluate containing Geelysin A, recovered the reagent, an...

Embodiment 3

[0027] Take 500g of the coarse powder of the stem bark of Zheshu, and use supercritical carbon dioxide technology to extract the oily substances in the bark of Zheshu, the extraction temperature is 45°C, the pressure is 28MPa, the extraction time is 0.5h, and the residue is increased by 10 times (V / W) 90% acetone solution was subjected to ultrasonic circulation extraction once, each time for 2 hours, the extracts were combined, concentrated and then applied to a polyamide resin column, first eluted with water and 35% ethanol solution, then eluted with 75% ethanol solution, and collected 75% ethanol Concentrate the eluent, mix well with 100-200 mesh silica gel at a weight ratio of 1:1, dry in the shade, put on a short and thick silica gel column with a diameter-to-height ratio of 1:5, and use ethyl acetate-acetone mixed solution as eluent , followed by elution according to the volume ratio of 1:5, 1:10, and 1:15, collecting the eluate containing Geelysin A, recovering the reagen...

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PUM

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Abstract

The invention discloses a method for extracting and purifying gericudranin A, which comprises the following steps of: 1) using barks of Cudrania tricuspidata Bureau as raw materials, drying and crushing the raw materials, and extracting grease substances in the barks of Cudrania tricuspidata Bureau by adopting a supercritical carbon dioxide technique; 2) adding residues into acetone solution for ultrasonic circulating extraction; 3) concentrating the extract, adding the concentrated extract into a polyamide resin column, firstly eluting by using water and 35% ethanol solution, then eluting by using 75% ethanol solution and collecting 75% ethanol eluent; 4) concentrating the eluent, adding the concentrated eluent into a silica gel short wide column, using ethyl acetate - acetone mixed solution as eluting agent, collecting the eluent, concentrating the eluent and placing for crystallization; and 5) separating out crystals, recrystallizing by using acetone - normal hexane mixed solvent, filtering out crystals and freeze-drying the crystals to obtain the gericudranin A. The method provided by the invention has the advantages that the method is simple to operate and large-scale production can be realized.

Description

technical field [0001] The invention belongs to the field of natural medicines, in particular, the invention relates to a method for extracting and purifying Gelicin A. Background technique [0002] Gericudranin A (Gericudranin A), is a flavonol compound, molecular formula: C 29 h 24 o 9 , Molecular weight: 516.5, yellow powder, mp135°C. Mainly found in Moraceae (Moraceae) Zhe tree Cudrania tricuspidata In the stem bark of Bureau. [0003] Modern pharmacological studies have shown that Gelicin A has cytotoxic activity. ED on human tumor cells 50 (μg / ml) is 3.65 for skin cancer CRL1579, 11.99 for skin cancer LOX-IMVI, 2.65 for leukemia MOLT-4F, 13.70 for colon cancer KM12, and 6.99 for kidney cancer UO-31. [0004] According to literature search, there is no report on the extraction and purification method suitable for high-purity Gelicin A. Contents of the invention [0005] The technical problem to be solved by the present invention is to provide a method for extr...

Claims

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Application Information

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IPC IPC(8): C07D311/32C07D311/40
CPCY02P20/54
Inventor 刘东锋
Owner NANJING ZELANG MEDICAL TECH
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