Method for simultaneously separating and preparing syringin and oleuropein from syringa oblate lindl.

A technology of syringin and oleuropein, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of low oleuropein content, affecting application, etc., and achieve high product yield and production The effect of simple process and low energy consumption

Inactive Publication Date: 2015-06-10
HEILONGJIANG BAYI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of oleuropein obtained by this method is low, which affects its further application.

Method used

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  • Method for simultaneously separating and preparing syringin and oleuropein from syringa oblate lindl.
  • Method for simultaneously separating and preparing syringin and oleuropein from syringa oblate lindl.
  • Method for simultaneously separating and preparing syringin and oleuropein from syringa oblate lindl.

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] S11, preparation of extract

[0035] Take 1 kg of lilac (Syringa oblata Lindl.) sprigs, crush them, and extract them three times with 40% ethanol solution, 10 min each time, with a solid-liquid ratio of 1:10 (kg / L). The extracts are combined, filtered, and concentrated to 4 L.

[0036] S12. Macroporous resin separation

[0037] The concentrated extract was absorbed by HPD-100B macroporous resin column at a flow rate of 3BV / h, and then eluted successively with ethanol solutions with a volume concentration of 20% and 40%, and the eluent was collected in sections, and thin-layer chromatography was used to Silica gel prefabricated plate (HSGF 254 ) rapid qualitative detection.

[0038] S13. Concentrate and dry the collected eluate of 20% ethanol aqueous solution to obtain crude syringin, which is dissolved in ethyl acetate, stirred with a small amount of silica gel, and then loaded onto a silica gel column by dry method. The silica gel column was eluted with ethyl acetat...

Embodiment 2

[0041] S21, preparation of extract

[0042]Take 0.5 kg of lilac (Syringa oblata Lindl.) sprigs, crush them and extract them twice with 30% ethanol solution, 8 min each time, the ratio of solid to liquid is 1:20 (kg / L), the extracts are combined and filtered, and concentrated to 2 L .

[0043] S22. Macroporous resin separation

[0044] The concentrated extract was absorbed by HPD-400A macroporous resin column at a flow rate of 2BV / h, and then eluted successively with ethanol solutions with a volume concentration of 25% and 50%, and the eluent was collected in sections, and thin-layer chromatography was used to Silica gel prefabricated plate (HSGF 254 ) rapid qualitative detection.

[0045] S23. Concentrate and dry the collected eluate of 25% aqueous ethanol solution, stir it with ethyl acetate, and load it through the silica gel column by dry method. Elute with ethyl acetate:methanol:water volume ratio 12:1:0.2, collect the eluate, concentrate and precipitate crystals, and ...

Embodiment 3

[0048] S31, preparation of extract

[0049] Get 0.5 kg of lilac (Syringa oblata Lindl.) sprigs, pulverize them and extract them 3 times with 50% ethanol solution homogenate, each time for 6 minutes, the ratio of solid to liquid is 1:10 (kg / L), the extracts are combined and filtered, concentrated to 1.5 L.

[0050] S32. Macroporous resin separation

[0051] The concentrated extract was absorbed by D101 macroporous resin column at a flow rate of 4BV / h, and then eluted successively with ethanol solutions with a volume concentration of 20% and 50%. plate (HSGF 254 ) rapid qualitative detection.

[0052] S33. Concentrate and dry the eluate obtained from the collected 20% ethanol aqueous solution, stir with ethyl acetate, and then dry-load the sample through the silica gel column. Elute with ethyl acetate:methanol:water volume ratio 12:1:0.2, collect the eluate, concentrate and precipitate crystals, and recrystallize twice with absolute ethanol to obtain 1.52 g of syringin cryst...

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Abstract

The invention discloses a method for simultaneously separating and preparing syringin and oleuropein from syringa oblate lindl. The method comprises the following steps: extracting by taking small branches of syringa oblate lindl. as raw materials by virtue of a homogenization process, carrying out macroporous resin column adsorption, implementing gradient elution with two ethanol solutions different in concentration, respectively separating eluents through column chromatography on silica gel and recrystallizing so as to obtain syringin crystal and oleuropein crystal. The method disclosed by the invention includes processes of syringin and oleuropein extraction from syringa oblate lindl., macroporous resin and silica gel column separation, and the like, and the method has the advantages of low raw material cost, simple process, recoverable adopted solvent and resin, and the like; two products prepared by the method are higher than 95% in purity; therefore, the method is applicable to industrial production on a large scale.

Description

technical field [0001] The invention relates to the field of natural product chemistry, in particular to a method for simultaneously separating and preparing syringin and oleuropein from lilac. Background technique [0002] Both syringin and oleuropein have various pharmacological activities, so they have a wide range of medical application prospects. [0003] Syringin, also known as eleutheroside B, is one of the main medicinal components of eleuthero, and it is a strong anti-hepatotoxic drug. At present, syringin mainly comes from Acanthopanax senticosus, which is a national third-level protected plant, and its processing and utilization are strictly restricted. Studies have shown that the content of syringin in lilac is more than twice that of Acanthopanax; oleuropein is mainly isolated from olive leaves. Olives are mainly distributed in Mediterranean countries. Although my country has introduced them in recent years, the resources are very limited. Therefore, it is of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H17/04C07H1/08
CPCC07H15/203C07H1/08C07H17/04
Inventor 刘香萍韩玉静李国良曲善民罗英花杨智明杨伟光
Owner HEILONGJIANG BAYI AGRICULTURAL UNIVERSITY
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