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A helianthene-type diterpenoid compound extracted and isolated from Lily chinensis and its preparation method and application

A technology of diterpenoids and compounds, which is applied in the field of helicanoid diterpenoids and their preparation, can solve problems such as no patents or literature reports, and achieve significant economic and social benefits and easy operation

Inactive Publication Date: 2017-07-07
HENAN UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Novel heuranane-type diterpenoids involved in the present invention and their biological activity have not been patented or reported in the literature so far

Method used

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  • A helianthene-type diterpenoid compound extracted and isolated from Lily chinensis and its preparation method and application
  • A helianthene-type diterpenoid compound extracted and isolated from Lily chinensis and its preparation method and application
  • A helianthene-type diterpenoid compound extracted and isolated from Lily chinensis and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0013] In the specific implementation of the present invention, add 9 kg of lotus lobes to 3 times the weight of lotus lobes, and extract 3 times under reflux with ethanol with a volume concentration of 95%. The extraction temperature is 95° C., and the extraction time is 1.5 hours. Paste ethanol extract, suspend the ethanol extract in 3.2L distilled water, extract 3 times with petroleum ether and dichloromethane successively, 3.2L each time; put the dichloromethane extraction part on a silica gel column, and use volume 100:0, 100:5, 100:7, 100:10 petroleum ether-acetone mixed solvents were used for gradient elution, each gradient used 15L eluent, and the flow rate was 15mLmin -1 , each volume of 300ml is a fraction, and 168 fractions are collected. Each fraction uses a GF254 thin-layer plate, with petroleum ether-acetone at a volume ratio of 1:1 as a developer, and a sulfuric acid-ethanol solution at a volume ratio of 10:90 as a developer. Chromogenic reagent, heated at 105°C...

Embodiment 2

[0015] In the specific implementation of the present invention, it is also possible to add 6 kg of lotus lobularis to 5 times the weight of lotus lobes and extract 3 times under reflux with ethanol with a volume concentration of 75%, the extraction temperature is 92 ° C, the extraction time is 1.5 hours, and the ethanol is recovered under reduced pressure , to obtain extract-like ethanol extract, suspend the ethanol extract in 2L of distilled water, extract 3 times with petroleum ether and dichloromethane successively, 2L each time; put the dichloromethane extraction part on a silica gel column, and use Petroleum ether-acetone mixed solvent with a volume ratio of 100:0, 100:5, 100:7, and 100:10 was used for gradient elution, and 10L of eluent was used for each gradient, and the flow rate was 10mLmin -1 , every 200ml volume is a fraction, collect 168 fractions, each fraction uses GF254 thin-layer plate, with the petroleum ether-acetone of volume ratio 1:1 as developer, the sulfu...

Embodiment 3

[0017] In the specific implementation of the present invention, 7 kg of lotus lobata can also be added to 4 times the weight of lotus lobes, and the volume concentration is 80% ethanol heating and reflux extraction for 3 times, the extraction temperature is 93 ° C, the extraction time is 1.8 hours, and the ethanol is recovered under reduced pressure. To obtain extract-like ethanol extract, suspend the ethanol extract in 2.5L of distilled water, extract 3 times with petroleum ether and dichloromethane successively, 2.5L each time; put the dichloromethane extraction part on a silica gel column, successively Use petroleum ether-acetone mixed solvents with volume ratios of 100:0, 100:5, 100:7, and 100:10 for gradient elution, each gradient uses 13L eluent, and the flow rate is 13mLmin -1 , every 260ml volume is a fraction, collect 168 fractions, each fraction uses a GF254 thin-layer plate, uses petroleum ether-acetone with a volume ratio of 1:1 as a developer, and a sulfuric acid-e...

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Abstract

The invention relates to a labdane-type diterpene compound extracted and separated from fructus podophylli and a preparation method and application of the labdane-type diterpene compound. The problems of the labdane-type diterpene compound extracted and separated from the fructus podophylli and the application in preparation of anti-liver cancer and anti-breast cancer medicines can be effectively solved. The method comprises the following steps: carrying out heating reflux extraction on the fructus podophylli with ethanol, suspending an ethanol extract in distilled water, and carrying out extraction with petroleum ether and dichloromethane in sequence; adding a dichloromethane extraction part to a silica gel column, eluting with petroleum ether-acetone, collecting 168 fractions, and merging the fractions 1-50, 51-134 and 135-168 to obtain components Fr.1 to Fr.3; processing the component Fr.3 through an ODS column chromatography, and carrying out gradient elution with methanol-water to obtain sub-components Fr.3-1, Fr.3-2 and Fr.3-3; adding the sub-component Fr.3-3 to the silica gel column, eluting with the petroleum ether-acetone, and collecting 38 fractions; and carrying out silica gel thin-layer chromatography detection and respectively merging the fractions containing target products, namely sinopodophyllum hexandrum terpene A and sinopodophyllum hexandrum terpene B. The method is stable, reliable and easy to operate, and has anti-breast cancer and anti-liver cancer activity.

Description

technical field [0001] The invention relates to medicine, in particular to a helianthene-type diterpenoid compound extracted and separated from Lily basilica, a preparation method and application thereof. Background technique [0002] Malignant tumors have become one of the major diseases that seriously affect human health and threaten human life. It has the characteristics of long course of treatment and difficult to cure. A research report at the 18th World Health Organization International Anti-Cancer Union Congress indicated that the number of newly diagnosed patients will increase from the current 10 million per year to 15 million in the next 20 years, and the number of deaths due to cancer will also increase from 6 million per year. increased to 10 million. The global cancer situation will become increasingly serious, and the mortality rate of malignant tumors in my country ranks first among all disease mortality rates. Synthetic antineoplastic drugs widely used in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/38C07C69/675C07C67/56C07C67/48A61P35/00
CPCC07C67/48C07C67/56C07C69/38C07C69/675
Inventor 孙彦君万焱王俊敏沈继朵裴莉昕陈辉郝志友高美玲付露
Owner HENAN UNIV OF CHINESE MEDICINE