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Method for separating and preparing cleome gynandra glycoside from capparis spinosa

A mouse melon and white flower technology, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc.

Inactive Publication Date: 2013-02-06
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] After searching, there is no patent report on the industrial production method for the separation and preparation of brackenin in China

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take the mouse melon fruit, crush it, weigh 1kg, extract it with 70% aqueous methanol solution of 5 times (v / w) the mass of the medicinal material, filter to obtain the extract, concentrate it in a vacuum to a small volume, and extract it 3 times with ethyl acetate , the aqueous phase was concentrated to obtain a crude extract, and the lilyflower glycoside in the crude extract was separated and purified by high-speed countercurrent chromatography, and n-butanol, acetonitrile, and pH4.5 ammonium acetate buffer were measured in a volume ratio of 2:0.5:1.5, Put it in a separatory funnel, shake it well, let it stand for stratification, separate the upper and lower phases, inject the upper phase into the high-speed countercurrent chromatographic column at a flow rate of 20ml / min, take the crude extract and dissolve it in the lower phase to prepare 1g / 25ml Turn on the countercurrent chromatograph until the rotation speed is 800r / min, input the sample solution at a flow rate of...

Embodiment 2

[0015] Take the mouse melon fruit, crush it, weigh 1kg, extract it with 70% aqueous methanol solution of 5 times (v / w) the mass of the medicinal material, filter to obtain the extract, concentrate it in a vacuum to a small volume, and extract it twice with ethyl acetate , the aqueous phase was concentrated to obtain a crude extract, and the lilyflower glycoside in the crude extract was separated and purified by high-speed countercurrent chromatography, and n-butanol, acetonitrile, and pH4.5 ammonium acetate buffer solution were measured in a volume ratio of 3:0.5:1.5, Put it in a separatory funnel, shake it well, let it stand for stratification, separate the upper and lower phases, inject the upper phase into the high-speed countercurrent chromatographic column at a flow rate of 20ml / min, take the crude extract and dissolve it in the lower phase to prepare 1g / 25ml Turn on the countercurrent chromatograph to a speed of 900r / min, input the sample solution at a flow rate of 1ml / mi...

Embodiment 3

[0017] Take the mouse melon fruit, crush it, weigh 1kg, extract it with 70% aqueous methanol solution of 8 times (v / w) the mass of the medicinal material, filter to obtain the extract, concentrate it in a vacuum to a small volume, and extract it three times with ethyl acetate , the aqueous phase was concentrated to obtain a crude extract, and the lilyflower glycoside in the crude extract was separated and purified by high-speed countercurrent chromatography, and n-butanol, acetonitrile, and pH4.5 ammonium acetate buffer solution were measured in a volume ratio of 3:0.5:1, Put it in a separatory funnel, shake it well, let it stand for stratification, separate the upper and lower phases, inject the upper phase into the high-speed countercurrent chromatographic column at a flow rate of 20ml / min, take the crude extract and dissolve it in the lower phase to prepare 1g / 25ml Turn on the countercurrent chromatograph until the rotation speed is 850r / min, input the sample solution at a f...

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Abstract

The invention discloses a method for separating and preparing cleome gynandra glycoside from capparis spinosa. The method comprises the steps that: (1) capparis spinosa fruits are crushed, and are subjected to soak extraction by using methanol; (2) the extract obtained by soak extraction is subjected to preliminary purification by using an extraction method, such that a crude extract is obtained; and (3) cleome gynandra glycoside in the crude extract is separated and purified by using a high-speed countercurrent chromatography method, wherein a solvent system is an n-butanol-acetonitrile-ph4.5 ammonium acetate buffer solution (a volume ratio is 2-3:0.5:1-1.5). The method provided by the invention has the advantages of simple operation, and low cost. The method is economical and practical. With the method, the purity of cleome gynandra glycoside obtained by separation is higher than 95%.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of traditional Chinese medicines, and relates to a method for separating and preparing lilyflower glycosides from mouse melon. Background technique [0002] Mouse melon Capparis spinosa L. is a plant of the genus Capparis in the cauliflower family, also known as capers and wild watermelons. It has a bitter taste and warm nature, and has the functions of expelling wind and cold, dehumidification, pain relief, regulating menstruation, and reducing swelling. It is mainly used to treat rheumatoid arthritis and gout. Modern pharmacological studies have shown that the water extract of mouse melon has the functions of protecting the liver, lowering blood sugar, lowering blood fat, antibacterial and scavenging free radicals. Sulfur-containing compounds are the main chemical components of mouse melon. It mainly exists in the form of glucosinolates, also known as glucose isothiocyanate. I...

Claims

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Application Information

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IPC IPC(8): C07H15/14C07H1/08
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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