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Method for purifying roburic acid

A purification method and technology of quercetin, which is applied in the field of traditional Chinese medicine extraction to achieve the effect of improving extraction rate and high product purity

Inactive Publication Date: 2012-01-25
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

After searching, there are no patents and literature reports on the industrial production method for preparing quercetin in China

Method used

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  • Method for purifying roburic acid

Examples

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Effect test

Embodiment 1

[0021] Take Gentiana medicinal material and crush it through a 50-mesh sieve, weigh 1kg, add 8L of cellulase aqueous solution of pH4.4 (140mg of cellulase per kilogram of crude drug) to soak for half an hour, and then enzymolyze it in a water bath at 40°C for 5 hours, and fully Stir, filter, take the filter residue and heat reflux with 8 times the amount of 80% ethanol to extract for 1 hour, extract 3 times, combine the extracts, concentrate under reduced pressure to obtain the extract, heat the extract to disperse, add NKA-2 macroporous adsorption Resin column, first take 3BV20% ethanol to elute the impurities, then take 5BV75% ethanol to elute the active ingredients, recover the ethanol under reduced pressure to obtain the crude extract, extract with ethyl acetate of equal volume, extract continuously for 4 times, combine the extracts, After concentration, the extract was subjected to silica gel column chromatography (silica gel particle size 100-200 mesh), eluted with cycloh...

Embodiment 2

[0024] Take Gentiana herb and crush it through a 60-mesh sieve, weigh 1 kg, add 8 L of cellulase aqueous solution (140 mg of cellulase per kg of crude drug) for soaking for half an hour, then enzymolyze it in a water bath at 50 °C for 2 hours, and fully Stir, filter, take the filter residue and heat reflux with 10 times the amount of 60% ethanol to extract for 1 hour, extract twice, combine the extracts, concentrate under reduced pressure to obtain the extract, heat the extract to disperse, add D4006 macroporous adsorption resin column , first take 3BV10% ethanol to elute impurities, then take 5BV80% ethanol to elute active ingredients, recover ethanol under reduced pressure to obtain crude extract, extract with equal volume of ethyl acetate, extract continuously for 3 times, combine extracts, extract After concentration, it was subjected to silica gel column chromatography (silica gel particle size: 100-200 mesh), eluted with cyclohexane-ethanol according to the gradient of 10...

Embodiment 3

[0027] Take Gentiana medicinal material and crush it through a 100-mesh sieve, weigh 1 kg, add 8 L of cellulase aqueous solution (140 mg of cellulase per kg of crude drug) for soaking for half an hour, then enzymatically hydrolyze in a water bath at 45°C for 4 hours, and fully Stir, filter, take the filter residue and heat reflux with 6 times the amount of 75% ethanol to extract for 1 hour, extract 3 times, combine the extracts, concentrate under reduced pressure to obtain the extract, heat the extract to disperse, add X-5 macroporous adsorption Resin column, first take 4BV20% ethanol to elute impurities, then take 5BV85% ethanol to elute active ingredients, recover ethanol under reduced pressure to obtain a crude extract, extract with equal volume of ethyl acetate, extract continuously for 4 times, combine the extracts, After the extract was concentrated, it was subjected to silica gel column chromatography (silica gel particle size: 200-300 mesh), eluted with cyclohexane-etha...

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Abstract

The invention discloses a method for purifying roburic acid, which comprises the following steps: (1) taking the raw material large leaf gentian root, drying, pulverizing, soaking in an enzyme solution, carrying out water bath enzymolysis, and sufficiently stirring; (2) filtering, extracting the filter residue with 5-10 times of ethanol water solution 2-3 times, merging the extracting solutions, and concentrating under reduced pressure to obtain an extract; (3) passing the extract through macroporous adsorbent resin columns, eluting with ethanol water solution, and collecting the eluate; (4) recycling ethanol from the eluate under reduced pressure, extracting by ethyl acetate, concentrating the extracting liquid, passing the extracting liquid through silica gel columns, carrying out cyclohexane-ethanol gradient elution, carrying out TLC (thin layer chromatography) tracking and monitoring, and collecting the roburic acid fraction; and (5) concentrating the roburic acid fraction under reduced pressure to small volume, standing to crystallize, and carrying out methanol / petroleum ether-acetone ethanol recrystallization. The invention is simple to operate, has the advantages of high product yield and low cost, and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of extraction of traditional Chinese medicines, and relates to a method for extracting and purifying quercetin from Gentiana quinquefolium. Background technique [0002] Roburic acid, also known as quercetin acid, molecular formula: C 30 h 48 o 2 ; Molecular weight: 440.707; Molecular structural formula is as follows: [0003] [0004] Querceric acid is an ingredient isolated from Gentiana chinensis. Gentiana chinensis is a commonly used Chinese herbal medicine. It was first recorded in "Shen Nong's Materia Medica". Pain, hemiplegia due to apoplexy, spasms of tendons, sore joints, jaundice due to damp heat, hot flashes due to bone steaming, and malnutrition fever in children. The 2010 edition of Pharmacopoeia stipulates that Gentiana is a Gentianaceae plant Gentiana Gentiana macrophyllia Pall., Gentiana chinensis Gentiana straminea Maxim., Gentiana thick stem Gentiana crassicaulis Duthie ex Burk...

Claims

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Application Information

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IPC IPC(8): C07C57/26C07C51/42
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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