CN106349136B - A method of zeaxanthin and its derivative in extraction matrimony vine - Google Patents

A method of zeaxanthin and its derivative in extraction matrimony vine Download PDF

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Publication number
CN106349136B
CN106349136B CN201610768879.3A CN201610768879A CN106349136B CN 106349136 B CN106349136 B CN 106349136B CN 201610768879 A CN201610768879 A CN 201610768879A CN 106349136 B CN106349136 B CN 106349136B
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extraction
matrimony vine
zeaxanthin
derivative
dry
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CN106349136A (en
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闫亚美
曹有龙
米佳
罗青
禄璐
李晓莺
李越鲲
冉林武
张曦燕
安巍
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Institute of Wolfberry Engineering Technology of Ningxia Academy of Agricultural and Forestry Sciences
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Institute of Wolfberry Engineering Technology of Ningxia Academy of Agricultural and Forestry Sciences
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C403/00Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
    • C07C403/24Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The present invention relates to a kind of methods of active principle in extraction matrimony vine, more particularly, to a kind of method of zeaxanthin and its derivative in extraction matrimony vine, this method is first by matrimony vine hypoglycemic, then 100 mesh are crushed to after taking 10kg to dry, it is placed in supercritical extraction reactor and is extracted, it is then combined with and collects 0.6h 3h extracts, be gained zeaxanthin and its derivative;The present invention provides a kind of overall process organic solvent-free, safe efficient, and the technical parameter is adapted to enlarged experiment production and purity is up to 80% or more.

Description

A method of zeaxanthin and its derivative in extraction matrimony vine
Technical field
The present invention relates to a kind of methods of active principle in extraction matrimony vine, more particularly, to the corn in a kind of extraction matrimony vine The method of yellow matter and its derivative.
Background technology
Zeaxanthin belongs to oxygen-containing carotenoid, molecular formula C40H58O2, it is primarily present in bottle green vegetables, yolk, jade In rice, citrus fruit etc., human body cannot be synthesized directly.Zeaxanthin is widely distributed in the tissues such as human serum, liver, Density highest in middle macula retinae, they are that light is prevented to expose the most effective ingredient for causing retinal damage.Zeaxanthin into It is protein mediated by particular combination to enter retina.Currently, age-related macular degeneration and cataract are to lead to inpairment of vision very To the several frequently seen eye disease of blindness, has the research in terms of many zeaxanthins and cataract relationship both at home and abroad.Increasingly More epidemiology and clinical test show that the zeaxanthin of high level in diet or serum can reduce eye disease illness wind Danger;Matrimony vine is traditional medicine-food two-purpose resource.Medlar health preserving historical origin for a long time, nowadays more by the height weight of experts and scholars Depending on.The outstanding medical scholar's Li Shizhen (1518-1593 A.D.) of the Ming Dynasty is written《Compendium of Materia Medica》It records:" matrimony vine, kidney-tonifying sperm-generating, nourishing the liver, improving eyesight, hard essence Bone goes fatigue, easy color to bleach, and improving eyesight is calmed the nerves, and makes us long-lived ".Modern medicine shows to be rich in main improving eyesight effect in matrimony vine Ingredient carotenoid substance, is 4-20 times of carotenoid in common fruits and vegetables, and predominantly zeaxanthin and its derivative, is had The condition of simple, functional health care product deep level development.
Zeaxanthin and its derivative belong to fat-soluble chemical substance, and extraction process is presently mainly solvent method.It is common Solvent have hexane, acetone, petroleum ether and tetrahydrofuran etc., these solvents all have different degrees of toxicity.Therefore, traditional Solvent extraction method because its solvent toxicity residual etc. factors, limit luteole extraction separation and its further deep processing It utilizes;Supercritical CO2Abstraction technique extraction natural carotenoid is that the main research of supercritical liquid extraction technique and application are led One of domain, and have become the hot spot of domestic and international research and development.But at present by matrimony vine sugared content, water content and seed oil content compared with High factor influences, and technique is rarely seen in the extraction application of matrimony vine zeaxanthin and its derivative.
Invention content
It is safe efficient the purpose of the present invention is overcoming the deficiencies of the prior art and provide a kind of overall process organic solvent-free, And the technical parameter be adapted to enlarged experiment production and purity up in a kind of 80% or more extraction matrimony vine zeaxanthin and its The method of derivative.
The present invention realizes in the following way:
A method of zeaxanthin and its derivative in extraction matrimony vine, it is characterised in that:This method is first by matrimony vine Hypoglycemic is crushed to 100 mesh after then taking 10kg to dry, is placed in supercritical extraction reactor and is extracted, and is then combined with and collects 0.6h- 3h extracts are gained zeaxanthin and its derivative;
The extraction conditions is:35-45 DEG C of extraction temperature, extracting pressure 35-45Mpa, CO2Flow 300-370L/h, Extraction time is 3 hours;
The process of the matrimony vine hypoglycemic is that the fruit of Chinese wolfberry of removal of impurities is placed in 50 DEG C of water of 6-10 times of quality, stands 1 hour, It is repeated 3 times, room temperature is dried or 40-50 DEG C of hot-air seasoning after draining, and matrimony vine raw material total sugar content is made to be reduced to from 41%-45% 25%-29%, water content are reduced to 10%-8% from 11%-12%;
The extraction quantity is 2-6kg/100kg, analyzes and detects through HPLC, gained extract is mainly two palm of luteole Acid esters, luteole monopalmitate, zeaxanthin, kryptoxanthin and beta carotene, wherein zeaxanthin dipalmitate contains Liang≤80%;
The matrimony vine is fresh fructus lycii or dry wolfberry.
The present invention has the following effects that:
1) method is unique:Method provided by the invention is that the fruit of Chinese wolfberry of removal of impurities is placed in 50 DEG C of water of 6-10 times of quality, 1 hour is stood, is repeated 3 times, room temperature is dried or 40-50 DEG C of hot-air seasoning after draining.Make matrimony vine raw material total sugar content from 41%- 45% is reduced to 25%-29%, water content to be reduced to 10%-8% from 11%-12%.Matrimony vine after taking 10kg to dry, is crushed to 100m mesh, is placed in supercritical extraction reactor and is extracted.Extraction conditions is:35-45 DEG C of extraction temperature, extracting pressure 35- 45Mpa、CO2Flow 300-370L/h, extraction time are 3 hours.Wherein, merge and collect 0.6h-3h extracts, be gained corn Yellow matter and its derivative.This method is using the fruit of Chinese wolfberry as raw material, using supercritical CO2Abstraction technique extraction is made purity and is more than 75% Matrimony vine zeaxanthin and its derivative.
2) extraction process is safe efficient:The present invention extract obtained 80% or more be zeaxanthin and its derivative, mainly For zeaxanthin dipalmitate, overall process does not use organic solvent after the pre-treatment of extraction raw material, extraction and extraction, safely, Efficiently.
3) it after method pre-treatment provided by the invention, solves enlarged experiment production extraction slag compacting and is difficult to take in extraction kettle The bottleneck problem gone out;
4) product extracted has the effects that improving eyesight, alleviates visual fatigue, prevents cardiovascular and cerebrovascular disease:Side provided by the invention Material residue after method extraction is convenient for the extraction of polysaccharides, the low small molecular sugar content of material residue to reduce 40%-50%.It is demonstrate,proved through function test It is bright, have the effects that improving eyesight, alleviates visual fatigue, prevents cardiovascular and cerebrovascular disease.Product can be directly used for healthy food material, processing Prepare various health foods and drug.
Specific implementation mode
Embodiment one:A method of zeaxanthin and its derivative in extraction matrimony vine, this method is the Chinese holly that will be cleaned Matrimony vine is placed in 50 DEG C of water of 6-10 times of quality, is stood 1 hour, is repeated 3 times, and room temperature is dried or 40 DEG C of hot-air seasonings after draining. Matrimony vine raw material total sugar content is set to be reduced to 25%-29%, water content to be reduced to 10%-8% from 11%-12% from 41%-45%, Matrimony vine after taking 10kg to dry, is crushed to 100m mesh, is placed in supercritical extraction reactor and is extracted.Extraction conditions is:Extraction temperature 35 DEG C, extracting pressure 35Mpa, CO2 flow 300L/h, extraction time are 3 hours, wherein merge and collect 0.6h-3h extractions Object is gained zeaxanthin and its derivative.Extraction quantity is 2-6kg/100kg, analyzes and detects through HPLC, and gained extract is main For zeaxanthin dipalmitate, luteole monopalmitate, zeaxanthin, kryptoxanthin and beta carotene.Wherein, corn Flavine dipalmitate Han Liang≤80%.
Embodiment two:A method of zeaxanthin and its derivative in extraction matrimony vine, this method is the Chinese holly that will be cleaned Matrimony vine is placed in 50 DEG C of water of 6-10 times of quality, is stood 1 hour, is repeated 3 times, and room temperature is dried or 50 DEG C of hot-air seasonings after draining. Matrimony vine raw material total sugar content is set to be reduced to 25%-29%, water content to be reduced to 10%-8% from 11%-12% from 41%-45%. Matrimony vine after taking 10kg to dry, is crushed to 100m mesh, is placed in supercritical extraction reactor and is extracted.Extraction conditions is:Extraction temperature 45 DEG C, extracting pressure 45Mpa, CO2 flow 370L/h, extraction time are 3 hours, wherein merge and collect 0.6h-3h extractions Object is gained zeaxanthin and its derivative.Extraction quantity is 2-6kg/100kg, analyzes and detects through HPLC, and gained extract is main For zeaxanthin dipalmitate, luteole monopalmitate, zeaxanthin, kryptoxanthin and beta carotene.Wherein, corn Flavine dipalmitate Han Liang≤80%.
Embodiment three:A method of zeaxanthin and its derivative in extraction matrimony vine, this method is the Chinese holly that will be cleaned Matrimony vine is placed in 50 DEG C of water of 6-10 times of quality, is stood 1 hour, is repeated 3 times, and room temperature is dried or 45 DEG C of hot-air seasonings after draining. Matrimony vine raw material total sugar content is set to be reduced to 25%-29%, water content to be reduced to 10%-8% from 11%-12% from 41%-45%. Matrimony vine after taking 10kg to dry, is crushed to 100m mesh, is placed in supercritical extraction reactor and is extracted.Extraction conditions is:Extraction temperature 40 DEG C, extracting pressure 40Mpa, CO2 flow 350L/h, extraction time are 3 hours, wherein merge and collect 0.6h-3h extractions Object is gained zeaxanthin and its derivative.Extraction quantity is 2-6kg/100kg, analyzes and detects through HPLC, and gained extract is main For zeaxanthin dipalmitate, luteole monopalmitate, zeaxanthin, kryptoxanthin and beta carotene.Wherein, corn Flavine dipalmitate Han Liang≤80%.
The fruit of Chinese wolfberry is fresh fructus lycii or dry wolfberry.

Claims (2)

1. a kind of method of the zeaxanthin and its derivative in extraction matrimony vine, it is characterised in that:This method is first to drop matrimony vine Sugar is crushed to 100 mesh after then taking 10kg to dry, is placed in supercritical extraction reactor and is extracted, and is then combined with and collects 0.6h-3h Extract, the extraction quantity are 2-6kg/100kg, analyze and detect through HPLC, gained extract is mainly two palm of luteole Acid esters, luteole monopalmitate, zeaxanthin, kryptoxanthin and beta carotene, wherein zeaxanthin dipalmitate contains Liang≤80%, the process of the matrimony vine hypoglycemic are that the fruit of Chinese wolfberry of removal of impurities is placed in 50 DEG C of water of 6-10 times of quality, and it is small to stand 1 When, it is repeated 3 times, room temperature is dried or 40-50 DEG C of hot-air seasoning after draining, and matrimony vine raw material total sugar content is made to be reduced from 41%-45% To 25%-29%, it is fresh fructus lycii or dry wolfberry that water content is reduced to 10%-8%, the matrimony vine from 11%-12%.
2. the method for the zeaxanthin and its derivative in a kind of extraction matrimony vine as described in claim 1, it is characterised in that:Institute Stating extraction conditions is:35-45 DEG C of extraction temperature, extracting pressure 35-45Mpa, CO2Flow 300-370L/h, extraction time 3 Hour.
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CN108047110A (en) * 2017-12-11 2018-05-18 宁夏农林科学院枸杞工程技术研究所 A kind of method that luteole acid dipalmitate is prepared using matrimony vine as raw material
CN111772091A (en) * 2020-07-29 2020-10-16 毛忠英 Method for extracting lycium barbarum pigment by using supercritical carbon dioxide and raw material pretreatment method
CN112075524A (en) * 2020-09-27 2020-12-15 宁夏农林科学院枸杞工程技术研究所 Wolfberry glycoprotein and zeaxanthin ester composite candy tablet
CN112255132B (en) * 2020-11-25 2023-07-28 宁夏农林科学院枸杞工程技术研究所 Method for measuring hardness of wolfberry fruits based on texture analyzer

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CN103130698B (en) * 2011-12-01 2016-03-16 周学义 The method of zeaxanthin is extracted from matrimony vine, Chinese wolfberry fruit dregs
CN102886153B (en) * 2012-10-24 2015-12-02 周学义 The extracting method of improving eyesight functional component in matrimony vine and the slag dregs of rice thereof
CN104230776A (en) * 2013-06-09 2014-12-24 中国科学院大连化学物理研究所 Method for preparing natural zeaxanthine by combination of enzymatic hydrolysis and supercritical extraction
CN103550402B (en) * 2013-11-21 2016-02-10 哈药集团中药二厂 A kind of preparation method of Fructus Lycii extract

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