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Thunberginol E extraction method

A sweet tea and flash extraction technology, which is applied in the field of extracting tea phenol E, can solve problems such as no reports on the production process of tea phenol E, and achieve the effects of easy large-scale production, high product purity, and large sample loading.

Inactive Publication Date: 2014-10-08
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, there is no report on the production process of industrialized preparation of Glycyrrhiol E

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Use sweet tea leaves as raw materials, cut into 1cm sections, put them into a high-speed tissue grinder, keep them for 5 minutes at a speed of 18,000rpm, pass through a 40-mesh sieve for later use, weigh 1kg, and weigh 1kg according to the material-to-liquid ratio of 1:12 (g / mL) after adding 85% ethanol aqueous solution, then adding 0.5% cellulase, and enzymatically hydrolyzing for 70min under the conditions of ultrasonic power 700W and 45°C to obtain enzymolysis raw materials, which were added to a flash extractor with an extraction voltage of 150V , the extraction time is 3min, flash extraction is carried out, the extract is obtained by filtration, the extract is concentrated and dried to obtain a crude extract, dissolved in methanol, and dry-loaded to a high-pressure silica gel (silica gel mesh is 200 mesh) column chromatography for purification. The pressure resistance is 35MPa, the inner diameter of the column is 250mm, the diameter-to-height ratio of the chromatog...

Embodiment 2

[0025] Use sweet tea leaves as raw materials, cut them into 1cm sections, put them into a high-speed tissue grinder, keep them at a speed of 18,000 rpm for 3 minutes, pass through a 40-mesh sieve for later use, weigh 1kg, and weigh 1kg according to the material-to-liquid ratio of 1:16 (g / mL) after adding 85% ethanol aqueous solution, then adding 0.5% cellulase, and enzymatically hydrolyzing for 90min under the conditions of ultrasonic power 700W and 45°C to obtain enzymolysis raw materials, which were added to a flash extractor with an extraction voltage of 150V , the extraction time is 5min, flash extraction is carried out, the extract is obtained by filtration, the extract is concentrated and dried to obtain a crude extract, dissolved in methanol, and dry-loaded to a high-pressure silica gel (silica gel mesh is 200 mesh) column chromatography for purification. The pressure resistance is 35MPa, the inner diameter of the column is 250mm, the diameter-to-height ratio of the chr...

Embodiment 3

[0027] Use sweet tea leaves as raw materials, cut into 1cm sections, put them into a high-speed tissue grinder, keep at a speed of 18,000rpm for 5 minutes, pass through a 40-mesh sieve for later use, weigh 1kg, and weigh 1kg according to the material-to-liquid ratio of 1:15 (g / mL) after adding 85% ethanol aqueous solution, then adding 0.5% cellulase, and enzymatically hydrolyzing for 65min under the conditions of ultrasonic power 700W and 45°C to obtain enzymolysis raw materials, which were added to a flash extractor with an extraction voltage of 150V , the extraction time is 4min, flash extraction is carried out, the extract is obtained by filtration, the extract is concentrated and dried to obtain a crude extract, dissolved in methanol, and dry-loaded to a high-pressure silica gel (silica gel mesh is 200 mesh) column chromatography for purification. The pressure resistance is 35MPa, the inner diameter of the column is 250mm, the diameter-to-height ratio of the chromatographi...

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PUM

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Abstract

The invention discloses a thunberginol E extraction method. The method is characterized in comprising the following steps: hydrangea macrophylla leaf is adopted as a raw material; through tissue crushing and cellulase enzymolysis, an enzymolyzed raw material is obtained; the material is added into a flash extractor and is subjected to flash extraction; filtering is carried out, such that an extract liquid is obtained; concentration and drying are carried out; high-pressure silica gel column chromatographic purification is carried out; thunberginol E fraction is collected; reduced-pressure concentration is carried out; and acetone recrystallization is carried out, such that thunberginol E is obtained. The method provided by the invention is simple to operate, and is suitable for large-scale productions. The method has the advantages of low energy consumption, low pollution, and short production period. The method is an environment-friendly production process.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicine chemistry, and relates to a method for extracting licoriceol E. Background technique [0002] Thunberginol E, mp.216-217℃, molecular formula C 16 h 14 o 6 , the molecular weight is 302.28, and the structural formula is: [0003] [0004] Glycyrrhiol E is an isocoumarin compound isolated from the leaves of Hydrangea macrophylla Seringe var. thunbergii Makin from the family Saxifragaceae. Pharmacological studies have shown that licoriceol E has anti-allergic activity, and it has anti-allergic effect on sensitized guinea pig bronchi. The IC50 (μM) for S.D. response and compound 48 / 80 sensitization are 37 and 85, respectively. At 100 μM, the group The amine release inhibition rate is 97.9%; it has antibacterial activity, the MIC for Fusobacterium nucleatum is 30ppm, and the MIC for Bacteroides melaninus is 50ppm. [0005] In the prior art, there is no report on the product...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/76
CPCC07D311/76
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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