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Method for separating and purifying sec-o-glucosylhamaudol

A technology for separation and purification of helicol glycosides, which is applied in the field of separation and purification of heliconia glycosides, and can solve problems such as the separation and purification of non-monomer components

Inactive Publication Date: 2012-07-04
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

Patent 200710001127.5 provides a total chromone extract of Fangfeng and its preparation method. The invention obtains a total chromone extraction with a total chromone content of 5-100% through solvent extraction, macroporous adsorption resin method and other preparations of Fangfeng substances, but did not separate and purify the individual monomer components, only the mixture

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 500g of the windproof chromone extract, heat and reflux extraction with 2.5L of 90% ethanol, control the temperature at about 70°C, extract twice, combine the extracts, recover the reagent to 500ml under reduced pressure, add D140 macroporous resin with a column volume of 1L Column adsorption, the flow rate of the upper column is 0.6BV / h, and after the adsorption is saturated, it is eluted with water until the sugar reaction is negative, and then eluted with 60% ethanol at a flow rate of 1.0L / h. Concentrate under pressure to a relative density of 1.15, add 100ml petroleum ether for extraction, extract twice, discard the extract, then extract twice with 150ml ethyl acetate, concentrate under reduced pressure, add the pretreated Toyopearl HW-40 (200g) column Chromatography, eluting with 80% methanol aqueous solution, TLC monitoring, collecting the effluent of the target component, combining the same fractions, and drying at low temperature to obtain coarse crystals, w...

Embodiment 2

[0017] Take 500g of Radix chromogenone extract, heat and reflux extraction with 2.0L 70% acetone, control the temperature at about 65°C, extract 3 times, combine the extracts, recover the reagent to 500ml under reduced pressure, add HPD600 macroporous resin with a column volume of 1L Column adsorption, the flow rate of the upper column is 0.7BV / h, and after the adsorption is saturated, it is eluted with water until the sugar reaction is negative, and then eluted with 80% ethanol, and the flow rate is 1.0L / h. Concentrate under reduced pressure to a relative density of 1.18, add 120ml petroleum ether for extraction, extract twice, discard the extract, then extract twice with 180ml ethyl acetate, concentrate under reduced pressure, add pretreated Sephadex G (200g) column chromatography , eluted with 60% ethanol aqueous solution, TLC monitoring, collected the effluent of the target component, combined the same fractions, dried at low temperature to obtain coarse crystals, and recry...

Embodiment 3

[0019] Take 1000g of the wind chromone extract, heat and reflux extraction with 5L of 90% methanol, control the temperature at 80°C, extract twice, combine the extracts, recover the reagents under reduced pressure to 500ml, add a D140 macroporous resin column with a column volume of 1L for adsorption , the flow rate on the column is 0.5BV / h, after the adsorption is saturated, it is eluted with water until the sugar reaction is negative, and then eluted with 75% ethanol at a flow rate of 1.0L / h. When the relative density is 1.20, add 170ml petroleum ether for extraction, extract twice, discard the extract, then extract twice with 200ml ethyl acetate, concentrate under reduced pressure, add pretreated Toyopearl HW-40 (400g) column chromatography , eluted with 70% acetone aqueous solution, TLC monitoring, collected the effluent of the target component, combined the same fractions, and dried at low temperature to obtain coarse crystals, which were recrystallized from acetone to obt...

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Abstract

The invention relates to a method for separating and purifying sec-o-glucosylhamaudol, which is characterized in that the method is a method for separating and purifying the sec-o-glucosylhamaudol from wind-resisting chromone extractive by using macroporous resin adsorption and gel column chromatography. The method uses the commercially available wind-resisting chromone extractive as raw materials, and comprises the steps of solvent backflow dissolving, resin adsorption, organic solvent extraction, gel column chromatography separation purification, recrystallization and the like. The method is characterized in that carbinol, ethanol, acetone or their mixed solvent serve as dissolving solvent and are heated for backflow for 1-3 hours, portions enriching the sec-o-glucosylhamaudol are obtained through resin adsorption and separation, and then the sec-o-glucosylhamaudol is separated and purified through the gel column chromatography. The method for extracting the sec-o-glucosylhamaudol is simple in method, high in repeatability, low in drying temperature, good in product quality and high purity.

Description

Technical field: [0001] The invention belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines, and in particular relates to a method for separation and purification of helichrenol glycosides. Background technique: [0002] The windproof is the dry root of the Umbelliferae plant windproof Saposhnikovia divaricata (Turcz.) Schischk. It is one of the commonly used bulk medicinal materials in my country. It has the functions of relieving exterior and expelling wind, eliminating dampness, and relieving spasm. The main active ingredients of Fangfeng are chromones such as acteoside, cimicrol glycoside, 5-O-methyl visamidol glycoside, and cochinol glycoside, as well as polysaccharides and coumarins. Modern pharmacological studies have shown that Fangfeng chromone has antipyretic, analgesic, anti-inflammatory, anti-tumor, anti-platelet aggregation and other functions, and is used to treat concussion, respiratory tract infe...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/06
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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