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Method for separating two kinds of bibenzyl compounds from common camellia oleifera

A common oil separation technology, applied in the preparation of organic compounds, chemical instruments and methods, sugar derivatives, etc., can solve problems such as difficult, unsuitable for industrial applications, and difficult to separate complex samples by pressurized thin layers, to achieve The preparation process is simple and the extraction rate is improved

Active Publication Date: 2016-04-06
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is very difficult to separate complex samples by the method of pressurized thin layer, which is mainly suitable for qualitative analysis, and it is still difficult to use for preparation; while the amount of sample processed by solid phase microextraction is small, it is not suitable for industrial applications

Method used

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  • Method for separating two kinds of bibenzyl compounds from common camellia oleifera
  • Method for separating two kinds of bibenzyl compounds from common camellia oleifera
  • Method for separating two kinds of bibenzyl compounds from common camellia oleifera

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Extraction of Compound 1 from Common Camellia oleifera:

[0058] (1) Raw material preparation: Fresh oil tea leaves are collected from Tianjiling National Forest Park in Hunan Province, and identified as ordinary oil tea leaves (Camellia Oleifera Abel.) by Professor Tan Xiaofeng of Central South University of Forestry and Technology; the ordinary oil tea leaves are washed and destemmed, naturally air-dried, and crushed to obtain Sample 20kg;

[0059] (2) Extraction: Use 60L of ethanol solution with a volume fraction of 50%, extract twice at 70°C for 2 hours each time, filter to obtain the extract, and concentrate the extract under reduced pressure at 40°C and a vacuum of 0.08MPa , concentrated to a volume of 30% before concentration to obtain a concentrated solution;

[0060] (3) Separation and purification: pass the concentrated solution of 3BV obtained in step (2) through D-101 macroporous resin. 3BV of distilled water, 6BV of ethanol solution with a volume fraction...

Embodiment 2

[0091] Extraction of Compound 1 from Common Camellia oleifera:

[0092] (1) Raw material preparation: Fresh oil tea leaves are collected from Tianjiling National Forest Park in Hunan Province, and identified as ordinary oil tea leaves (Camellia Oleifera Abel.) by Professor Tan Xiaofeng of Central South University of Forestry and Technology; the ordinary oil tea leaves are washed and destemmed, naturally air-dried, and crushed to obtain Sample 20kg;

[0093] (2) Extraction: Use 40L of ethanol solution with a volume fraction of 60%, extract 3 times at 60°C for 2 hours each time, filter the extract, and concentrate the extract under reduced pressure at 50°C and a vacuum of 0.09MPa , concentrated to a volume of 35% before concentration to obtain a concentrated solution;

[0094] (3) Separation and purification: pass the concentrated solution of 3BV obtained in step (2) through D-101 macroporous resin, wherein the amount of macroporous resin is 9L, and the diameter-to-height ratio...

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Abstract

The invention discloses a method for separating two bibenzyl compounds from ordinary oil tea camellia. The method comprises the following steps: (1) raw materials preparation, namely cleaning ordinary oil tea camellia, removing impurities, airing and crushing; (2) extraction, namely heating and extracting the ordinary oil tea camellia with an ethanol solution, filtering and concentrating to obtain concentrated liquid; (3) separation and purification, namely processing the concentrated liquid with macroporous resin, sequentially eluting with distilled water and the ethanol solution, respectively collecting, and merging eluants, so as to obtain an eluant mixture; (4) silica gel separation, namely concentrating the eluant mixture, carrying out silica gel chromatography, eluting with a mixed liquid of dichloromethane, methyl alcohol and water, and respectively collecting a target distillate fractions; and (5) liquid phase preparation, namely respectively concentrating the target distillate fractions, dissolving, and carrying out semi-preparation and collection with the liquid phase. Two target product components are confirmed by identification; the yields can be up to 37mg / kg and 200mg / kg; the purity is greater than 90%; and the method disclosed by the invention is simple and convenient in preparation process, and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for separating bibenzyl compounds, in particular to a method for separating two kinds of bibenzyl compounds from common oil tea leaves. Background technique [0002] Camellia oleifera grown in my country mainly includes the following types: common camellia oleifera (Camellia oleifera Abel) accounts for about 98% of the total area, followed by Zhejiang safflower camellia in Zhejiang province, Tengchong safflower camellia in Yunnan province, Nanshan camellia in Guangdong province and Guangxi, etc. Camellia oleifera research mostly focuses on camellia oleifera fruit or its germplasm resources, and a large number of fallen leaves produced by threshing leaves in April and May every year have caused a great waste of resources. [0003] Studies have shown that the composition of Camellia oleifera is complex, containing fat, reducing sugar, protein, amino acid, acid, ash, chlorophyll, tea saponin and flavonoids and other compo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/16C07C37/70C07C37/82C07H15/203C07H1/08
CPCC07C37/70C07C37/72C07C37/82C07H1/08C07H15/203C07C39/16
Inventor 曹清明邬靖宇钟海雁
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY