CN103319389A - Method for preparing food-grade lutein crystal from marigold extract - Google Patents
Method for preparing food-grade lutein crystal from marigold extract Download PDFInfo
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- CN103319389A CN103319389A CN2013102728254A CN201310272825A CN103319389A CN 103319389 A CN103319389 A CN 103319389A CN 2013102728254 A CN2013102728254 A CN 2013102728254A CN 201310272825 A CN201310272825 A CN 201310272825A CN 103319389 A CN103319389 A CN 103319389A
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Abstract
The invention provides a method for preparing a food-grade lutein crystal from a marigold extract. The method comprises the following steps of: performing a saponification reaction on the marigold extract in a food-grade lower alcohol solvent by adding a solid alkali; diluting; then cooling and crystallizing; regulating the pH value; filtering; washing by adding an alcohol-water solution; and drying by adding a small amount of antioxidant, thereby obtaining lutein crystal powder. According to the method, the process is simple; the adopted solvent is recycled after being distilled, so that the treatment cost is low. Thus, the method is liable to industrial production. As the method is used, the defects of the existing lutein preparation method that the cost is high, the process is complicated, the time consumption is long and the lutein ester is unstable by performing reactions via harmful organic solvents under an acidic condition and at a high temperature are overcome. For the prepared lutein crystal, the actual yield is greater than 85%; and the purity reaches 80% to 90%. The prepared lutein crystal can be further prepared into an oil suspension or micro capsule powder which is applied to the fields of food additives, food supplements, functional foods and the like.
Description
Technical field
The present invention relates to the production technology research field of natural pigment, relate in particular to the method that is prepared high yield food grade lutein crystal by marigold extractum.
Background technology
Xenthophylls extensively is present in people and the nature animal and plant body, and the human and animal can not self synthesize, and xenthophylls synthetic in the plant materials mainly exists with the form of fatty acid ester.Human from fruit, vegetables, take in lutein ester by diet, in small intestine, be hydrolyzed to the xenthophylls monomer and enter blood circulation and run up to each organ and play a role.Studies show that xenthophylls has multiple functions such as painted, anti-oxidant, eye protection, anti-cardiovascular disease and cancer, is widely used in fields such as food, medicine, eye care product, makeup and aquaculture.In recent years, the market of xenthophylls product increased fast, and the research report of BCC points out that its market scale in 2010 is about 300,000,000 U.S. dollars.
The xenthophylls monomer mainly is to be raw material with the marigold extractum, utilizes the method production of saponification, recrystallization.But the solvent species of using in a lot of production methods is more, and the solvent intersection causes solvent recuperation cost height, and the recycling difficulty is big.Can use some harmful organic solvent such as normal hexane, methylene dichloride etc. in the recrystallization process, deal with improperly and can cause hazardous solvent residual, health risk, and recrystallization method uses, and quantity of solvent is big, energy consumption is high, length consuming time.
Feng Qinsheng etc. apply for a patent among the CN101130512, adopt adding potassium hydroxide aqueous solution saponification marigold extractum in ethanol and the tetrahydrofuran (THF) mixed solution, obtain the xenthophylls crude product after adding water crystallization, use washing with acetone again, and ethanol drip washing obtains the lutein crystal product.Used organic solvent kind is many in the technology, complex process.
Among the patent CN101429146 such as Lu state is fixed, adopt ethanol, sodium hydroxide system to carry out the saponification of marigold extractum, obtain coarse crystal after adding water, use the halogenated alkane recrystallization, add the ethanol molecular distillation again and remove halogenated alkane, obtain the lutein crystal of purity 90%.This technology need be carried out the recrystallization operation, uses harmful halogenated alkane solvent, and length consuming time.
Xue Jianduo applies for a patent among the CN101693681A, uses potassium hydroxide, ethanol and propylene glycol system to carry out the saponification of marigold extractum, behind the thin up, and the dry lutein crystal product that obtains after the centrifugation.This technology length consuming time, because of water content height in the product, only vacuum-drying just needs 24 hours, and propylene glycol boiling point height, is difficult for removing, and can cause dissolvent residual to exceed standard.
Among the patent CN1733719A of Xu Xinde etc. application, disclose a kind of from plant oil resin the method for extracting and purifying high content lutein crystal, adopt the absolute alcohol solvent in its process, through saponification, transfer pH, washing, alcohol to wash, dry and obtain lutein crystal.Be easy to generate a large amount of pure water mixed solvents in the technological process, be processed into absolute alcohol solvent cost height; And reaction solution adopts acid to transfer pH to 1-7, is warming up to 40-85 ℃, then separates out crystal again under 50-75 ℃ of condition, and the polyenoid chain in the xenthophylls molecule is easy to the oxidative degradation facilitated by light and heat, and is unstable under sour environment simultaneously.
In the US Patent No. 6380442, adopt Virahol, potassium hydroxide system to carry out the marigold extractum saponification, back thin up, centrifugal, obtain the lutein crystal product of UV content 95% through washing again, but the yield of technology is low, about 7%.
In the US Patent No. 5382714, saponified with the Flower of Aztec Marigold of desolventizing after the saponification is raw material, through alcohol-water mixture washing precipitation, distillation washing, low temperature organic solvent washing, again through methylene dichloride and normal hexane low temperature recrystallization, finally obtain purity and be higher than 90% lutein crystal after the oven dry earlier.This process steps is many, need cold operation, use food limiter stage solvent such as methylene dichloride etc., and needs recrystallization operation, length consuming time.
Among the US Patent No. 6380442B1, earlier marigold extractum is dissolved in the Virahol, adds the buck saponification then, be down to and add water solution after the room temperature and separate out crystal, reclaim crystal then.Whole process is simple relatively, does not use hazardous solvent.Can obtain the lutein crystal of UV content 53-95% according to pigment content in the raw material.But this process productive rate is low, uses the raw material of total pigment content 11%, and productive rate is less than 10%.
Among the US Patent No. 6743953B2, earlier with alkali dissolution in alcohol, add 65-80 ℃ of saponification under relatively-high temperature in the marigold extractum then, distill desolventizing then, thin up is used ethyl acetate extraction then, and distillation is removed ethyl acetate and obtained crude product, and then through n-hexane/acetone and washing with alcohol, oven dry obtains total pigment content and is higher than 85% lutein crystal.Too many, the consuming time length of this process steps, need use food grade restriction solvent, and productive rate also is lower than 10%.
In sum, exist common problem to be in most methods for the preparation of xenthophylls at present: (1) employed solvent is pure alcoholic solvent, and temperature is lower in (2) later stage crystal drying process.Pure solvent is in production process, and will inevitably bring water into and make its purity drop, aqueous alcohol solvent need special rectifying device to purify is neat solvent, need to consume bigger heat energy, and efficient is lower.The low production efficiency that can make of the drying temperature of lutein crystal reduces, and is in for a long time and can makes pigment produce degraded in the drying course.
Summary of the invention
In view of the further investigation of above problem, the invention provides and a kind ofly prepare the method for food grade lutein crystal powder by marigold extractum, to overcome problems such as cost height among the present xenthophylls preparation method, step complexity, length consuming time, product yield be low.Method technology of the present invention is simple, and environmental protection, content height, yield height, solvent for use are through the simple distillation reusable edible, and processing cost is low, is suitable for large-scale industrial production.
In order to realize purpose of the present invention, adopt following technical scheme.
A kind ofly prepare the method for food grade lutein crystal powder by marigold extractum, this method comprises the steps:
(1) add food grade aqueous alcohol solvent in the marigold extractum, stir, add sodium hydrate solid, complete to saponification at 50-60 ℃ of following stirring reaction;
(2) reaction solution of step (1) adds water and is cooled to 30-50 ℃ and kept 10-30 hour after the dilution, separates out crystallization;
(3) crystalloid solution of step (2) is transferred pH to 7-10, and insulation is filtered, and obtains filter cake I;
(4) after filter cake I washed with 50-60 ℃ of aqueous ethanolic solution, insulation was filtered, and obtains the filter cake II;
(5) the filter cake II with 95% washing with alcohol after, filter and to obtain the filter cake III;
(6) add small amount of antioxidant in the filter cake III, oven dry obtains the lutein crystal powder.
In the step (1), described saponification reaction is that the lutein ester in the marigold extractum is converted into the xenthophylls monomer and it is free in process in the reaction solution, and whether saponification reaction can be monitored by the area normalization content of lutein ester in the HPLC method detection reaction liquid fully.Among the present invention, it is the Virahol of 12-14% that the described aqueous alcohol solvent of step (1) is preferably ethanol or the water content that water content is 5-6%; The described aqueous alcohol solvent load of step (1) is preferably 3-8 times of marigold extractum quality, and more preferably 4-6 doubly; The sodium hydrate solid consumption is preferably the 15-40% of marigold extractum quality, more preferably 20-35%.
In the step (2), add water-reducible reaction solution and place in the crystallization process down at 30-50 ℃, reaction solution will slowly stir, and is conducive to promote separating out and improving the purity of separating out crystallization of crystal.Among the present invention, reaction solution adds water and is diluted in the reaction solution water content between 55-68%, preferred 55-65% in the step (2).
In the step (3), the pH value of crystalloid solution is adjusted to 7-10, neutrality or weak basic condition effectively prevent the degraded of free lutein crystal, improve purification efficiency.Among the present invention, the pH value of crystalloid solution preferably transfers to 7.5-9.0.
In the step (4), filter cake I removes water soluble components such as fatty acid sodium soap with 50-60 ℃ of aqueous ethanolic solution washing.Among the present invention, the volume percent of ethanol is preferably 40%-70% in the described aqueous ethanolic solution of step (4), more preferably 50-60%; Described aqueous ethanolic solution consumption is preferably 2-7 times of marigold extractum quality, and more preferably 3-5 doubly.
Among the present invention, described 95% consumption of ethanol of step (5) is preferably 2-8 times of marigold extractum quality, and more preferably 3-6 doubly.
In the step (6), described antioxidant kind and add-on will not limit, can use in this area the normal antioxidant that is suitable for human edible product that uses with and consumption commonly used.Among the present invention, the described bake out temperature of step (6) is preferably 50-90 ℃.
Of the present inventionly prepare the method for food grade lutein crystal powder by marigold extractum, in the saponification reaction and last handling process of marigold extractum, only use food grade aqueous alcohol solvent, in the product that obtains, no hazardous solvent is residual, can be suitable for human edible; Solvent after the use can be recycled after simple process, avoids in the prior art resource that the purification because of solvent brings, the consumption on the heat energy, significantly reduces production costs, and is conducive to suitability for industrialized production.
In the method for the present invention, marigold extractum is taked hyperthermia drying through the lutein crystal (filter cake III) that saponification reaction and subsequent separation, purification process obtain, finish oven dry at short notice, enhance productivity and guarantee that crystal do not degrade, the content of the lutein crystal powder that drying obtains all reaches the 80-90%(UV detection level), wherein the alltrans lutein content is higher than 90%.
In the method for the present invention, the alkali that uses in the saponification reaction is solid alkali, can directly add in the commercial process, and is easy to operate.Can avoid the personal security problem of using alkali aqueous solution in process for preparation, to cause, and heat release need be lowered the temperature and the energy consumption problem that brings in the alkali dissolution process.
Polyenoid chain in the xenthophylls molecule is easy to the oxidative degradation facilitated by light and heat, and is unstable under sour environment simultaneously.In the present invention in order to reduce the degraded of xenthophylls molecule in operating process as much as possible, after marigold extractum saponification in alcohol-water system (step (1)), crystallization solution (step (3)) the adjustment pH that separates out crystallization through cooling is neutrality or weakly alkaline, prevent the degraded of free lutein, guarantee the stability of xenthophylls, improve extraction efficiency.
Preparation method of the present invention the institute in steps in, the water described in water-containing solvent or the thin up process can also can be ordinary tap water for deionized water, preferably uses tap water, to reach the purpose that further reduces production costs.
Another object of the present invention provides the lutein crystal powder by method preparation of the present invention.Detect through ultraviolet-visible spectrophotometer, lutein content meets China to purity requirement 〉=80% of lutein crystal powder food additive up to 80-90% in this lutein crystal powder, and pure yield＞85% of lutein crystal among the present invention.Lutein crystal powder of the present invention can further be made oil suspension, the micro-capsule powder is applied to fields such as foodstuff additive, dietary supplements, functional food.
Beneficial effect of the present invention:
1. after the alcohol-water system saponification, separate out the crystallization solution of crystallization through cooling and transfer pH to be neutrality or weakly alkaline, prevent the degraded of free lutein, guarantee the stability of xenthophylls;
2. adopt gentle crystallization condition to make the pure yield of xenthophylls up to more than 85%;
3. the solvent of all uses directly recycle after reclaiming in the preparation process need not carried out purification process, significantly reduces cost.
4. use the food-grade alcohol solvent in the preparation process, no hazardous solvent is residual, preparation technology's environmental protection.
5. preparation process is simple, need not carry out the recrystallization operation, is easy to amplify and carries out suitability for industrialized production.
Embodiment
Following non-limiting example can make those of ordinary skill in the art more fully understand the present invention, but does not limit the present invention in any way.
Xenthophylls Determination on content in the marigold extractum, the method for AOAC official method 970.64 records in the concrete grammar reference.
Described saponification reaction is that the lutein ester in the marigold extractum is converted into the xenthophylls monomer and it is free in process in the reaction solution, whether saponification reaction can be monitored by the area normalization content of lutein ester in the HPLC method detection reaction liquid fully, thinks that saponification reaction is complete when detection level is≤0.7%.
Embodiment 1
20.0g marigold extractum, wherein lutein content is 156.29mg/g, adding volume is 95% ethanol of 3 times of medicinal extract quality, stir, add the sodium hydrate solid of medicinal extract quality 20% again, 50 ℃ down reaction 6 hours is complete to saponification reaction, add the dilution of 100mL tap water and be cooled to 35 ℃, slowly stir crystallization down 16 hours, to the 8-9 after-filtration, get the filter cake I with the Glacial acetic acid adjust pH; The filter cake I adds 100mL50% aqueous ethanolic solution washing after-filtration under 50 ℃, gets the filter cake II; The filter cake II adds 60mL95% washing with alcohol after-filtration again, and filter cake is dried down in 60 ℃ after adding antioxidant, obtains lutein crystal powder 3.50g, wherein xenthophylls UV content is 83.27%, detect through HPLC, the alltrans lutein content is 92.45%, and the pure yield of xenthophylls is 86.20%.
Embodiment 2
20.0g marigold extractum, wherein lutein content is 156.29mg/g, adding volume is 88% Virahol of 5.5 times of medicinal extract quality, stir, add the sodium hydrate solid of medicinal extract quality 30% again, 50 ℃ down reaction 3 hours is complete to saponification reaction, add the dilution of 105mL tap water and be cooled to 45 ℃, slowly stir crystallization down 24 hours, to the 8-9 after-filtration, get the filter cake I with the Glacial acetic acid adjust pH; The filter cake I adds 80mL60% isopropanol water solution washing after-filtration under 50 ℃, gets the filter cake II; The filter cake II adds 40mL95% washing with alcohol after-filtration again, and filter cake is dried down in 80 ℃ after adding antioxidant.Obtain lutein crystal powder 3.65g, wherein xenthophylls UV content is 81.52%, detects through HPLC, and the alltrans lutein content is 91.32%, and the pure yield of xenthophylls is 86.93%.
Embodiment 3
20.0g marigold extractum, wherein lutein content is 153.55mg/g, adding volume is 95% ethanol of 7 times of medicinal extract quality, stir, add the sodium hydrate solid of medicinal extract quality 35% again, 50 ℃ down reaction 5 hours is complete to saponification reaction, add the dilution of 170mL tap water and be cooled to 40 ℃, slowly stir crystallization down 24 hours, to the 8-9 after-filtration, get the filter cake I with the Glacial acetic acid adjust pH; The filter cake I adds 100mL60% aqueous ethanolic solution washing after-filtration under 60 ℃, gets the filter cake II; The filter cake II adds 120mL95% washing with alcohol after-filtration again, and filter cake is dried down in 50 ℃ after adding antioxidant.Obtain lutein crystal powder 3.13g, wherein xenthophylls UV content is 90.20%, detects through HPLC, and the alltrans lutein content is 92.75%, and the pure yield of xenthophylls is 85.27%.
Embodiment 4
20.0g marigold extractum, wherein lutein content is 152.53mg/g, adding volume is 95% ethanol of 6 times of medicinal extract quality, stir, add the sodium hydrate solid of medicinal extract quality 25% again, 60 ℃ down reaction 5 hours is complete to saponification reaction, add the dilution of 200mL tap water and be cooled to 50 ℃, slowly stir crystallization down 24 hours, to the 8-9 after-filtration, get the filter cake I with the Glacial acetic acid adjust pH; The filter cake I adds 140mL40% aqueous ethanolic solution washing after-filtration under 50 ℃, gets the filter cake II; The filter cake II adds 160mL95% washing with alcohol after-filtration again, and filter cake is dried down in 70 ℃ after adding antioxidant.Obtain lutein crystal powder 3.34g, wherein xenthophylls UV content is 85.36%, detects through HPLC, and the alltrans lutein content is 92.15%, and the pure yield of xenthophylls is 86.12%.
The lutein crystal powder for preparing among all embodiment is safran, crystal grain can pass through 40 mesh sieves more than 95%.
Claims (8)
1. one kind prepares the method for food grade lutein crystal by marigold extractum, it is characterized in that this method comprises the steps:
(1) add food grade aqueous alcohol solvent in the marigold extractum, stir, add sodium hydrate solid, complete to saponification at 50-60 ℃ of following stirring reaction;
(2) reaction solution of step (1) adds water and is cooled to 30-50 ℃ and kept 10-30 hour after the dilution, separates out crystallization;
(3) crystalloid solution of step (2) is transferred pH to 7-10, and insulation is filtered, and obtains filter cake I;
(4) after filter cake I washed with 50-60 ℃ of aqueous ethanolic solution, insulation was filtered, and obtains the filter cake II;
(5) the filter cake II with 95% washing with alcohol after, filter and to obtain the filter cake III;
(6) add small amount of antioxidant in the filter cake III, oven dry obtains the lutein crystal powder.
2. method according to claim 1 is characterized in that, the described aqueous alcohol solvent of step (1) is that water content is that ethanol or the water content of 5-6% is the Virahol of 12-14%.
3. method according to claim 1 is characterized in that, the 3-8 that the described aqueous alcohol solvent load of step (1) is the marigold extractum quality doubly; The sodium hydrate solid consumption is the 15-40% of marigold extractum quality.
4. method according to claim 1 is characterized in that, reaction solution described in the step (2) adds water and is diluted in the reaction solution water content between 55-68%.
5. method according to claim 1 is characterized in that, the volume percent of ethanol is 40%-70% in the described aqueous ethanolic solution of step (4), and the aqueous ethanolic solution consumption is 2-7 times of marigold extractum quality.
6. method according to claim 1 is characterized in that, the 2-8 that described 95% consumption of ethanol of step (5) is the marigold extractum quality doubly.
7. method according to claim 1 is characterized in that, the described bake out temperature of step (6) is 50-90 ℃.
8. the lutein crystal powder of the described method of each of claim 1-7 preparation.
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Cited By (7)
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| CN103755615A (en) * | 2014-01-14 | 2014-04-30 | 青岛赛特香料有限公司 | Production method of liquid lutein |
| CN103936643A (en) * | 2014-03-20 | 2014-07-23 | 江苏大学 | Method for extraction and separation of xanthophyll and flavones in marigold |
| CN104447468A (en) * | 2014-11-17 | 2015-03-25 | 晨光生物科技集团股份有限公司 | Deep processing method of lutein extract |
| CN106748947A (en) * | 2017-02-20 | 2017-05-31 | 青岛藻蓝生物有限公司 | A kind of method that efficient joint prepares high-purity lutein ester and lutein |
| CN112704739A (en) * | 2020-12-29 | 2021-04-27 | 佛山市南海东方澳龙制药有限公司 | Preparation method of lutein preparation and lutein preparation |
| CN110590629B (en) * | 2019-09-29 | 2021-07-13 | 山东天音生物科技有限公司 | Method for separating and purifying lutein from marigold oleoresin |
| CN115925602A (en) * | 2022-11-30 | 2023-04-07 | 西安交通大学 | Method for extracting lutein from marigold by using eutectic solvent |
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| CN103755615A (en) * | 2014-01-14 | 2014-04-30 | 青岛赛特香料有限公司 | Production method of liquid lutein |
| CN103755615B (en) * | 2014-01-14 | 2015-10-21 | 青岛赛特香料有限公司 | A kind of production method of liquid lutein |
| CN103936643A (en) * | 2014-03-20 | 2014-07-23 | 江苏大学 | Method for extraction and separation of xanthophyll and flavones in marigold |
| CN103936643B (en) * | 2014-03-20 | 2016-07-06 | 江苏大学 | A kind of method extracting separation Flos Tagetis Erectae Lutein and flavone |
| CN104447468A (en) * | 2014-11-17 | 2015-03-25 | 晨光生物科技集团股份有限公司 | Deep processing method of lutein extract |
| CN106748947A (en) * | 2017-02-20 | 2017-05-31 | 青岛藻蓝生物有限公司 | A kind of method that efficient joint prepares high-purity lutein ester and lutein |
| CN106748947B (en) * | 2017-02-20 | 2018-06-26 | 青岛藻蓝生物有限公司 | It is a kind of to combine the method for preparing lutein ester and lutein |
| CN110590629B (en) * | 2019-09-29 | 2021-07-13 | 山东天音生物科技有限公司 | Method for separating and purifying lutein from marigold oleoresin |
| CN112704739A (en) * | 2020-12-29 | 2021-04-27 | 佛山市南海东方澳龙制药有限公司 | Preparation method of lutein preparation and lutein preparation |
| CN115925602A (en) * | 2022-11-30 | 2023-04-07 | 西安交通大学 | Method for extracting lutein from marigold by using eutectic solvent |
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