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A kind of preparation method of hydrangea phenol

A hydrangea phenol, supercritical technology, applied in the production of bulk chemicals, organic chemistry, etc., to achieve the effect of low energy consumption, low pollution, and conducive to large-scale production operations

Inactive Publication Date: 2011-12-07
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity hydrangea phenol

Method used

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  • A kind of preparation method of hydrangea phenol

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Embodiment 1

[0025] Get 10Kg of hydrangea leaves, crush them, and add them to CO 2 In the supercritical extractor, ethyl acetate is used as the entrainer, the entrainer accounts for 1% by volume of the total extraction solvent, the extraction pressure is 20MPa, the temperature is 50°C, CO 2 The flow rate is 1ml / g crude drug·min, the extraction time is 100min, and the extract is obtained, which is added to a HPD-700 macroporous adsorption resin column for adsorption, eluted with 50% ethanol, and the eluate that is 3 times the volume of the column is collected, and recovered under reduced pressure Ethanol was concentrated, and dichloromethane was added to crystallize, the crystals were separated, washed and dried to obtain 56.7 g of hydrangel, which was detected by HPLC with a purity of 95.5%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 2

[0027] Get 10Kg of hydrangea leaves, crush them, and add them to CO 2 In the supercritical extractor, ethyl acetate is used as the entrainer, the entrainer accounts for 3% by volume of the total extraction solvent, the extraction pressure is 40MPa, the temperature is 60°C, CO 2 The flow rate is 3ml / g crude drug·min, the extraction time is 150min, and the extract is obtained, which is added to the H-50 macroporous adsorption resin column for adsorption, eluted with 70% ethanol, and the eluate with 8 times the volume of the column is collected, and recovered under reduced pressure Ethanol was concentrated, and dichloromethane was added to crystallize, the crystals were separated, washed, and dried to obtain 63.2 g of hydrangel, which was detected by HPLC with a purity of 94.7%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 3

[0029] Get 10Kg of hydrangea leaves, crush them, and add them to CO 2 In the supercritical extractor, ethyl acetate is used as the entrainer, the entrainer accounts for 2% by volume of the total extraction solvent, the extraction pressure is 30MPa, the temperature is 55°C, CO 2 The flow rate is 2 ml / g crude drug·min, the extraction time is 120min, and the extract is obtained, which is added to a CD-180 macroporous adsorption resin column for adsorption, eluted with 60% ethanol, and the eluate with 5 times the volume of the column is collected and decompressed. Recover ethanol and concentrate, add dichloromethane to crystallize, separate and crystallize, wash and dry to obtain 61.9g hydrangenol, which is detected by HPLC with a purity of 98.2%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

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Abstract

The invention relates to a preparation method of hydrangea phenol with simple and convenient operation, less pollution and less energy consumption. The process steps are: take hydrangea leaves, crush them, add them to a CO2 supercritical extractor, use ethyl acetate as an entrainer to obtain an extract, add them to a macroporous adsorption resin column for adsorption, elute with 50-70% ethanol, and depressurize Recover ethanol and concentrate, add dichloromethane to crystallize, separate the crystals, wash and dry. By adopting the invention to prepare hydrangea phenol, the product has high purity and is easy to realize industrial scale-up.

Description

technical field [0001] The invention relates to a preparation method of hydrangenol, in particular to a preparation method of extracting hydrangenol from plants. Background technique [0002] Hydrangenol, molecular formula: C 15 h 12 o 4 , molecular weight: 256.257, CAS accession number: 480-47-7, mainly exists in various plants of Saxifragaceae. Hydrangea Hydrangea macrophylla (Thunb.) Ser. is rich in content, and its molecular formula is as follows. [0003] [0004] Modern studies have shown that hydrangen has anti-allergic, antibacterial, and choleretic effects, and it is also used as a raw material for the synthesis of other active derivatives. [0005] Saxifragaceae hydrangea Hydrangea macrophylla (Thunb.) Ser. The roots and leaves are used as traditional Chinese medicine Hydrangea, which can clear away heat, detoxify, resist malaria, and kill insects. [0006] In the prior art, there is no report on the preparation process applicable to the large-scale ind...

Claims

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Application Information

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IPC IPC(8): C07D311/76
CPCY02P20/54
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH