CN105130867A - Method for extracting and enriching zeaxanthin from barbary wolfberry fruit - Google Patents
Method for extracting and enriching zeaxanthin from barbary wolfberry fruit Download PDFInfo
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- CN105130867A CN105130867A CN201510647650.XA CN201510647650A CN105130867A CN 105130867 A CN105130867 A CN 105130867A CN 201510647650 A CN201510647650 A CN 201510647650A CN 105130867 A CN105130867 A CN 105130867A
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Abstract
The invention discloses a method for extracting and enriching zeaxanthin from barbary wolfberry fruit. The method comprises the steps that 1, dried barbary wolfberry fruit and an extracting agent are put into an extraction kettle of a subcritical fluid extraction device on the basis that the massic volume ratio is 1:1-1:20 for continuous extraction for 1-20 times, and extraction is performed for 10-150 min every time to obtain an extract; 2, a decompression temperature raising method is utilized for separating the extract at the separation pressure of 0.10-1.95 MPa and the separation temperature of 10-90 DEG C to obtain an extract solution; 3, the extract solution is placed at the room temperature for standing for 10-90 min, then, ethyl acetate is added for extraction, and an organic phase is recycled and concentrated to obtain an extractum; 4, the extractum is diluted, a macroporous resin column is selected, ethyl alcohol is used for elution, the ethyl alcohol is recycled from an obtained eluate, and then the ethyl alcohol is used for crystallization to obtain zeaxanthin. The extraction yield is high, the preparation technology is simple, and the cost is low.
Description
Technical field
The invention belongs to matrimony vine active component extraction separation technical field, be specifically related to the method for zeaxanthin in a kind of Extraction and enrichment wolfberry fruit.
Background technology
Zeaxanthin (Zeaxanthin, 3,3 '-dihydroxyl-β-carotene), also known as zeaxanthin, molecular weight is 566.88, belongs to isoprenoid, is a kind of oxygen containing carotenoid, belongs to isomers with xenthophylls (Luein).The zeaxanthin that major part is present in occurring in nature is all trans isomer.
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.
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.
In human body chronic disease is prevented and treated, zeaxanthin has the unique function of vision protection, anti-cardiovascular disorder and cancer and strengthening immunity aspect.Zeaxanthin is a kind of powerful antioxidant, also 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.
The extraction technology of preparing of zeaxanthin comprises organic solvent extractionprocess, ultrasonic extraction, microwave―assisted extraction, surfactant method, Enzymatic Extraction, supercritical fluid extraction and film and assists separation and extraction technology etc.Organic solvent extraction can consume a large amount of organic solvent, ultrasonic wave, microwave and surfactant method can only as solvent extraction process supplement, enzyme process and film assist separation and Extraction to improve extraction efficiency, but also must and solvent-extraction process with the use of, supercritical liquid extraction technique is higher for the requirement of equipment, large-scale industrial production can't be formed, and output capacity is lower.
Therefore invention can be applicable to the development of matrimony vine process deeply industry, is particularly applicable to the Extraction and separation of zeaxanthin in wolfberry fruit.
Summary of the invention
The object of the present invention is to provide the method for zeaxanthin in a kind of Extraction and enrichment wolfberry fruit, it extracts, and income rate is high, preparation technology simple, and cost is low.
In order to achieve the above object, the invention provides the method for zeaxanthin in a kind of Extraction and enrichment wolfberry fruit, comprising following steps:
(1) by dried wolfberry and extraction agent by expecting that molten mass volume ratio is put in the extraction kettle of subcritical fluid extraction device continuous extraction 1 ~ 20 time at 1: 1 ~ 1: 20, each 10 ~ 150min, is extracted thing;
(2) utilize decompression temperature-raising method make the extract in step (1) separating pressure be 0.10 ~ 1.95MPa, separation temperature is separated under being the condition of 10 ~ 90 DEG C, is extracted liquid;
(3) by after extraction liquid left at room temperature 10 ~ 90min, add extraction into ethyl acetate, after reclaiming organic phase, be concentrated into medicinal extract;
(4) diluted by medicinal extract, upper selectivity macroporous adsorptive resins, with ethanol elution, gained elutriant obtains zeaxanthin with alcohol crystal after reclaiming ethanol.
The method of zeaxanthin in a kind of Extraction and enrichment wolfberry fruit of the present invention, in wherein said step (1), extraction agent is any one in propane, butane, Trimethylmethane, dme, liquefied petroleum gas (LPG), HFA 134a.
The method of zeaxanthin in a kind of Extraction and enrichment wolfberry fruit of the present invention, in wherein said step (1), extraction conditions is extraction temperature 5 ~ 85 DEG C, extracting pressure 0.15 ~ 2.95MPa, extraction agent flow 10 ~ 200L/h.
The method of zeaxanthin in a kind of Extraction and enrichment wolfberry fruit of the present invention, the volume of the ethyl acetate added in wherein said step (3) and the volume ratio of extraction liquid are 1: 1, and the number of times of extraction is 2 times.
The method of zeaxanthin in a kind of Extraction and enrichment wolfberry fruit of the present invention, the selectivity macroreticular resin in wherein said step (4) is ADS-15 or ADS-17 or ADS-F8.
The method of zeaxanthin in a kind of Extraction and enrichment wolfberry fruit of the present invention, in wherein said step (4), the volumetric concentration of wash-out ethanol is 50-70%, and the volumetric concentration of crystallization ethanol is 50-80%.
The method of zeaxanthin in a kind of Extraction and enrichment wolfberry fruit of the present invention, medicinal extract 50-200 doubly upper prop after the water dilution of its weight in wherein said step (4), the volumetric usage of described eluent ethanol is 30-60 times of medicinal extract weight.
After adopting such scheme, subcritical abstraction technology is applied to the extraction of zeaxanthin in wolfberry fruit by this research first, substantially increases the extraction efficiency of zeaxanthin in wolfberry fruit, and reduces cost.
Macroporous adsorbent resin technology, due to features such as cost are low, efficiency is high, solvent consumption is few, can reuse, is used widely at Chinese herbal medicine extracting separation field.But be separated for zeaxanthin in wolfberry fruit at present and have not been reported, macroporous resin adsorption isolation technique is applied to the separation of zeaxanthin in wolfberry fruit, provides important technical support by the development for matrimony vine deep processed product.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further, but these embodiments are only limitted to illustrate that the present invention and being not used in limits the scope of the invention.
Embodiment 1
The embodiment of the method for zeaxanthin in a kind of Extraction and enrichment wolfberry fruit of the present invention, it comprises the steps:
(1) by 200 of drying grams of matrimony vines and extraction agent-propane by 1: 1 the molten mass volume ratio of material (matrimony vine quality: extraction agent volume ratio) (g/mL) put into subcritical fluid extraction device (this subcritical abstraction device be the extraction and fractionation device of existing market sale, the subcritical abstraction instrument of subcritical Bioisystech Co., Ltd of such as Henan Province production and selling) extraction kettle in, extraction temperature be 5 DEG C, extracting pressure is 0.15MPa, extraction agent flow be the condition of 10L/h under continuous extraction 2 times, each 10min, is extracted thing;
(2) utilize decompression temperature-raising method make extract separating pressure be 0.10MPa, separation temperature is separated under being the condition of 10 DEG C, is extracted liquid; Wherein subcritical fluid extraction agent becomes gaseous state from liquid state and is recycled;
(3) after extraction liquid left at room temperature 72min, add the extraction into ethyl acetate 2 times of 1 times of volume extraction liquid, merge the organic phase that extracting and separating goes out, concentratedly after reclaiming organic phase obtain medicinal extract;
(4) gained medicinal extract in step (3) is added 50 times of rear upper ADS-15 posts of volume water dilution, first wash with water, until effluent liquid is colourless, use the ethanol elution of 70% of 50 times of volume medicinal extract again, collect elutriant, reclaim ethanol, be concentrated into medicinal extract, be the alcohol crystal of 80% by volumetric concentration again, obtain 0.45 gram of zeaxanthin.
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 is 70.3%.
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 (7)
1. the method for zeaxanthin in Extraction and enrichment wolfberry fruit, is characterized in that: comprise the steps:
(1) by dried wolfberry and extraction agent by expecting that molten mass volume ratio is put in the extraction kettle of subcritical fluid extraction device continuous extraction 1 ~ 20 time at 1: 1 ~ 1: 20, each 10 ~ 150min, is extracted thing;
(2) utilize decompression temperature-raising method make the extract in step (1) separating pressure be 0.10 ~ 1.95MPa, separation temperature is separated under being the condition of 10 ~ 90 DEG C, is extracted liquid;
(3) by after extraction liquid left at room temperature 10 ~ 90min, add extraction into ethyl acetate, after reclaiming organic phase, be concentrated into medicinal extract;
(4) diluted by medicinal extract, upper selectivity macroporous adsorptive resins, with ethanol elution, gained elutriant obtains zeaxanthin with alcohol crystal after reclaiming ethanol.
2. the method for zeaxanthin in a kind of Extraction and enrichment wolfberry fruit as claimed in claim 1, is characterized in that: in described step (1), extraction agent is any one in propane, butane, Trimethylmethane, dme, liquefied petroleum gas (LPG), HFA 134a.
3. the method for zeaxanthin in a kind of Extraction and enrichment wolfberry fruit as claimed in claim 1, is characterized in that: in described step (1), extraction conditions is extraction temperature 5 ~ 85 DEG C, extracting pressure 0.15 ~ 2.95MPa, extraction agent flow 10 ~ 200L/h.
4. the method for zeaxanthin in a kind of Extraction and enrichment wolfberry fruit according to claim 1, it is characterized in that: the volume of the ethyl acetate added in described step (3) and the volume ratio of extraction liquid are 1: 1, the number of times of extraction is 2 times.
5. the method for zeaxanthin in a kind of Extraction and enrichment wolfberry fruit according to claim 1, is characterized in that: the selectivity macroreticular resin in described step (4) is ADS-15 or ADS-17 or ADS-F8.
6. the method for zeaxanthin in a kind of Extraction and enrichment wolfberry fruit according to claim 1, is characterized in that: in described step (4), the volumetric concentration of wash-out ethanol is 50-70%, and the volumetric concentration of crystallization ethanol is 50-80%.
7. the method for zeaxanthin in a kind of Extraction and enrichment wolfberry fruit according to claim 1, it is characterized in that: medicinal extract 50-200 doubly upper prop after the water dilution of its weight in described step (4), the volumetric usage of described eluent ethanol is 30-60 times of medicinal extract weight.
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Cited By (3)
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| CN105462287A (en) * | 2016-01-26 | 2016-04-06 | 青岛百草纤维科技股份有限公司 | Method for extracting lavender dye and application of method to regenerated cellulose fiber dyeing |
| CN107459838A (en) * | 2017-06-05 | 2017-12-12 | 中国科学院兰州化学物理研究所 | Subcritical abstraction is combined the method for preparing medlar carotenoid class natural pigment with membrane separating and purifying concentration |
| CN107950867A (en) * | 2017-11-30 | 2018-04-24 | 周子云 | A kind of matrimony vine flour and preparation method thereof |
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| CN107459838A (en) * | 2017-06-05 | 2017-12-12 | 中国科学院兰州化学物理研究所 | Subcritical abstraction is combined the method for preparing medlar carotenoid class natural pigment with membrane separating and purifying concentration |
| CN107459838B (en) * | 2017-06-05 | 2019-07-30 | 中国科学院兰州化学物理研究所 | Subcritical abstraction combines the method for preparing medlar carotenoid class natural pigment with membrane separating and purifying concentration |
| CN107950867A (en) * | 2017-11-30 | 2018-04-24 | 周子云 | A kind of matrimony vine flour and preparation method thereof |
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Effective date of registration: 20200922 Address after: No.20, agricultural and sideline products processing park, hongguozhen, Huinong District, Shizuishan City, Ningxia Hui Autonomous Region Patentee after: Ningxia Haohan Biotechnology Industry Co.,Ltd. Address before: 753204 Yan Zi Dun Township, Hui Nong District, Shizuishan, the Ningxia Hui Autonomous Region Patentee before: Ningxia Bo Rui Yuan Industry and Trade Co.,Ltd. |
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