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Preparation method of pedunculoside

A long-stemmed glucoside and extraction technology, which is applied in the field of medicine, can solve the problems of long production cycle, high cost, and low output of silica gel column chromatography, and achieve the effects of obvious energy saving, simple operation, and low pollution

Inactive Publication Date: 2012-08-29
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses highly toxic chloroform to degrease, and the silica gel column chromatography has small output, long production cycle and high cost, and cannot meet the needs of industrial production.

Method used

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  • Preparation method of pedunculoside

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Take 1 kg of Sijiqing medicinal material, crush it into a coarse powder of 20-40 mesh, add it to the extraction kettle, set the extraction temperature to 40°C, the pressure to 35MPa, CO 2 The flow rate is 22L / h, the separation pressure is 9MPa, and the separation temperature is 45°C; after the system reaches the set temperature, turn on the CO 2 Cylinder valves that allow CO 2 Enter the extraction kettle, start the extraction after the system pressure is balanced, extract for 4 hours, and collect the extract after the extraction is completed. Dissolve the extract in hot water, filter, and add the filtrate to the XDA-1 macroporous adsorption resin column at a flow rate of 1BV / h. After applying the drug solution, first elute with 4BV deionized water, and then elute with 50% ethanol solution. Collect the eluate, concentrate under reduced pressure to 1 / 5 of the total volume, place it at 4°C for 10 hours, centrifuge (10000r / min), recrystallize the precipitate with 80% ethan...

Embodiment 2

[0020] Take 1 kg of Sijiqing medicinal material, crush it into a coarse powder of 20-40 mesh, add it to the extraction kettle, set the extraction temperature to 55 ° C, the pressure to 33 MPa, CO 2 The flow rate is 28L / h, the separation pressure is 5MPa, and the separation temperature is 42°C; after the system reaches the set temperature, turn on the CO 2 Cylinder valves that allow CO 2 Enter the extraction kettle, start the extraction after the system pressure is balanced, extract for 3 hours, and collect the extract after the extraction is completed. Dissolve the extract in hot water, filter, and add the filtrate to the AB-8 macroporous adsorption resin column with a flow rate of 1.5BV / h. After the liquid is applied, it is first eluted with 6BV deionized water, and then eluted with 50% ethanol solution , collect the eluate, concentrate under reduced pressure to 1 / 4 of the total volume, place it at 5°C for 8 hours, centrifuge (10000r / min), recrystallize the precipitate with ...

Embodiment 3

[0022] Take 1 kg of Sijiqing medicinal material, crush it into a coarse powder of 20-40 mesh, add it to the extraction kettle, set the extraction temperature to 47°C, the pressure to 21MPa, CO 2 The flow rate is 18L / h, the separation pressure is 7MPa, and the separation temperature is 43°C; after the system reaches the set temperature, turn on the CO 2 Cylinder valves that allow CO 2 Enter the extraction kettle, start the extraction after the system pressure is balanced, extract for 3 hours, and collect the extract after the extraction is completed. Dissolve the extract in hot water, filter, add the filtrate to the AB-8 macroporous adsorption resin column, the flow rate is 1.5BV / h, after the liquid is applied, first elute with 5BV deionized water, and then elute with 50% ethanol solution , collect the eluate, concentrate under reduced pressure to 1 / 4 of the total volume, place it at 5°C for 8 hours, centrifuge (10000r / min), recrystallize the precipitate with 80% ethanol, and ...

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PUM

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Abstract

The invention discloses a preparation method of pedunculoside. The method sequentially comprises the following steps of: (a) crushing leaf of purpleflower holly, adding into an extraction kettle, and collecting pedunculoside extract by using supercritical CO2 extraction; (2) dissolving the extract with hot water, filtering, adding a macoporous resin column into filtrate to adsorb, eluting with water to remove impurities, eluting with 30-50 percent ethanol solution, concentrating eluate under reduced pressure, standing at low temperature and centrifuging to obtain precipitate; and (3) recrystallizing the precipitate with ethanol to obtain the pedunculoside. The preparation method is simple, suitable for industrial large-scale production, low in energy consumption and low in pollution and is an environment-friendly production process.

Description

Technical field: [0001] The invention belongs to the field of medicine, and in particular relates to a preparation method of pedicel glucoside. Background technique: [0002] Sijiqing is a commonly used Chinese herbal medicine in my country, which is the dried leaves of Ilex purpurea Hassk. Harvested in autumn and winter and sun-dried. Sijiqing has the effects of clearing heat and detoxifying, reducing swelling and blood stasis. Clinically used for acute and chronic bronchitis, pneumonia, acute pharyngitis, biliary tract infection, urinary tract infection, dysentery, burns, etc. Sijiqing is widely distributed in all provinces and regions south of the Yangtze River, and its medicinal resources are very rich. Folks use Sijiqing water decoction to treat burns and scalds, and the effect is particularly good. Modern studies have shown that Sijiqing has broad-spectrum antibacterial effects and significant pharmacological effects on the cardiovascular system. Injections, tablet...

Claims

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Application Information

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IPC IPC(8): C07J63/00
CPCY02P20/54
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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