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Novel diaryl nonane V, VI and VII free radical inhibitors in saxifraga tangutica as well as separation and preparation process and application thereof

A technology of diaryl nonane and tangut saxifera, which is applied in the field of separation of diaryl nonane free radical inhibitors, and achieves the effects of low cost, easy operation, and easy batch material preparation

Active Publication Date: 2021-07-09
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The relevant research of this research group has applied for a national invention patent (application number: 202010041021.3), which describes the separation, preparation and application of six galloyl-based natural free radical scavengers with known structures in Saxifrage tangutica, and up to now There are no literature or patent reports involving new diarylnonane free radical inhibitors

Method used

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  • Novel diaryl nonane V, VI and VII free radical inhibitors in saxifraga tangutica as well as separation and preparation process and application thereof
  • Novel diaryl nonane V, VI and VII free radical inhibitors in saxifraga tangutica as well as separation and preparation process and application thereof
  • Novel diaryl nonane V, VI and VII free radical inhibitors in saxifraga tangutica as well as separation and preparation process and application thereof

Examples

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Effect test

Embodiment 1

[0067] A process for the separation and preparation of new diarylnonane class V, VI and VII free radical inhibitors in Saxifrage tangutica, specifically comprising the following steps:

[0068] Step 1, extraction: dry 500g of saxifrage whole herb in the shade, coarsely crush it and extract it with methanol at a material-to-liquid ratio of 1g: 5mL, extract 4 times at room temperature for 2 hours each time, filter and combine the filtrates, namely filtrate A, The filtrate A is mixed according to the amount of polyamide: the amount of saxifrage tangutica medicinal material = 1:5 and then dried under reduced pressure. The conditions for drying under reduced pressure are: vacuum degree 50mbar, temperature 40°C, to obtain saxifrage tangutatus Grass extract mixed sample 160.2g;

[0069] Step 2, coarse separation of microporous resin column: sample mixed with saxifrage extract of Tangutia tanguticae, the sample is separated by medium-pressure chromatography equipped with microporous r...

Embodiment 2

[0074] A process for the separation and preparation of new diarylnonane class V, VI and VII free radical inhibitors in Saxifrage tangutica, specifically comprising the following steps:

[0075] Step 1, extraction: dry 1000g of saxifrage whole herb in the shade, coarsely crush it and extract it according to the ratio of solid to liquid: 1g: 100mL of methanol, extract twice at room temperature, each time for 4h, filter and combine the filtrates, that is, filtrate A, The filtrate A is mixed according to the amount of polyamide: the amount of saxifrage tangutica medicinal material = 1:5 and then dried under reduced pressure, wherein the conditions for drying under reduced pressure are: vacuum degree 250mbar, temperature 60°C, to obtain saxifrage tangutatus Grass extract mixed sample 319.3g;

[0076] Step 2, coarse separation of microporous resin column: sample mixed with saxifrage extract of Tangutia tanguticae, the sample is separated by medium-pressure chromatography equipped wi...

Embodiment 3

[0081] A process for the separation and preparation of new diarylnonane class V, VI and VII free radical inhibitors in Saxifrage tangutica, specifically comprising the following steps:

[0082] Step 1, extraction: dry 1200g of saxifrage whole herb in the shade, coarsely crush it and extract it according to the ratio of solid to liquid: 1g: 50mL of methanol, extract at room temperature 3 times, each time for 3h, filter and combine the filtrates, that is, filtrate A, The filtrate A is mixed according to the amount of polyamide: the amount of saxifrage tangutica medicinal material = 1:5 and then dried under reduced pressure, wherein the conditions for drying under reduced pressure are: vacuum degree 150mbar, temperature 50°C, to obtain saxifrage tangutatus Grass extract mixed sample 363.7g;

[0083] Step 2, coarse separation of microporous resin column: sample mixed with saxifrage extract of Tangutia tanguticae, the sample is separated by medium-pressure chromatography equipped w...

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Abstract

The invention discloses novel diaryl nonane free radical inhibitors V, VI and VII in saxifraga tangutica as well as a separation and preparation process and application thereof. The specific preparation process comprises the following four steps: extraction, coarse separation with a microporous resin column, on-line free radical inhibitor component screening and high-pressure reversed-phase chromatographic column separation. The prepared diaryl nonane Saxitansin B, the prepared diaryl nonane Saxitansin C and the prepared diaryl nonane Saxitansin D can be applied to preparation of free radical inhibition drugs or health-care foods, and are specifically used as active ingredients to be prepared into various medicinal preparations or health-care foods according to any pharmaceutically or food science acceptable carrier. An extraction solvent, a microporous resin column, a solvent used for high-pressure reversed-phase chromatographic column separation and an analysis material in the preparation process can be recycled; the raw materials are wide in source, large-scale operation can be realized in the process steps of methanol room-temperature cold leaching extraction, microporous resin column coarse separation, high-pressure reversed-phase isocratic liquid chromatography preparation and the like, and the isocratic separation of high-pressure preparative chromatography can ensure that the purity of the product is greater than 95%.

Description

technical field [0001] The invention relates to the technical field of separation of new diarylnonane free radical inhibitors in saxifrage tangutica, in particular to new diarylnonane class V, VI and VII free radical inhibitors in saxifrage tangutica And its separation preparation process and application. Background technique [0002] Saxifraga tangutica Engl., also known as Ganqing saxifrage, is an annual evergreen herb of Saxifragaceae (Saxifragaceae) genus Saxifraga. Tibetan medicine name: "Songjidi", traditional Chinese medicine It is called "Dieda" in Chinese, and it is mainly distributed in Qinghai, Gansu, Tibet, Sichuan, and Bhutan and Kashmir under the coniferous forest shrubs at an altitude of 2900-4900 meters. Tangut saxifrage is a commonly used Tibetan medicine, and the whole herb can be used as medicine. "Chinese Medicine Cihai" records: its nature and taste are slightly bitter, pungent, and cold. Main effects: clearing the liver and gallbladder, invigorating t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/255C07C49/248C07C45/79C07C45/80A61P39/06A23L33/105
CPCC07C49/255C07C49/248A61P39/06A23L33/105A23V2002/00A23V2200/30A23V2250/21Y02A50/30
Inventor 党军王启兰陶燕铎
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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