CN104610398A - Method for extracting oleuropein from syringa reticulata - Google Patents

Method for extracting oleuropein from syringa reticulata Download PDF

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Publication number
CN104610398A
CN104610398A CN201510055056.1A CN201510055056A CN104610398A CN 104610398 A CN104610398 A CN 104610398A CN 201510055056 A CN201510055056 A CN 201510055056A CN 104610398 A CN104610398 A CN 104610398A
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oleuropein
mandshurica
alkyl glycoside
syringa
extracting
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CN104610398B (en
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张悦
王化
周丽萍
李梦莎
朱良玉
周琳
沈光
何丹娆
魏殿文
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Institute Of Nature And Ecology Heilongjiang Academy Of Sciences
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Institute Of Nature And Ecology Heilongjiang Academy Of Sciences
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H17/00Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
    • C07H17/04Heterocyclic radicals containing only oxygen as ring hetero atoms
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • C07H1/08Separation; Purification from natural products

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Biotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Molecular Biology (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Saccharide Compounds (AREA)

Abstract

The invention discloses a method for extracting oleuropein from syringa reticulata, and belongs to a method for extracting active substance from natural products. The method disclosed by the invention comprises the following steps: adding an ethanol solution with alkyl glycoside concentration of 0.5-3% into dry syringa reticulata powder according to a mass volume ratio (g/ml) of 1: (10-25), and uniformly mixing the components, wherein the volume concentration of the ethanol solution is 0-95%; extracting the mixed solution, filtering to obtain an extracting solution, recycling the ethanol in the extracting solution, adding an equal amount of water to recover the original volume, filtering, and gathering by macroporous resin for one time, eluting via 40-60% (volume) of ethanol solution, collecting eluant, and concentrating and drying the eluant to obtain an oleuropein extract. The method disclosed by the invention is high in extraction efficiency, simple and convenient to operate, pollution-free and non-toxic, thereby having great potential for development.

Description

A kind of method extracting Oleuropein from Syringa veticulata var.mandshurica
Technical field
The invention belongs to natural product active substance and extract field, specifically a kind of method using alkyl glycoside assisted extraction Oleuropein from Syringa veticulata var.mandshurica.
Background technology
Syringa veticulata var.mandshurica ( syringa reticulata) be Oleaceae genus syringa, be distributed widely in northeast, North China, northwest and Central China.Syringa veticulata var.mandshurica has good pharmaceutical use, ornamental value and the ecological value, and complete stool can be used as medicine, there is clearing lung-heat, eliminate the phlegm, cough-relieving, anti-inflammatory, relieving asthma, the effect such as diuresis.
Oleuropein (Oleuropein) is the important active pharmaceutical ingredients of Syringa veticulata var.mandshurica, and content is relatively high, has larger research and development to be worth.Oleuropein is a kind of nontoxic Secoiridoid Glycosides compound; along with deepening continuously of Chinese scholars research; find that it has many pharmacologically actives; comprise: anti-oxidant activity, anti-inflammatory activity, anti-atherogenic activity, antitumour activity, anti-microbial activity, antiviral activity etc., it also shows the provide protection of caused by doxorubicin heart damage and reducing blood-fat, blood sugar reducing function in addition.At present, Oleuropein is used to the fields such as medicine, protective foods, makeup just gradually, has a extensive future.Based on the above-mentioned important activity of Oleuropein, seem particularly important for the extraction of Oleuropein and related products exploitation.
At present, Oleuropein is mainly from the leaf of Fructus oleae europaeae, fruit and bark, and Syringa oblata Lindl., obtains in the plants such as daphne lilac.Extracting method has solvent-extraction process, ultrasonic extraction, microwave loss mechanisms, supercritical fluid extraction, and Extraction solvent used is mainly ethanol-water system.
Summary of the invention
At present, the research report adding alkyl glycoside assisted extraction Oleuropein in Extraction solvent is not yet had.
The object of the invention is just to provide a kind of method using alkyl glycoside assisted extraction Oleuropein from Syringa veticulata var.mandshurica.
The method extracting Oleuropein in the present invention from Syringa veticulata var.mandshurica is carried out in the steps below:
Step one, to the ethanolic soln containing alkyl glycoside or containing alkyl glycoside the aqueous solution in add Syringa veticulata var.mandshurica wood powder after extract;
Step 2, then to filter, add water, refilter, with macroporous adsorbing resin for purification, ethanolic soln wash-out, collect elutriant, elutriant concentrate drying, obtains oleuropein extract.
Further restriction, the mass percent containing alkyl glycoside in the ethanolic soln of alkyl glycoside described in step one is 0.5% ~ 3.0%.The mass percent containing alkyl glycoside in the aqueous solution of alkyl glycoside described in step one is 0.5% ~ 3.0%.Step one extracting method is refluxing extraction, supersound extraction or microwave extraction.
The present invention has the following advantages: solvent for use is second alcohol and water, and recoverable is pollution-free, the alkyl glycoside toxicological harmless of interpolation, preserves the security of product, and has good environmental benefit; Extraction efficiency of the present invention is high, simple to operation, has good economic benefit and social benefit, has very large development potentiality.
Embodiment
Embodiment one: a kind of method using alkyl glycoside assisted extraction Oleuropein from Syringa veticulata var.mandshurica in present embodiment, it comprises the steps: to get dry Syringa veticulata var.mandshurica wood powder, be 1:(10 ~ 25 by quality and volume ratio (g/ml)) add the ethanolic soln that alkyl glycoside concentration is 0.5% ~ 3%, volumes of aqueous ethanol concentration is 0% ~ 95%, mixing; Mixing solutions is extracted, filters to obtain extracting solution, after extracting solution is reclaimed ethanol, the water gaging such as to add, return to original volume, after filtration through macroporous adsorbing resin for purification once, 40% ~ 60% ethanolic soln wash-out, collect elutriant, elutriant concentrate drying, obtains oleuropein extract.
Embodiment two: present embodiment with specifically implement one unlike: described volumes of aqueous ethanol concentration is 1% ~ 80%.Other step and parameter are with specifically to implement one identical.
Embodiment three: the method extracting Oleuropein in present embodiment from Syringa veticulata var.mandshurica is carried out in the steps below:
Get dry Syringa veticulata var.mandshurica branch wood powder 10.0g, adding 200mL alkyl glycoside concentration is the ethanolic soln of 0.5%, and described volumes of aqueous ethanol concentration is 60%, mixing; Mixing solutions is carried out supersound extraction, controls ultrasonic power 150W, temperature 40 DEG C, time 60min, filters to obtain extracting solution, after extracting solution is reclaimed ethanol, the water gaging such as to add, return to original volume, after filtration through macroporous adsorbent resin HPD-100B enrichment once, 60% (volume) ethanolic soln wash-out, elution flow rate 3BV/h, collects elutriant, elutriant concentrate drying, obtain Oleuropein 0.78g, purity 35.48%.
The extraction yield of present embodiment method Oleuropein is 85.23%.And adopt 60% ethanolic soln as Extraction solvent, extract under the same conditions, the extraction yield of Oleuropein is 79.65%.Present embodiment method improves the utilization ratio of Syringa veticulata var.mandshurica raw material.
Embodiment four: present embodiment and embodiment three unlike: the volumes of aqueous ethanol concentration extracted is 70%.Other step is identical with embodiment three with parameter.
Embodiment five: the method extracting Oleuropein in present embodiment from Syringa veticulata var.mandshurica is carried out in the steps below:
Get dry Syringa veticulata var.mandshurica wood powder 20.0g, adding 300mL alkyl glycoside concentration is the ethanolic soln of 1.0%, and volumes of aqueous ethanol concentration is 50%, mixing; Mixing solutions is carried out supersound extraction, controls ultrasonic power 150W, temperature 50 C, time 60min, filters to obtain extracting solution, after extracting solution is reclaimed ethanol, the water gaging such as to add, return to original volume, after filtration through macroporous adsorbent resin HPD-400A enrichment once, 40% (volume) ethanolic soln wash-out, elution flow rate 3BV/h, collects elutriant, elutriant concentrate drying, obtain oleuropein extract 1.39g, purity 33.51%.
The extraction yield of present embodiment method Oleuropein is 78.26%.And adopt 60% ethanolic soln as Extraction solvent, extract under the same conditions, the extraction yield of Oleuropein is 73.14%.
Embodiment six: present embodiment and embodiment five unlike: the volumes of aqueous ethanol concentration extracted is 80%.Other step is identical with embodiment five with parameter.

Claims (10)

1. from Syringa veticulata var.mandshurica, extract a method for Oleuropein, it is characterized in that the method extracting Oleuropein from Syringa veticulata var.mandshurica is carried out in the steps below:
Step one, to the ethanolic soln containing alkyl glycoside or containing alkyl glycoside the aqueous solution in add Syringa veticulata var.mandshurica wood powder after extract;
Step 2, then to filter, add water, refilter, with macroporous adsorbing resin for purification, ethanolic soln wash-out, collect elutriant, elutriant concentrate drying, obtains oleuropein extract.
2. a kind of method extracting Oleuropein from Syringa veticulata var.mandshurica according to claim 1, is characterized in that the volumetric concentration of ethanolic soln described in step one is 1% ~ 95%.
3. a kind of method extracting Oleuropein from Syringa veticulata var.mandshurica according to claim 1, is characterized in that the volumetric concentration of ethanolic soln described in step one is 50% ~ 80%.
4. a kind of method extracting Oleuropein from Syringa veticulata var.mandshurica according to claim 1, is characterized in that the volumetric concentration of ethanolic soln described in step one is 60% ~ 70%.
5. a kind of method extracting Oleuropein from Syringa veticulata var.mandshurica according to claim 1, to is characterized in that described in step one containing the mass percent of alkyl glycoside in the ethanolic soln of alkyl glycoside being 0.5% ~ 3.0%.
6. a kind of method extracting Oleuropein from Syringa veticulata var.mandshurica according to claim 1, to is characterized in that described in step one containing the mass percent of alkyl glycoside in the ethanolic soln of alkyl glycoside being 1.0%.
7. a kind of method extracting Oleuropein from Syringa veticulata var.mandshurica according to claim 1, to is characterized in that described in step one containing the mass percent of alkyl glycoside in the aqueous solution of alkyl glycoside being 0.5% ~ 3.0%.
8. a kind of method extracting Oleuropein from Syringa veticulata var.mandshurica according to claim 1, to is characterized in that described in step one containing the mass percent of alkyl glycoside in the aqueous solution of alkyl glycoside being 1.0%.
9. a kind of method extracting Oleuropein from Syringa veticulata var.mandshurica according to claim 1, is characterized in that step one extracting method is refluxing extraction, supersound extraction or microwave extraction.
10. a kind of method extracting Oleuropein from Syringa veticulata var.mandshurica according to claim 1, is characterized in that: in step 2, wash-out volumes of aqueous ethanol concentration is 40% ~ 60%.
CN201510055056.1A 2015-02-03 2015-02-03 Method for extracting oleuropein from syringa reticulata Expired - Fee Related CN104610398B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102228514A (en) * 2011-05-05 2011-11-02 陕西禾博天然产物有限公司 Method for extracting oleuropein from olive leaves
CN102464683A (en) * 2010-11-19 2012-05-23 苏州宝泽堂医药科技有限公司 Method for extracting oleuropein from olive leaves
CN103113433A (en) * 2013-02-27 2013-05-22 河南科技大学 Method for extracting oleuropein from syringa pubescens

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102464683A (en) * 2010-11-19 2012-05-23 苏州宝泽堂医药科技有限公司 Method for extracting oleuropein from olive leaves
CN102228514A (en) * 2011-05-05 2011-11-02 陕西禾博天然产物有限公司 Method for extracting oleuropein from olive leaves
CN103113433A (en) * 2013-02-27 2013-05-22 河南科技大学 Method for extracting oleuropein from syringa pubescens

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
乔振峰: "《兰州大学硕士学位论文》", 31 December 2011 *
徐国兴: "《吉林大学硕士学位论文》", 31 December 2005 *
韩刚: "《表面活性剂提高姜黄素提取率的研究》", 《中成药》 *

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