Method for extracting stephanine from stephania

A technology of stephine and stephine, which is applied in the field of extracting stephine by means of supercritical CO2 extraction, which can solve the problems of small separation capacity and long extraction cycle, and achieve high extract content, good reproducibility and high efficiency Effect

Inactive Publication Date: 2011-04-20
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is relatively simple, but the extraction period is long, and the amount of subsequent separation processing is small

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take Stephania medicinal material, grind it into 80 meshes, take 500g and put it into the extraction kettle, turn on the equipment and adjust the parameters: the extraction temperature is 50°C, the extraction pressure is 45MPa, the temperature of the separation kettle I is 45°C, the pressure is 8MPa, the temperature of the separation kettle II is 40 ℃, the pressure is 5MPa. After the above parameters are reached, extract at a flow rate of 30L / h and pump 95% ethanol entrainer at a flow rate of 70g / h at the same time, extract for 3 hours, analyze the extract, dissolve the extract with 2% hydrochloric acid, filter, and add the filtrate to the D151 cationic resin column for adsorption , deionized water to elute neutrality, take 1L of 80% ethanol solution, adjust the pH to 9 with ammonia water, elute the resin column, concentrate the eluent under reduced pressure, add 200g of neutral alumina (particle size 100-300 mesh) to the concentrated solution, mix well and dry , using ...

Embodiment 2

[0023] Take Stephania medicinal material, crush 60 meshes, take 500g and put it into the extraction kettle, start the equipment and adjust the parameters: the extraction temperature is 45°C, the extraction pressure is 50MPa, the temperature of the separation kettle I is 45°C, the pressure is 6MPa, the temperature of the separation kettle II is 30 ℃, the pressure is 4MPa. After reaching the above parameters, extract at a flow rate of 35L / h and pump 99% methanol entrainer at a flow rate of 100g / h at the same time, extract for 2 hours, analyze the extract, dissolve the extract with 1% sulfuric acid, filter, add HZD-5 cationic resin to the filtrate Column adsorption, neutral elution with deionized water, take 2L of 40% methanol solution, adjust the pH to 11 with ammonia water, elute the resin column, concentrate the eluent under reduced pressure, add 200g of neutral alumina (particle size 100-300 mesh) to the concentrated solution and mix well Drying, ultrasonic extraction with 90...

Embodiment 3

[0025] Take Stephania medicinal material, crush 40 meshes, take 500g and put it into the extraction kettle, start the equipment and adjust the parameters: the extraction temperature is 45°C, the extraction pressure is 50MPa, the temperature of the separation kettle I is 40°C, the pressure is 6MPa, the temperature of the separation kettle II is 30 ℃, the pressure is 4MPa. After reaching the above parameters, extract at a flow rate of 40L / h and pump 99% methanol entrainer at a flow rate of 150g / h, extract for 1 hour, analyze the extract, dissolve the extract with 1% sulfuric acid, filter, and add HD-8 cationic resin to the filtrate Column adsorption, neutral elution with deionized water, take 1.5L of 60% methanol solution, adjust the pH to 10 with ammonia water, elute the resin column, concentrate the eluent under reduced pressure, add 250g of neutral alumina (particle size 100-300 mesh) to the concentrated solution and mix Dry it evenly, use 80% methanol for ultrasonic extracti...

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PUM

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Abstract

The invention provides a method for extracting stephanine from stephania. In the invention, stephania medicinal materials are taken as raw materials. The method comprises the following steps of: smashing the raw material into 40 to 80 meshes, and adding the raw material to an extractor; extracting by adopting supercritical CO2; collecting stephanine extracts; dissolving the stephanine extracts by acid water, and filtering the stephanine extracts; adding cation exchange resin for absorption; washing ion columns by water until the ion columns are neutral, and eluting by utilizing 4 to 7 times of alkaline alcohol; decompressing and concentrating eluent, and adding alumina mixed samples to the concentrated solution for drying; ultrasonically extracting by utilizing methyl alcohol solution; decompressing and concentrating extracting solution; adjusting pH by utilizing ammonia water, and standing for crystallizing; and recrystallizing by utilizing ethanol solution and drying to obtain a product. The method for producing stephanine has the advantages of little energy consumption, little pollution and high product content and is suitable for industrial production.

Description

Technical field: [0001] The present invention relates to a kind of method extracting stephanine from Stephania vine, particularly relates to a kind of application supercritical CO 2 Extraction means A method for extracting stephine. Background technique: [0002] Stephanine is also known as Stephanine, molecular formula C 37 h 38 N 2 o 6 , Molecular weight 606.71, easily soluble in chloroform, methanol, ethanol, slightly soluble in petroleum ether, insoluble in water. [0003] Stephanine can increase peripheral blood leukocytes. Animal experiments have found that it can significantly prevent leukopenia caused by mitomycin, but it does not inhibit the anticancer effect of mitomycin. Its mechanism of action is to promote the proliferation of bone marrow tissue, thereby producing the effect of increasing white blood cells. It is used for agranulocytosis caused by tumor chemotherapy and radiotherapy and leukopenia caused by other reasons. [0004] The existing method of s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22
CPCY02P20/54
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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