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Separation and preparation method of lignan derivatives in thuja arborvitae

A technology for lignans and derivatives, applied in the field of natural medicinal chemistry, can solve the problems of complex separation methods, unsuitable for large-scale preparation, etc., and achieve the effects of high product purity, suitable for large-scale production, and low requirements for raw materials

Active Publication Date: 2022-05-17
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above two separation methods are quite complicated and not suitable for large-scale preparation

Method used

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  • Separation and preparation method of lignan derivatives in thuja arborvitae
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  • Separation and preparation method of lignan derivatives in thuja arborvitae

Examples

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Effect test

Embodiment 1

[0030] A method for separating and preparing lignan derivatives (7E)-7,8-Dehydroheliobuphthalmin from cypress arborvitae, the method specifically comprising the following steps:

[0031] Step 1, extraction: take 550g of Arborvitae branches and dry them in the shade, add n-hexane with 10 times its mass after crushing, percolate and extract 3 times at room temperature, each time for 10 h, percolate and combine the filtrates, i.e. filtrate A, filtrate A. Drying under reduced pressure, that is, 60 mL of the crude extract of Arborvitae branches, wherein the conditions for drying under reduced pressure are a vacuum degree of 100 mbar and a temperature of 40 °C;

[0032] Step 2, microporous resin enrichment: 30 mL of the crude extract of Arborvitae branches was taken, the sample was separated by a medium-pressure chromatographic column equipped with microporous resin, detected by an ultraviolet detector with a detection wavelength of 210 nm, and collected to prepare a chromatogram Th...

Embodiment 2

[0036] A method for separating and preparing lignan derivatives (7E)-7,8-Dehydroheliobuphthalmin from cypress arborvitae, the method specifically comprising the following steps:

[0037] Step 1, extraction: take 200g of Arborvitae branches, dry in the shade, add n-hexane with 10 times its mass after crushing, percolate and extract 3 times at room temperature, each time for 10 h, percolate and combine the filtrates, i.e. filtrate A, filtrate A. Drying under reduced pressure, that is, 21 mL of the crude extract of Arborvitae branches, wherein the conditions for drying under reduced pressure are a vacuum degree of 150 mbar and a temperature of 45°C;

[0038] Step 2, microporous resin enrichment: take 21mL of the crude extract of Arborvitae branches, separate the sample through a medium-pressure chromatographic column equipped with microporous resin, detect it with an ultraviolet detector with a detection wavelength of 210 nm, and collect and prepare a chromatogram The second main...

Embodiment 3

[0042] A method for separating and preparing lignan derivatives (7E)-7,8-Dehydroheliobuphthalmin from cypress arborvitae, the method specifically comprising the following steps:

[0043] Step 1, extraction: take 1000 g of Arborvitae branches and dry in the shade, add n-hexane with 10 times its mass after crushing, extract by percolation at room temperature for 3 times, each time for 12 h, percolate and combine the filtrates, i.e. filtrate A, The filtrate A was dried under reduced pressure, that is, 110 mL of the crude extract of Arborvitae twigs, wherein the conditions for drying under reduced pressure were a vacuum degree of 250 mbar and a temperature of 50°C;

[0044] Step 2, microporous resin column enrichment: take 60 mL of the crude extract of Arborvitae twigs, separate the sample through a medium-pressure chromatographic column equipped with a microporous resin, detect it with an ultraviolet detector with a detection wavelength of 210 nm, collect and prepare The second m...

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Abstract

The invention relates to the technical field of natural medicinal chemistry, in particular to a method for separating and preparing lignan derivatives from cypress arborvitae. Its preparation method includes four steps: extraction, microporous resin enrichment, reversed-phase C18 liquid chromatography separation, and reversed-phase phenyl column liquid chromatography purification and separation. The technical means adopted in the present invention can carry out large-scale production: the raw materials are widely planted, the cost is low, and it is easy to prepare materials in batches; n-hexane room temperature percolation extraction is easy to operate; the separation adopts microporous resin rough separation, and the microporous resin separation material can be installed In the medium-pressure column chromatography system, it is easy to scale up; the reverse-phase high-pressure preparative liquid chromatography used in the separation and purification is a fast isocratic method and can ensure that the product purity is greater than 98%.

Description

technical field [0001] The invention relates to the technical field of natural medicinal chemistry, in particular to a method for separating and preparing lignan derivatives from cypress arborvitae. Background technique [0002] arborvitae Platycladus orientalis (L)Franco is Bai Ke ( Cupressaceae ) Arborvitae subfamily ( Thujoideae ) Arborvitae ( Platycladus Spach ) Evergreen trees, rich in resources, are distributed in various regions of the country. Thuja arborvitae has a long history as a medicinal plant, modern research shows that its chemical composition is mainly composed of volatile oils, flavonoids and tannins. Except that Arborvitae is used as a garden ornamental plant, its leaves, fruits and seeds can be used as medicine. Modern pharmacological research shows that the leaves and branches are used as medicine, which can astringe and stop bleeding, diuretic and stomach invigorating, detoxify and disperse blood stasis. In order to speed up the evaluation of g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/60
CPCC07D317/60
Inventor 李刚吕悦李承钊方艳马成俊
Owner YANTAI UNIV
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