CN103626686A - Method for extracting lutein ester from marigold - Google Patents
Method for extracting lutein ester from marigold Download PDFInfo
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- CN103626686A CN103626686A CN201310654637.8A CN201310654637A CN103626686A CN 103626686 A CN103626686 A CN 103626686A CN 201310654637 A CN201310654637 A CN 201310654637A CN 103626686 A CN103626686 A CN 103626686A
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Abstract
The invention discloses a method for extracting lutein ester from marigold. The method comprises the following steps: selecting a raw material, fermenting, pressing, grinding, pelleting, extracting, filtering, concentrating by using a reverse osmosis membrane, thin film evaporation, blending, and barreling and warehousing after passing the inspection. Isopropyl alcohol is used as a solvent for extracting the lutein ester without containing benzene, phenol and hydrocarbon substances, so that harms to human bodies are avoided and the residual amount of harmful substances is reduced; harmful residues can be discharged without gasification, so that the production time and the production cost are reduced greatly; by a reverse osmosis membrane concentration technology, a lutein ester extract is concentrated at room temperature, without heating; the reverse osmosis membrane concentration technology is good in technical and economic performance; by the reverse osmosis membrane concentration technology, the quality and the yield of the lutein ester are greatly improved.
Description
Technical field
The present invention relates to a kind of method of extracting concentrated lutein factice, be specifically related to a kind of method of extracting xanthophyll-oil from dried marigold flower pellets.
Background technology
Xenthophylls (Lutein) belongs to carotenoid, chemical name is 3,3 '-dihydroxyl-alpha-carotene, molecular formula C40H5602, molecular weight is 568.85, and fusing point is 190 ℃, water insoluble and propylene glycol, be soluble in the ester solvents such as grease and ethanol, acetone, normal hexane, its chemical structural formula is:
By its structure, can find out, in the structural formula of lutein ester, contain a lot of unsaturated link(age)s, this structure just makes its physico-chemical property unstable especially, especially unstable to illumination, oxygen and temperature, is stored at ordinary times shady and cool dry place, lucifuge sealing.
Since xenthophylls is found, people study its pharmacologically active successively, find that it is a kind of antioxidant of excellent performance, there is the effect of anti-cancer, the a series of diseases that can prevent human body to cause because of organ senescence, prevention and treatment macula retinae degenerate and cause blind, control cardiovascula arteriosclerosis, coronary heart disease and tumor disease.Xenthophylls is distributed widely in the plants such as Caulis et Folium Brassicae capitatae, spinach, rape, mung bean, Kiwifruit, Flower of Aztec Marigold.In above-mentioned plant, it is the highest that the content of Flower of Aztec Marigold Lutein is found at present.In Flower of Aztec Marigold, except containing xenthophylls, also contain lutein ester, lutein ester is the binding substances of xenthophylls and lipid acid, and lutein ester can be sloughed lipid acid by the mode of hydrolysis under certain condition and be converted into xenthophylls.Due to the products characteristics of xenthophylls, it has extremely wide market application foreground, can apply to dietary supplements, heath food, functional drinks, makeup and bread and cheese.And because xenthophylls has 8 kinds of isomer, be difficult to, with chemosynthesis, can only from natural phant, extract so far.
The solvent great majority of current domestic extraction lutein factice are No. 6 main solvent oils for normal hexane with containing normal hexane 70%.Therefore residual a large amount of benzene, phenol and alkanes substance in the lutein ester after leaching, these materials are harmful to, and the later stage, in order to control the residual of these materials, can increase vaporizer, extend the time of evaporation, has rolled up production cost.And, utilize vacuum concentration equipment thickening temperature when concentrated too high, and concentration time is long.And its distinctive structures shape of xenthophylls lutein ester there is very strong unstable, the decomposition that it will be very fast in conditions such as temperature, illumination and oxygen, causes a large amount of losses of product.In addition, owing to using conventional thickening equipment, caused the low problem of trans-lutein in xenthophylls.
Summary of the invention
For the defect existing in prior art, the invention provides a kind of method of extracting lutein ester from Flower of Aztec Marigold, it is characterized in that comprising the steps:
1) Flower of Aztec Marigold is plucked, get its flower, with milk-acid bacteria, carry out lucifuge fermentation;
2) the Flower of Aztec Marigold flower after fermentation, through squeezing, after oven dry, is granulated after pulverizing;
3) above-mentioned particle is placed in airtight and the leacher with agitating function, adds leaching solvent, extraction temperature is 50 ℃, and extraction time is 2-3 hours, and stirring velocity is 10 turn/min, obtains the extracting solution of lutein ester;
4) under normal temperature condition, the extracting solution impeller pump of lutein ester is squeezed in temporary tank, start the concentrated program of reverse osmosis membrane, system return flow is controlled at 25M3/H-30M3/H, enters film pressure and is controlled at 10-15bar and concentrates;
5) above-mentioned lutein ester concentrated solution is carried out to reconcentration through thin-film evaporator;
6) lutein ester having concentrated is squeezed in treatment tank and allocated, under vacuum tightness-0.01～-0.02MPa, add massfraction and be 2% antioxidant;
7) detect qualified rear barrelling warehouse-in.
Further, the leavening temperature 25-35 ℃ in described step 1, fermentation time 7-15 days.
Further, the initial temperature of drying in described step 2 is 120-135 ℃, and dry rear damp-heat air temperature is 70-90 ℃, dried chrysanthemum is granulated after pulverizing, making grain diameter is 3-5mm, and particle length is 12-15mm, and particle water content is 7%-10%.
Further, the leaching solvent in described step 3 is Virahol.
Further, make system quantity of reflux be controlled between 25M3/H-30M3/H in described step 4, dialysis quantity of reflux is controlled between 35LPM-40LPM, enters film pressure and is controlled at 1.0MPa and concentrates below.
Further, in described step 5, the thickening temperature of thin-film evaporator is 50-55 ℃, turn/min of stirring velocity 20-30, concentration time 30min.
Further, the antioxidant in described step 6 is vitamin-E.
Further, lutein extract look valency content in described step 7 reaches 120-145g/Kg, and trans-lutein content reaches more than 75%, when dissolvent residual drops to 20ppm, gained food grade lutein ester is packed in the steel drum that meets food requirement, then enter stockyard and preserve.
The invention has the beneficial effects as follows,
1) the present invention uses Virahol as solvent, lutein ester to be extracted, not containing benzene, phenol and alkanes substance, so to not injury of human body, reduced the residual quantity of objectionable impurities, do not need gasification to discharge the Harmful Residue, thereby greatly shortened the production time, reduced production cost.
2) the present invention utilizes reverse osmosis membrane concentration technique, at normal temperatures lutein ester extracting solution is concentrated, do not need heating, it utilize lutein ester molecule and solvent Virahol molecular weight difference large, select a species specific reverse osmosis membrane, then give the two ends pressurization of film, solvent molecule can pass through this species specific reverse osmosis membrane, and lutein ester molecule can not pass through this film, thereby make solvent Virahol separated with solute lutein ester, reach concentrated object.Use this technical costs low, quality and the yield of lutein ester are all greatly improved.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
As shown in Figure 1, a kind of method of extracting lutein ester from Flower of Aztec Marigold, comprises the steps: to select materials, ferments, squeezing, pulverizing, granulation, extraction, filtration, reverse osmosis membrane are concentrated, thin film evaporation, allotment, the qualified rear barrelling warehouse-in of detection.Flower of Aztec Marigold is plucked, get its flower, with milk-acid bacteria, carry out lucifuge fermentation; 25-35 ℃ of leavening temperatures; fermentation time 7-15 days, the Flower of Aztec Marigold flower after fermentation, through squeezing, is dried; the initial temperature of drying is 120-135 ℃; after dry, damp-heat air temperature is 70-90 ℃, and dried chrysanthemum is granulated through ring film nodulizer by pulverizing again, and grain diameter is 3-5mm; particle length is 12-15mm, and particle water content is 7%-10%.Above-mentioned particle is transported in airtight and leacher with agitating function by lift and auger, add Virahol as the leaching solvent of lutein ester, the volume ratio of particle and solvent is 1: 5-1: 6, extraction temperature is 50 ℃, extraction time is 2-3 hour, and stirring velocity is 10 turn/min.Marigold particles after leaching is transported to sludge-store cabin by scraper plate, and bag bag packing, dispatches from the factory and use as feed.The extracting solution impeller pump of lutein ester is squeezed in temporary tank, opened reverse osmosis membrane thickening equipment, each valve of first monitoring device is controlled, and guarantees that each valve, all in correct on off state, opens equipment general supply, starts dehvery pump, start dehvery pump, after circular flow is stable (judgement system is substantially without gas), start high-pressure pump, regulate frequency converter frequency, the return flow of take is controlled between 25M3/H-30M3/H as good, adjustable cut-off valve, make system reach entering film flow (concentrated flow adds dialysis flow) and entering film pressure of setting, make into film pressure pressure-controlling at 10-15bar, (note: frequency converter frequency and stopping valve should regulate the system quantity of reflux of making to be controlled between 25M3/H-30M3/H simultaneously, dialysis quantity of reflux is controlled between 35LPM-40LPM, entering film pressure is controlled at 1.0MPa and concentrates below, in concentration process, do not do any operation) this concentration process carries out at normal temperatures.In order to control the residual of solvent in medicinal extract, by the lutein ester concentrated solution after reverse osmosis membrane concentration, through thin-film evaporator, concentrate again again thickening temperature 50-55 ℃, turn/min of stirring velocity 20-30, concentration time 30min.The lutein ester having concentrated is squeezed in treatment tank and allocated, under vacuum tightness-0.01～-0.02MPa, add massfraction and be 2% antioxidant, increase the storage life, according to the vegetables oil method for detecting residue in 4.8 standards in GB/T5009.37-2003, detect, lutein extract look valency content in food grade treatment tank reaches 120-145g/Kg, trans-lutein content reaches more than 75%, when dissolvent residual drops to 20ppm, food grade lutein ester is packed in the steel drum that meets food requirement, then enter stockyard and preserve.
The above,, only to the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various modifications and variations.Every in claim limited range of the present invention, any modification of making, be equal to replacement, improvement etc., all should be within protection scope of the present invention.
Claims (8)
1. from Flower of Aztec Marigold, extract a method for lutein ester, it is characterized in that comprising the steps:
1) Flower of Aztec Marigold is plucked, get its flower, with milk-acid bacteria, carry out lucifuge fermentation;
2) the Flower of Aztec Marigold flower after fermentation, through squeezing, after oven dry, is granulated after pulverizing;
3) above-mentioned particle is placed in airtight and the leacher with agitating function, adds leaching solvent, extraction temperature is 50 ℃, and extraction time is 2-3 hour, and stirring velocity is 10 turn/min, obtains the extracting solution of lutein ester;
4) under normal temperature condition, the extracting solution impeller pump of lutein ester is squeezed in temporary tank, start the concentrated program of reverse osmosis membrane, Controlling System return flow is at 25M3/H-30M3/H, enters film pressure and is controlled at 10-15bar and concentrates;
5) above-mentioned lutein ester concentrated solution is carried out to reconcentration through thin-film evaporator;
6) lutein ester having concentrated is squeezed in treatment tank and allocated, under vacuum tightness-0.01～-0.02MPa, add massfraction and be 2% antioxidant;
7) detect qualified rear barrelling warehouse-in.
2. a kind of method of extracting lutein ester from Flower of Aztec Marigold according to claim 1, is characterized in that: 25-35 ℃ of the leavening temperatures in described step 1, fermentation time 7-15 days.
3. a kind of method of extracting lutein ester from Flower of Aztec Marigold according to claim 1, it is characterized in that: the initial temperature of drying in described step 2 is 120-135 ℃, after dry, damp-heat air temperature is 70-90 ℃, dried chrysanthemum is granulated after pulverizing, making grain diameter is 3-5mm, particle length is 12-15mm, and particle water content is 7%-10%.
4. a kind of method of extracting lutein ester from Flower of Aztec Marigold according to claim 1, is characterized in that: the leaching solvent in described step 3 is Virahol.
5. a kind of method of extracting lutein ester from Flower of Aztec Marigold according to claim 1, it is characterized in that: in described step 4, make system quantity of reflux be controlled between 25M3/H-30M3/H, dialysis quantity of reflux is controlled between 35LPM-40LPM, enters film pressure and is controlled at 1.0MPa and concentrates below.
6. a kind of method of extracting lutein ester from Flower of Aztec Marigold according to claim 1, is characterized in that: in described step 5, the thickening temperature of thin-film evaporator is 50-55 ℃, turn/min of stirring velocity 20-30, concentration time 30min.
7. a kind of method of extracting lutein ester from Flower of Aztec Marigold according to claim 1, is characterized in that: the antioxidant in described step 6 is vitamin-E.
8. a kind of method of extracting lutein ester from Flower of Aztec Marigold according to claim 1, it is characterized in that: the lutein extract look valency content in described step 7 reaches 120-145g/Kg, trans-lutein content reaches more than 75%, when dissolvent residual drops to 20ppm, gained food grade lutein ester is packed in the steel drum that meets food requirement, then enter stockyard and preserve.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107629481A (en) * | 2017-09-06 | 2018-01-26 | 晨光生物科技集团莎车有限公司 | The production method of the marigold particles of lutein content can be improved |
| CN107652213A (en) * | 2017-09-06 | 2018-02-02 | 晨光生物科技集团股份有限公司 | The method for removing benzene homologues in lutein extract |
| CN109400512A (en) * | 2018-11-15 | 2019-03-01 | 北京联合大学 | It is a kind of for improving the fresh marigold flower inorganic agent of carotenoid extraction efficiency |
| CN111214846A (en) * | 2019-11-29 | 2020-06-02 | 云南绿A生物产业园有限公司 | Haematococcus pluvialis extract and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107629481A (en) * | 2017-09-06 | 2018-01-26 | 晨光生物科技集团莎车有限公司 | The production method of the marigold particles of lutein content can be improved |
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| CN107652213B (en) * | 2017-09-06 | 2019-09-10 | 晨光生物科技集团股份有限公司 | The method for removing benzene homologues in lutein extract |
| CN109400512A (en) * | 2018-11-15 | 2019-03-01 | 北京联合大学 | It is a kind of for improving the fresh marigold flower inorganic agent of carotenoid extraction efficiency |
| CN109400512B (en) * | 2018-11-15 | 2021-05-25 | 北京联合大学 | Tagetes fresh flower treating agent for improving carotenoid extraction efficiency |
| CN111214846A (en) * | 2019-11-29 | 2020-06-02 | 云南绿A生物产业园有限公司 | Haematococcus pluvialis extract and preparation method thereof |
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