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Method for extracting fucosterol from bladder-wrack

A fucosterol and Fucus algae technology is applied in the production of steroids, bulk chemicals, organic chemistry, etc. to achieve the effect of being beneficial to large-scale production operations, low energy consumption, and low pollution

Inactive Publication Date: 2012-03-14
SUZHOU PAITENG BIOLOGICAL 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 preparation process applicable to the industrialized large-scale production of high-purity fucosterol

Method used

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  • Method for extracting fucosterol from bladder-wrack

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Get Fucus 10Kg, pulverize, add to CO 2 In a supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 1%, the extraction pressure is 20MPa, the temperature is 40°C, CO 2 The flow rate is 1ml / g crude drug·min, the extraction time is 140min, and the extract is obtained, which is subjected to 6-stage countercurrent extraction with water-saturated n-butanol, collects the n-butanol layer, recovers the solvent under reduced pressure, and adds it to an AB8 macroporous adsorption resin column to obtain 50% elution, collect 3 times the column volume eluate, recover ethanol under reduced pressure and concentrate, add methanol to crystallize, separate the crystals, wash and dry to obtain fucosterol 9.6g, the purity is 96.6% by HPLC detection , UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 2

[0023] Get Fucus 10Kg, pulverize, add to CO 2 In the supercritical extractor, ethanol is used as an entrainer, the entrainer accounts for 3% by volume of the total extraction solvent, the extraction pressure is 30MPa, the temperature is 55°C, CO 2 The flow rate is 3ml / g crude drug·min, the extraction time is 140min, and the extract is obtained, which is subjected to 6-stage countercurrent extraction with water-saturated n-butanol. 50% elution, collect the eluate with 8 times the volume of the column, recover ethanol under reduced pressure and concentrate, add methanol to crystallize, separate the crystals, wash and dry to obtain 12.7g of fucosterol, which is detected by HPLC with a purity of 95.4% , UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 3

[0025] Get Fucus 10Kg, pulverize, add to CO 2 In the supercritical extractor, ethanol is used as an entrainer, the entrainer accounts for 2% by volume of the total extraction solvent, the extraction pressure is 25MPa, the temperature is 50°C, CO 2 The flow rate is 2ml / g crude drug·min, the extraction time is 140min, and the extract is obtained, which is subjected to 6-stage countercurrent extraction with water-saturated n-butanol, collects the n-butanol layer, recovers the solvent under reduced pressure, and adds it to an AB8 macroporous adsorption resin column to 50% elution, collect the eluate with 5 times the volume of the column, recover ethanol under reduced pressure and concentrate, add methanol to crystallize, separate the crystals, wash and dry to obtain 11.5g of fucosterol, which is detected by HPLC with a purity of 97.8% , 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 method for extracting fucosterol from bladder-wrack, which is simple and convenient to operate and has small pollution and low energy consumption. The method comprises the following steps of: smashing bladder-wrack; adding into a CO2 supercritical extractor to obtain an extract by taking ethanol as an entrainer; performing level 6 countercurrent extraction by using water-saturated n-butyl alcohol; collecting a n-butyl alcohol layer; recovering a solvent under reduced pressure; adding onto an AB8 macroporous absorption resin column; eluting at 50 percent; collecting an eluent; recovering ethanol under reduced pressure and concentrating; adding methanol for crystallizing; separating a crystal; and washing and drying to obtain the fucosterol. By adopting the method for preparing fucosterol, the product purity is high, and industrial amplification is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of fucosterol, in particular to a preparation method of extracting fucosterol from plants. Background technique [0002] Fucosterol (Fucosterol), molecular formula: C 29 h 48 O, molecular weight: 412.698, CAS accession number: 17605-67-3, exists in a variety of plants of Lauraceae, among which Fucus, a plant of Fucus family Fucus vesiculosus L. is rich in content. Its molecular formula is as follows. [0003] [0004] Modern studies have shown that fucosterol has strong cardiovascular and cerebrovascular activity, and it is also used as a raw material for the synthesis of other active derivatives. [0005] In the prior art, there is no report on the preparation process applicable to the large-scale industrial production of high-purity fucosterol. Contents of the invention [0006] The technical problem to be solved by the present invention is to provide a method for preparing fucosterol which is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
CPCY02P20/54
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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