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Method for extracting swertiamarin with supercritical fluid

A technology of rubiacin and supercritical fluid, which is applied in the production of bulk chemicals, organic chemistry, etc., can solve the problems such as the inability to obtain high content of rubiacin, and achieves no solvent residue, good reproducibility, and extraction temperature. low effect

Inactive Publication Date: 2012-07-11
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

[0005] At present, there are few domestic literatures on the extraction and purification process of rubidin. Tan Chaoyang, Liu Qian, Peng Liang, etc. all use ethanol reflux extraction. This method only obtains the crude extract of madder, and cannot obtain high content of rubidin.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 1kg madder and crush it to 50 meshes, then infiltrate it with 4L of 90% ethanol in an airtight manner for 1 hour, put it into a 5L supercritical extraction kettle, and use CO 2 As the extraction solvent, the extraction pressure is 26MPa, the temperature is 37°C, the extraction time is 3h, CO 2 The flow rate was 0.3L / min. During the whole extraction process, 200ml of ethanol as an entrainer was injected at a flow rate of 2ml / min; the separation kettle was analyzed and separated under a pressure of 4MPa to obtain 81g of extract. Dissolve the extract in petroleum ether, put it on a silica gel chromatography column, first elute with petroleum ether-ethyl acetate 50:1, and then elute with 90% ethanol, collect the ethanol eluted part, recover ethanol under reduced pressure, and concentrate to 6.05 g of Rubidolin is obtained by extracting the extract and drying at low temperature, with a content of 92%.

Embodiment 2

[0019] Take 1kg madder and crush it to 20 meshes, then infiltrate it with 6L of 70% ethanol in an airtight manner for 2 hours, put it into a 5L supercritical extraction kettle, and use CO 2 As the extraction solvent, the extraction pressure is 28MPa, the temperature is 36°C, the extraction time is 2h, CO 2 The flow rate was 0.4L / min. During the whole extraction process, 280ml of entrainer ethanol was introduced at a flow rate of 3ml / min; the separation kettle was analyzed and separated at a pressure of 7MPa to obtain 78g of extract. Dissolve the extract in petroleum ether, put it on a silica gel chromatography column, first elute with petroleum ether-ethyl acetate 34:1, and then elute with 95% methanol, collect the methanol eluted part, recover methanol under reduced pressure, and concentrate to Extraction, low-temperature drying can obtain 6.43g rubiacin, the content is 92%.

Embodiment 3

[0021] Take 1kg madder and crush it to 40 meshes, then infiltrate it with 8L of 80% ethanol in an airtight manner for 3 hours, put it into a 5L supercritical extraction kettle, and use CO 2 As the extraction solvent, the extraction pressure is 32MPa, the temperature is 39°C, the extraction time is 4h, CO 2 The flow rate was 0.25L / min. During the whole extraction process, 330ml of entrainer ethanol was introduced at a flow rate of 5ml / min; the separation kettle was analyzed and separated at a pressure of 4MPa to obtain 79g of extract. Dissolve the extract in petroleum ether, put it on a silica gel chromatography column, first elute with petroleum ether-ethyl acetate 48:1, and then elute with 95% ethanol, collect the eluted part of ethanol, recover ethanol under reduced pressure, and concentrate to Extraction, low-temperature drying can obtain 5.49g rubiacin, the content is 95%.

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Abstract

The invention belongs to the technical field of extraction of Chinese medicinal active ingredients, and particularly relates to a method for extracting swertiamarin with a supercritical fluid. The method comprises the following steps of: soaking swertiamarin with an ethanol solution; putting into an extracting kettle; extracting by taking supercritical CO2 as an extracting agent and taking ethanol as an entrainer; decompressing, separating and discharging; and purifying and separating an extract through column chromatography, and eluting with an eluent, wherein the extracting pressure is 25-45 MPa, the temperature is 30-60 DEG C, the extracting time is 1-5 hours, and the resolution pressure is 4-8 MPa; silica gel is taken as a column chromatography filler; and a petroleum ether-ethyl acetate mixed solvent, ethanol or methanol is taken as the eluent. Through supercritical CO2 extraction, the obtained swertiamarin has good quality and high purity; and the entire method has short operating time and a simple process.

Description

Technical field: [0001] The invention belongs to the technical field of extracting active ingredients of traditional Chinese medicine, and relates to a method for extracting rubia rubidis with supercritical fluid, in particular to a method using supercritical CO 2 A method for extracting and purifying Rubioside from Radix Rubiae by extraction and silica gel column chromatography. Background technique: [0002] Rubidolin is a naphthoquinone. Molecular formula: C 17 h 15 o 4 , molecular weight: 283.30, mp.128-132°C. It is a yellow flaky crystal with a melting point of 128-132°C. It is sublimable, insoluble in water, soluble in ether and ethanol, and easily soluble in chloroform and ethyl acetate. [0003] Rubia cordifolia L. was first recorded in "Shen Nong's Materia Medica", and has the effects of cooling blood, removing blood stasis, stopping bleeding, and promoting menstruation. Tumbling and swelling. Rubia is mainly produced in Shaanxi, Henan and other places. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/92
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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