Method for extracting and separating labdane diterpenes from Himalayan mayapple fruit and application thereof

A technology for compounds and diterpenoids, applied in the separation/purification of hydroxy compounds, separation/purification of carbonyl compounds, organic chemical methods, etc., can solve the problems such as the purity of the diterpenoids that have not been seen yet, Achieve significant economic and social benefits, easy to operate

Inactive Publication Date: 2016-06-15
HENAN UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But have not seen the open report that adopts quantitative proton nuclear magnetic resonance spectrometry to measure the purity of the helicanoid diterpenoid compound with 7 (8) double bond so far

Method used

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  • Method for extracting and separating labdane diterpenes from Himalayan mayapple fruit and application thereof
  • Method for extracting and separating labdane diterpenes from Himalayan mayapple fruit and application thereof
  • Method for extracting and separating labdane diterpenes from Himalayan mayapple fruit and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0015] In the specific implementation of the present invention, 9 kg of lotus lobata is heated and refluxed for 3 times with ethanol with 3 times the weight of lotus lobes and a volume concentration of 95%, and 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 ratio Carry out gradient elution for 100:0, 100:5, 100:7, 100:10, 100:30 petroleum ether-acetone mixed solvents, each gradient uses 15L eluent, and the flow rate is 15mLmin -1 , each 300ml volume is a fraction, collect 215 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-ethanol solution with a volume ratio of 10:90 as Chromogenic agent, heated at 105°C for 5mi...

Embodiment 2

[0017] In the specific implementation of the present invention, 6 kg of lotus lobes can also be heated and refluxed for 3 times with ethanol with 5 times the weight of lotus lobes and a volume concentration of 75%, the extraction temperature is 92°C, the extraction time is 1.8 hours, and the ethanol is recovered under reduced pressure to obtain For extract-like ethanol extract, suspend the ethanol extract in 2L of distilled water, extract with petroleum ether and dichloromethane three times, 2L each time; put the dichloromethane extraction part on a silica gel column, and use 100:0, 100:5, 100:7, 100:10, 100:30 petroleum ether-acetone mixed solvents for gradient elution, each gradient uses 10L eluent, the flow rate is 10mLmin -1 , every 200ml volume is a fraction, collect 215 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-ethanol solution with a volume ratio of 10:90 as a Chrom...

Embodiment 3

[0019] In the specific implementation of the present invention, 7 kg of lotus lobes can also be heated and refluxed for 3 times with ethanol with 4 times the weight of lotus lobes and 80% volume concentration, the extraction temperature is 93° C., the extraction time is 2 hours, and the ethanol is recovered under reduced pressure to obtain For extract-like ethanol extract, suspend the ethanol extract in 2.5L of distilled water, extract with petroleum ether and dichloromethane three times, 2.5L each time; put the dichloromethane extraction part on a silica gel column, and use volume Gradient elution was carried out with petroleum ether-acetone mixed solvents with ratios of 100:0, 100:5, 100:7, 100:10, and 100:30. Each gradient used 13L eluent with a flow rate of 13mLmin. -1 , every 260ml volume is a fraction, collect 215 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-ethanol solu...

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Abstract

The invention relates to a method for extracting and separating labdane diterpenes from Himalayan mayapple fruit and application thereof. The method effectively solves problems of extraction of labdane diterpenes from Himalayan mayapple fruit, purity determination and application of the labdane diterpenes in preparing drugs for resisting mammary cancer and liver cancer. The method comprises the following steps: extracting Himalayan mayapple fruit with ethanol, suspending the ethanol extract in distilled water, extracting sequentially with petroleum ether and dichloromethane, passing the dichloromethane extraction part through a silica gel column, eluting with petroleum ether-acetone, collecting 215 fractions, and merging the 1st-50th fractions, 51st-134th fractions, 135th-178th fractions and 179th-215th fractions to obtain components Fr.1-Fr.4; passing the component Fr.4 through a Sephadex LH-20 column, eluting with methanol, collecting 22 fractions, and merging the 1st-4th fractions and 5th-22nd fractions to obtain sub-components Fr.4-1 and Fr.4-2; and carrying out open ODS (octadecylsilyl) column chromatography on the sub-component Fr.4-2, eluting with methanol-water, collecting 45 fractions, carrying out detection and analysis by silica gel thin-layer chromatography, and respectively merging the fractions containing labda-7, 13-diene-3, 15-diol (I) and 14,15-dinor-3beta-hydroxy-7-labden-13-one (II). The method is stable and reliable, is easy to operate, and can be effectively used for preparing drugs for resisting mammary cancer and liver cancer.

Description

technical field [0001] The invention relates to medicine, in particular to a method for extracting and separating helianthene-type diterpenoids from lotus lobata and its application. 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 clinical practice gene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/242C07C45/78C07C35/36C07C29/76A61P35/00
CPCC07B2200/07C07C29/76C07C45/78C07C35/36C07C49/242
Inventor 孙彦君张艳丽沈继朵王俊敏纪宝玉陈辉郝志友高美玲付露
Owner HENAN UNIV OF CHINESE MEDICINE
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