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Method for separating and purifying (+)-isolariciresinol and (-)-lariciresinol from folium isatidis

A technology for larch resin alcohol and larch resin, which is applied in the field of medicine, can solve the problems of easy loss of target compounds, unfavorable environmental protection and health, and long process, and achieves the effects of few steps, simple operation and low reagent toxicity.

Inactive Publication Date: 2013-05-15
NORTHEAST FORESTRY UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the activity of (+)-isolaricoresinol and (-)-lariforesin obtained from plants is outstanding, there are few reports on their isolation and purification (Liu Jifeng et al., 2006; Li Bin et al., 2005; Liu Haili et al. et al., 2002), and traditional purification techniques were used in these reports, which required organic solvent extraction and normal phase silica gel column chromatography. The process was long, the target compound was easy to lose, and the toxic organic reagents such as chloroform and dichloromethane A large amount of use is not conducive to environmental protection and health

Method used

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  • Method for separating and purifying (+)-isolariciresinol and (-)-lariciresinol from folium isatidis
  • Method for separating and purifying (+)-isolariciresinol and (-)-lariciresinol from folium isatidis

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Embodiment 1

[0020] A method for rapidly and massively separating and purifying high-purity (+)-isolaricoresinol and (-)-larigoresinin from Folium chinensis is carried out according to the following process steps:

[0021] A. Enzymatic hydrolysis of homogenate crushing: add 5L water to 1kg of dried Folium Folium and carry out homogenate crushing for 5 minutes, adjust the pH of the slurry to 4.0 with hydrochloric acid, add cellulase to make the enzyme concentration 500U / mL, and then enzyme at 40°C Solution for 3h, filter, collect filtrate and filter residue.

[0022] B. Negative pressure cavitation enhanced extraction: add 17L ethanol to the above filter residue to carry out negative pressure cavitation enhanced extraction, the extraction temperature is 45°C, the extraction pressure is -0.06MPa, extract 2 times, each time 50min, combine the extract and step A The obtained filtrate was recovered under reduced pressure to remove the solvent to obtain 170 g of Daqingye extract.

[0023] C. Re...

Embodiment 2

[0027] A method for rapidly and massively separating and purifying high-purity (+)-isolaricoresinol and (-)-larigoresinin from Folium chinensis is carried out according to the following process steps:

[0028] A. Enzyme hydrolysis of homogenate crushing: add 7L water to 1kg of dry Folium baccatum and carry out homogenate crushing for 8 minutes, adjust the pH of the slurry to 5.0 with glacial acetic acid, add a compound enzyme of cellulase and pectinase to make the concentration of cellulase 350U / mL, the concentration of pectinase is 200U / mL, then enzymatically hydrolyze at 45°C for 2h, filter, and collect the filtrate and filter residue.

[0029] B. Negative pressure cavitation enhanced extraction: add 10L80% ethanol to the above filter residue to carry out negative pressure cavitation enhanced extraction, the extraction temperature is 35°C, the extraction pressure is -0.075MPa, extract 3 times, each time for 30min, combine the extract and the steps A obtained filtrate was re...

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Abstract

The invention relates to a method for separating and purifying (+)-isolariciresinol and (-)-lariciresinol from folium isatidis. The method comprises the following five steps of: (A) homogenate crushing enzymolysis: performing homogenate crushing of folium isatidis, and adding cellulase, pectinase or complex enzyme of the two for enzymolysis; (B) negative-pressure cavitation reinforced extraction: performing negative-pressure cavitation reinforced extraction of methanol, ethanol or alcohol-water mixed solution; (C) resin enrichment: loading a sample into a macroporous resin column, and performing stepwise elution and adsorption of macroporous resin column with target by use of 30-35% ethanol and 50-60% ethanol; (D) chromatographic separation: dissolving the sample with 90% methanol, performing gradient elution in a Toyopearl HW-40S gel resin column, and performing fractional collection of the fraction; and (E) crystallization: crystallizing a crude product of (+)-isolariciresinol and a crude product of (-)-lariciresinol with methanol to obtain the products of (+)-isolariciresinol and (-)-lariciresinol with purity over 95%. The method provided by the invention has the advantages of few steps, short time, little solvent consumption, high yield and relatively high economic value, and is more economical and environment-friendly and suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of medicines, in particular to a method for quickly and massively separating and purifying high-purity (+)-isolaricoresinol and (-)-laricine resin from Folium chinensis. Background technique [0002] Daqingye is a traditional Chinese medicine in my country, which is the leaf of Isatis indigotica Fort., a cruciferous plant. Bitter and cold in nature and flavor, Guixin and Stomach Meridian. It has the effects of clearing away heat and detoxification, cooling blood and eliminating spots, and is clinically used to treat infectious diseases such as various viral influenza, mumps and viral hepatitis (Zhong Weiguo et al., 2011). Pharmacological studies have shown that it has biological activities such as anti-virus, enhancing immunity, anti-endotoxin, anti-tumor, protecting liver and gallbladder, antibacterial, antipyretic, and anti-inflammatory (Zheng Xuehua, 2007). [0003] (+)-isolaricoresinol and (-)-laricine...

Claims

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Application Information

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IPC IPC(8): C07C43/23C07C41/34C07D307/12
Inventor 付玉杰祖元刚魏作富罗猛潘有智李婷婷齐晓琳
Owner NORTHEAST FORESTRY UNIVERSITY
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