CN105503681A - Preparation method of high purity Chinese wolfberry zeaxanthin palmitate - Google Patents
Preparation method of high purity Chinese wolfberry zeaxanthin palmitate Download PDFInfo
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- CN105503681A CN105503681A CN201410498454.6A CN201410498454A CN105503681A CN 105503681 A CN105503681 A CN 105503681A CN 201410498454 A CN201410498454 A CN 201410498454A CN 105503681 A CN105503681 A CN 105503681A
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- zeaxanthin
- cetylate
- matrimony vine
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- high purity
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a preparation method of high purity Chinese wolfberry zeaxanthin palmitate. The method comprises the steps of: (1) crushing dried Chinese wolfberry, employing acetone to perform pressure reduced heating reflux extraction at least two times, and then conducting concentration to obtain an extract; (2) dissolving the concentrated extract with acetone, subjecting settled and separated supernatant to alumina column adsorption separation, using a mixed solvent of petroleum ether and ethanol to perform polarity gradient elution, conducting monitoring with a high performance liquid chromatograph, and collecting eluent containing Chinese wolfberry zeaxanthin palmitate; (3) concentrating the eluent to a proportion of 1.0, and performing extraction with ethyl acetate; and (4) concentrating the ethyl acetate extracted liquid to obtain an extract, placing the extract in an extraction kettle of a supercritical extraction apparatus, using supercritical CO2 as the solvent and adopting anhydrous ethanol as the entrainer, thus obtaining the zeaxanthin palmitate high purity extract. With the preparation method provided by the invention, a Chinese wolfberry extract with a zeaxanthin palmitate content of higher than 90% can be obtained, the preparation process is simple and the cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of zeaxanthin cetylate, be specifically related to a kind of preparation method of high purity matrimony vine zeaxanthin cetylate.
Background technology
Matrimony vine whole body is all precious, is famous and precious medicinal material and invigorant, can nourishes the liver to improve visual acuity and calm the nerves, make us long-lived.Matrimony vine is rich in the multiple nutritional components such as matrimony vine albumen, polysaccharide, vitamins C, phosphorus, iron, and energy qi-restoratives production of sperm, is used for being used as medicine or making tea, steep in wine, stew, if often drink, just can improves the health.The leaf of matrimony vine, flower, root are also first-class cuisines tonics.The effective constituent lycium barbarum polysaccharide (LBP) be rich in matrimony vine has obvious enhancement to hemopoietic function of bone marrow and every Immunological Markers for Cell-Mediated Immunity, the active quantities of superoxide dismutase (SOD) of body blood, liver and muscular tissue can be significantly improved, thus be conducive to the removing of active oxygen, delay senility and antifatigue; Increase the quantity of antibody forming cell, improve antibody effects.The producing region of matrimony vine mainly concentrates on the Northwest, and the matrimony vine in Ningxia is the most famous, and the Lycium barbarum. L Quality on the ground such as Gansu, Qinghai is also very high in addition.
The carotenoid that cannot synthesize containing human body in matrimony vine, wherein zeaxanthin cetylate is that zeaxanthin connects palmitinic acid and formed on two hydroxyls, also can decompose obtain zeaxanthin through saponification.In matrimony vine, zeaxanthin cetylate has been in the news content up to 0.219%, is the highest in all known plants.
Zeaxanthin is a kind of novel oil soluble natural pigment, is extensively present in green leafy vegetable, flowers, fruit, matrimony vine and Semen Maydis.Usually coexist with xenthophylls, β-carotene, kryptoxanthin etc. at occurring in nature, composition carotenoid mixture.Zeaxanthin is typical oil soluble chloroplast pigment.The primary pigments of Semen Maydis is exactly zeaxanthin, and the content in corn kernel is about 0.1-9mg/kg.Green leafy vegetables is the main dietary source of xenthophylls, but wherein zeaxanthin is less.
In human body, zeaxanthin is mainly distributed in the histoorgans such as eye, liver, pancreas, kidney, spleen, ovary, plays an important role to health.In eyes, zeaxanthin mainly concentrates on amphiblestroid macular area center.Human body and animal self cannot synthesize zeaxanthin, must be obtained by food or supplement.The dietary source of zeaxanthin mainly comprises Semen Maydis, orange pimento, orange juice, honeydew melon, mango, raspberry, blueberry, peach, wolfberry fruit, egg yolk etc.
In human body, zeaxanthin is a kind of powerful antioxidant, protects body tissue cell by the Anti-oxidation behavior such as quenching singlet oxygen, scavenging free radicals, thus protects biosystem from some because excessive oxidation reacts the potential deleterious effect produced.
Extract technology of preparing and comprise organic solvent extractionprocess, ultrasonic extraction, microwave―assisted extraction, surfactant method, Enzymatic Extraction, supercritical fluid extraction and film assist separation and extraction technology etc., and conventional separation purification method has tlc and high performance liquid chromatography.
But find through inspection information, the zeaxanthin cetylate content that the patent system of open report is standby is at present all not high, the present invention utilizes prior art, invent the preparation method of high purity matrimony vine zeaxanthin cetylate, for the further strengthened research of matrimony vine zeaxanthin, provide one and effectively prepare approach.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high purity matrimony vine zeaxanthin cetylate, it can obtain the zeaxanthin cetylate of high-content, and its preparation technology is simple, and cost is low.
In order to achieve the above object, technical solution of the present invention is: a kind of preparation method of high purity matrimony vine zeaxanthin cetylate, it comprises the steps:
(1) dried matrimony vine is pulverized, by acetone heating under reduced pressure refluxing extraction at least twice, then concentrate to obtain medicinal extract;
(2) by concentrated extract acetone solution, supernatant liquor after settlement separate carries out alumina column fractionation by adsorption, with the mixed solvent polarity gradient wash-out of sherwood oil and ethanol, high performance liquid chromatograph is monitored, and collects the elutriant containing matrimony vine zeaxanthin cetylate;
(3) elutriant being concentrated into proportion is 1.0, is extracted with ethyl acetate;
(4) acetic acid ethyl acetate extract is concentrated the medicinal extract obtained, the extraction kettle being placed in supercritical extraction instrument uses supercritical CO
2as solvent, with dehydrated alcohol as entrainment agent, obtain zeaxanthin cetylate high purity extract.
The preparation method of high purity matrimony vine zeaxanthin cetylate of the present invention, in wherein said step (1), matrimony vine is pulverized is 60 ~ 80 order powder.
The preparation method of high purity matrimony vine zeaxanthin cetylate of the present invention, each extraction time 60-90min in wherein said step (1), described acetone consumption is at least 4 ~ 8 times of raw material, during extraction, vacuum tightness 0.07 ~ 0.01MPa, temperature 50 ~ 80 DEG C.
The preparation method of high purity matrimony vine zeaxanthin cetylate of the present invention, the concentrated condition in wherein said step (1): vacuum ranges 0.07 ~ 0.01MPa, temperature is not higher than 75 DEG C, and being concentrated into proportion is 1.0.
The preparation method of high purity matrimony vine zeaxanthin cetylate of the present invention, the mixed solvent polarity gradient wash-out of wherein said step (2) PetroChina Company Limited.'s ether and ethanol, co-elute four times, the volume ratio of sherwood oil and ethanol is 1: 1 for the first time, second time is 2: 1, third time is the 3: 1, four time is 4: 1.
The preparation method of high purity matrimony vine zeaxanthin cetylate of the present invention, in wherein said step (3), the volume ratio of ethyl acetate and concentrated solution is 1.5-3: 1, and extraction is for 1-4 time.
The preparation method of high purity matrimony vine zeaxanthin cetylate of the present invention, in wherein said step (4), the extracting pressure of supercritical extraction instrument controls at 30 ~ 60MPa, and temperature controls at 30 ~ 50 DEG C, CO
2flow control is at 10 ~ 20L/h, and extraction time controls at 80 ~ 100min.
The preparation method of high purity matrimony vine zeaxanthin cetylate of the present invention, wherein said step (1), (2), (3), (4) are all carried out in high pure nitrogen protection.
After adopting such scheme, the preparation method of high purity matrimony vine zeaxanthin cetylate of the present invention, can obtain zeaxanthin cetylate content higher than 90% wolfberry fruit extract, it is the further strengthened research of matrimony vine zeaxanthin, provide one and effectively prepare approach, its preparation technology is simple, and cost is low.
Embodiment
The preparation method of high purity matrimony vine zeaxanthin cetylate of the present invention is illustrated below in conjunction with embodiment.
Embodiment 1
Preparation method's embodiment of high purity matrimony vine zeaxanthin cetylate of the present invention, it comprises the steps:
(1) get dry matrimony vine raw material 200g, drop into after being crushed to 60 orders in extractor; Add acetone 800ml, be decompressed to vacuum tightness 0.05MPa, be heated to 75 DEG C, refluxing extraction twice, each 60min, merge extracted twice liquid and concentrate to obtain medicinal extract, concentrated proportion is 1.0;
(2) by concentrated extract acetone solution, supernatant liquor after settlement separate carries out alumina column fractionation by adsorption, with the mixed solvent polarity gradient wash-out of sherwood oil and ethanol, co-elute four times, the volume ratio of sherwood oil and ethanol is 1: 1 for the first time, second time is 2: 1, and third time is the 3: 1, four time is 4: 1; High performance liquid chromatograph is monitored, and collects the elutriant containing matrimony vine zeaxanthin cetylate;
(3) elutriant being concentrated into proportion is 1.0, is extracted with ethyl acetate; The volume ratio of ethyl acetate and concentrated solution is 2.5: 1, extracts 2 times;
(4) acetic acid ethyl acetate extract is concentrated the medicinal extract obtained, the extraction kettle being placed in supercritical extraction instrument uses supercritical CO
2as solvent, with dehydrated alcohol as entrainment agent, obtain zeaxanthin cetylate high purity extract, step (1), (2), (3), (4) are all carried out in high pure nitrogen protection.Extracting pressure controls at 35MPa, and temperature controls at 40 DEG C, CO
2flow control is at 10L/h, and extraction time controls at 100min.Vacuum-drying, obtains zeaxanthin cetylate extract 0.32g.
After testing, Waters high performance liquid chromatograph, chromatographic column C18 (4.6mm × 250mm, 5um), moving phase is acetonitrile: methyl alcohol: triethylamine=80: 20: 0.05; Determined wavelength is 450nm, and flow velocity is 1ml/min; Sample size 60uL.Zeaxanthin cetylate content is 92.2%.
Embodiment 2
Preparation method's embodiment of high purity matrimony vine zeaxanthin cetylate of the present invention, it comprises the steps:
(1) get dry matrimony vine raw material 100kg, drop into after being crushed to 60 orders in extractor; Add acetone 500L, be decompressed to vacuum tightness 0.05MPa, be heated to 75 DEG C, refluxing extraction twice, each 60min, merge extracted twice liquid and concentrate to obtain medicinal extract, concentrated proportion is 1.0;
(2) by concentrated extract acetone solution, supernatant liquor after settlement separate carries out alumina column fractionation by adsorption, with the mixed solvent polarity gradient wash-out of sherwood oil and ethanol, collect elutriant, co-elute four times, the volume ratio of sherwood oil and ethanol is 1: 1 for the first time, and second time is 2: 1, third time is the 3: 1, four time is 4: 1; High performance liquid chromatograph is monitored, and collects the elutriant containing matrimony vine zeaxanthin cetylate;
(3) elutriant being concentrated into proportion is 1.0, is extracted with ethyl acetate; The volume ratio of ethyl acetate and concentrated solution is 2.5: 1, extracts 2 times;
(4) acetic acid ethyl acetate extract is concentrated the medicinal extract obtained, the extraction kettle being placed in supercritical extraction instrument uses supercritical CO
2as solvent, with dehydrated alcohol as entrainment agent, obtain zeaxanthin cetylate high purity extract, step (1), (2), (3), (4) are all carried out in high pure nitrogen protection.Extracting pressure controls at 35MPa, and temperature controls at 40 DEG C, CO
2flow control is at 10L/h, and extraction time controls at 100min.Vacuum-drying, obtains zeaxanthin cetylate 132g.
After testing, zeaxanthin cetylate content is 93.6%.
The above embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that the common engineering technical personnel in this area make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (8)
1. a preparation method for high purity matrimony vine zeaxanthin cetylate, is characterized in that: comprise the steps:
(1) dried matrimony vine is pulverized, by acetone heating under reduced pressure refluxing extraction at least twice, then concentrate to obtain medicinal extract;
(2) by concentrated extract acetone solution, supernatant liquor after settlement separate carries out alumina column fractionation by adsorption, with the mixed solvent polarity gradient wash-out of sherwood oil and ethanol, high performance liquid chromatograph is monitored, and collects the elutriant containing matrimony vine zeaxanthin cetylate;
(3) elutriant being concentrated into proportion is 1.0, is extracted with ethyl acetate;
(4) acetic acid ethyl acetate extract is concentrated the medicinal extract obtained, the extraction kettle being placed in supercritical extraction instrument uses supercritical CO
2as solvent, with dehydrated alcohol as entrainment agent, obtain zeaxanthin cetylate high purity extract.
2. the preparation method of high purity matrimony vine zeaxanthin cetylate as claimed in claim 1, is characterized in that: in described step (1), matrimony vine is pulverized is 60 ~ 80 order powder.
3. the preparation method of high purity matrimony vine zeaxanthin cetylate as claimed in claim 1, it is characterized in that: each extraction time 60-90min in described step (1), described acetone consumption is at least 4 ~ 8 times of raw material, during extraction, vacuum tightness 0.07 ~ 0.01MPa, temperature 50 ~ 80 DEG C.
4. the preparation method of high purity matrimony vine zeaxanthin cetylate as claimed in claim 1, it is characterized in that: the concentrated condition in described step (1): vacuum ranges 0.07 ~ 0.01MPa, temperature is not higher than 75 DEG C, and being concentrated into proportion is 1.0.
5. the preparation method of high purity matrimony vine zeaxanthin cetylate as claimed in claim 1, it is characterized in that: the mixed solvent polarity gradient wash-out of described step (2) PetroChina Company Limited.'s ether and ethanol, co-elute four times, the volume ratio of sherwood oil and ethanol is 1: 1 for the first time, second time is 2: 1, third time is the 3: 1, four time is 4: 1.
6. the preparation method of high purity matrimony vine zeaxanthin cetylate as claimed in claim 1, it is characterized in that: in described step (3), the volume ratio of ethyl acetate and concentrated solution is 1.5-3: 1, and extraction is for 1-4 time.
7. the preparation method of high purity matrimony vine zeaxanthin cetylate as claimed in claim 1, is characterized in that: in described step (4), the extracting pressure of supercritical extraction instrument controls at 30 ~ 60MPa, and temperature controls at 30 ~ 50 DEG C, CO
2flow control is at 10 ~ 20L/h, and extraction time controls at 80 ~ 100min.
8. the preparation method of high purity matrimony vine zeaxanthin cetylate as claimed in claim 1, is characterized in that: described step (1), (2), (3), (4) are all carried out in high pure nitrogen protection.
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Cited By (4)
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| CN107868028A (en) * | 2017-11-05 | 2018-04-03 | 周学义 | A kind of method that zeaxanthin acid dipalmitate is extracted in the raw material from liquid medlar |
| CN110628236A (en) * | 2018-06-22 | 2019-12-31 | 宁夏宝丰生态牧场有限公司 | Extraction method of lycium chinense berrubin |
| CN110835315A (en) * | 2019-10-28 | 2020-02-25 | 百瑞源枸杞股份有限公司 | Preparation method of lycium ruthenicum red pigment |
| CN114354784A (en) * | 2021-12-21 | 2022-04-15 | 江苏汉邦科技有限公司 | Method for separating zeaxanthin and canthaxanthin from carotenoid by supercritical fluid chromatography |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107868028A (en) * | 2017-11-05 | 2018-04-03 | 周学义 | A kind of method that zeaxanthin acid dipalmitate is extracted in the raw material from liquid medlar |
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| CN110835315A (en) * | 2019-10-28 | 2020-02-25 | 百瑞源枸杞股份有限公司 | Preparation method of lycium ruthenicum red pigment |
| CN114354784A (en) * | 2021-12-21 | 2022-04-15 | 江苏汉邦科技有限公司 | Method for separating zeaxanthin and canthaxanthin from carotenoid by supercritical fluid chromatography |
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Application publication date: 20160420 |