CN104447465A - Food-grade lutein ester preparation technique - Google Patents
Food-grade lutein ester preparation technique Download PDFInfo
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- CN104447465A CN104447465A CN201310440374.0A CN201310440374A CN104447465A CN 104447465 A CN104447465 A CN 104447465A CN 201310440374 A CN201310440374 A CN 201310440374A CN 104447465 A CN104447465 A CN 104447465A
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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
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Abstract
The invention relates to a food-grade lutein ester preparation technique. A supercritical technique is utilized to carry out deep processing on the lutein ester which is prepared by an organic solvent extraction process, so that the lutein ester is applicable to food, medicine, nutriment and the like. Three-stage extraction is performed by using a lutein ester extractum as a raw material and supercritical CO2 as an extraction fluid: secondary and tertiary extraction fluids of the previous cycle are used as primary and secondary extraction fluids of the next cycle, the tertiary extraction of each cycle uses the fresh supercritical CO2 fluid, and the pressure and temperature for extraction are respectively 15-25 MPa and 50-70 DEG C; and two-stage separation is performed after each extraction stage, wherein the pressure and temperature for primary separation are respectively 7-12 MPa and 35-45 DEG C, and pressure and temperature for secondary separation are respectively 5-7 MPa and 25-35 DEG C. The method can enhance the lutein content and effectively remove impurity free fatty acids, unpleasant odor and residual solvent in the product, so that the product satisfies the food safety standard.
Description
Technical field
The present invention utilizes supercritical technology, carries out deep processing to lutein ester prepared by organic solvent extractionprocess, makes lutein ester be applied to food, medicine and nutritious prod etc.
Background technology
Xenthophylls is a kind of oxygen containing class trailing plants L element recklessly, is generally present in banana, Kiwifruit, corn and Flower of Aztec Marigold, has different physiological roles, as anti-oxidant, eliminate the functions such as free radical, anticancer, the sickness rate that reduces cardiovascular diseases and vision protection.China's plantation marigold flower has reached 40 ~ 500,000 mu, accounts for more than 80% of grown worldwide area.Extract lutein ester medicinal extract with organic solvent method from Flower of Aztec Marigold and form industrialization, but containing the fatty acid ester of more than 60% in medicinal extract, lutein content only has about 15%, because organic solvent and fatty acid ester combine, low temperature conventional at present vacuumizes the method removing solvent, do not reach food grade to residual solvent required standard, residual solvent is up to 20000ppm.The taste of fermentation residue is denseer, and acid value is up to more than 40, and great majority are used for fodder additives and process raw material, and can not be used for foodstuffs industry processing.In Chinese patent literature, " a kind of method of refining lutein by supercritical extraction " (application number 201010517156.9) discloses the method removing Flos Tagetis Erectae extract peculiar smell, and new organic solvent-acetone and propyl carbinol is being with the addition of again in overcritical processing and refining process, although the method can remove Flos Tagetis Erectae extract peculiar smell, and improve the content of xenthophylls to a certain extent, but solvents still residual a large amount of in product, is also difficult to reach food grade standard.
Summary of the invention
This technical problem to be solved by this invention is to provide a kind of method preparing food-grade lutein ester, can improve lutein content, effectively removes impurity free fatty acid, unpleasant odor and residual solvent in product, reaches food security standard.
Realizing the technical scheme that the object of the invention takes is: with lutein ester medicinal extract for raw material, supercritical CO 2 is extraction fluid, carry out three grades of extractions, 2nd, 3 grade of extraction fluid of last circulation is used as the 1st, 2 grade of extraction fluid of next circulation, and the 3rd grade of extraction of each circulation use the fluid of fresh supercritical CO 2, extracting pressure and temperature be respectively 18 ~ 28MPa, 55 ~ 65 DEG C; Carry out the second-order separation after every grade of extraction, first step separating pressure and temperature are respectively 6 ~ 10MPa and 30 ~ 40 DEG C, and second stage separating pressure and temperature are respectively 4 ~ 6MPa and 20 ~ 30 DEG C.
In above-mentioned operation, the extraction time of every one-level is 1 ~ 2h, and every flash trapping stage time is 1 ~ 2h.
Lutein ester medicinal extract first should carry out heating in water bath before extraction, and temperature is 50 ~ 60 DEG C, and under agitation keeps 30 ~ 120 min, or is placed in vacuum degasser by medicinal extract and removes smell; First extraction kettle temperature should be increased to 55 ~ 65 DEG C during extraction, then medicinal extract is loaded in still, open air valve door, make whole extracting system pressure equilibrium, and keep 30min, then start pressure extraction.
Advantageous Effects of the present invention is as follows.
(1) product Lutein content can be increased to 240 ~ 280g/kg from about 150g/kg, and on average can reach 260g/kg, lutein content on average improves 67%, and the active substance rate of recovery reaches more than 90%;
(2) the total residual solvent in product can be reduced to below 50ppm from 20000ppm, reaches the requirement of food security standard;
(3) effectively can remove the impurity free fatty acid in product and unpleasant odor, acid value drops to about 10 from 40, is more conducive to storage and the use of product;
(4) present method does not introduce other organic solvent, good to environment.
The present invention's supercritical extraction technique, add counter-current extraction scheme, supercutical fluid is divided into three grades, the parameters such as variation extraction pressure and temperature, can be separated and remove some free fatty acids and organic residual solvent, remove the taste of lutein extract, the more effective content that improve xenthophylls, do not add other organic solvent, extend the shelf life, reach food grade standard.
Embodiment
Embodiment 1
1, get marigold flower slightly to carry lutein extract 120g and be placed in beaker, heating in water bath to 60 DEG C also keeps 30min;
2, overcritical equipment is opened, after still temperature to be extracted is increased to 55 DEG C, medicinal extract is transferred in extraction kettle, build plug, open air valve door, make whole extracting system pressure equilibrium, and keep 30min, put into the 2nd grade of supercritical CO 2 extraction fluid of last circulation, then start pressure extraction;
3, extraction conditions is: extracting pressure 26Mpa, extraction temperature 60 DEG C, and first step separating pressure and temperature are respectively 8MPa and 40 DEG C, and second stage separating pressure and temperature are respectively 5MPa and 30 DEG C;
4, after extracting 2h, release separated product, and be replaced with the 3rd grade of supercritical CO 2 extraction fluid of last circulation; Then keep previous step extraction conditions constant continuation extraction 1h, release separated product, and change fresh supercritical CO
2extraction fluid; Continue again to keep extraction conditions constant continuation extraction 1h, shut down release, from separating still, take out extraction product food-grade lutein ester 62.4g;
5, according to corresponding method of detection in GB, detect lutein content, Determination of Residual Organic Solvents and the free fatty acid content in raw material marigold flower medicinal extract and extraction product food-grade lutein ester, detected result is as shown in table 1.
In step 1 described above, if medicinal extract smell is overweight, soaking time to 1 ~ 2h can be extended, words with good conditionsi, can whipping appts be installed additional, or medicinal extract is placed in vacuum degasser.
Table 1 marigold flower medicinal extract and each index contrast of food-grade lutein ester
| Marigold extractum | Food-grade lutein ester | |
| Lutein content (g/kg) | 150.5 | 250.5 |
| Determination of Residual Organic Solvents (ppm) | 19500 | 40 |
| Acid value | 48 | 10 |
Embodiment 2
1, get the thick extracted extract 105g of marigold flower and be placed in beaker, heating in water bath to 60 DEG C also keeps 30min;
2, open overcritical equipment, after still temperature to be extracted is increased to 60 DEG C, medicinal extract is transferred in extraction kettle, builds plug, open air valve door, make whole extracting system pressure equilibrium, and keep 30min, put into the 2nd grade of supercritical CO of last circulation
2extraction fluid, then starts pressure extraction;
3, extraction conditions is: extracting pressure 25Mpa, extraction temperature 60 DEG C, and first step separating pressure and temperature are respectively 10MPa and 36 DEG C, and second stage separating pressure and temperature are respectively 5MPa and 26 DEG C;
4, after extracting 2h, release separated product, and be replaced with the 3rd grade of supercritical CO of last circulation
2extraction fluid; Then keep extraction conditions constant continuation extraction 2h, release separated product, and change fresh supercritical CO
2extraction fluid; Continue again to keep extraction conditions constant continuation extraction 2h, shut down release, from separating still, take out extraction product food-grade lutein ester 58.3g;
5, according to corresponding method of detection in GB, detect lutein content, Determination of Residual Organic Solvents and the free fatty acid content in raw material marigold flower medicinal extract and extraction product food-grade lutein ester, detected result is as shown in table 2.
Table 2 marigold flower medicinal extract and each index contrast of food-grade lutein ester
| Marigold extractum | Food-grade lutein ester | |
| Lutein content (g/kg) | 160.5 | 270.8 |
| Determination of Residual Organic Solvents (ppm) | 21500 | 40 |
| Acid value | 50 | 12 |
Embodiment 3:
1, get the thick extracted extract 110g of marigold flower and be placed in beaker, heating in water bath to 65 DEG C also keeps 30min;
2, open overcritical equipment, after still temperature to be extracted is increased to 65 DEG C, medicinal extract is transferred in extraction kettle, builds plug, open air valve door, make whole extracting system pressure equilibrium, and keep 30min, put into the 2nd grade of supercritical CO of last circulation
2extraction fluid, then starts pressure extraction;
3, extraction conditions is: extracting pressure 20Mpa, extraction temperature 65 DEG C, and first step separating pressure and temperature are respectively 8MPa and 40 DEG C, and second stage separating pressure and temperature are respectively 4MPa and 30 DEG C;
4, after extracting 2h, release separated product, and be replaced with the 3rd grade of supercritical CO 2 extraction fluid of last circulation; Then keep extraction conditions constant continuation extraction 2h, release separated product, and change fresh supercritical CO
2extraction fluid; Continue again to keep extraction conditions constant continuation extraction 1h, shut down release, from separating still, take out extraction product food-grade lutein ester 55.7g;
5, according to corresponding method of detection in GB, detect lutein content, Determination of Residual Organic Solvents and the free fatty acid content in raw material marigold flower medicinal extract and extraction product food-grade lutein ester, detected result is as shown in table 3.
Table 3 marigold flower medicinal extract and each index contrast of food-grade lutein ester
| Marigold extractum | Food-grade lutein ester | |
| Lutein content (g/kg) | 155.2 | 276.4 |
| Determination of Residual Organic Solvents (ppm) | 19000 | 38 |
| Acid value | 45 | 11 |
Claims (3)
1. prepare a method for food-grade lutein ester, it is characterized in that: with lutein ester medicinal extract for raw material, supercritical CO
2for extraction fluid, carry out three grades of extractions, the 2nd, 3 grade of extraction fluid of last circulation is used as the 1st, 2 grade of extraction fluid of next circulation, and the 3rd grade of extraction of each circulation uses fresh supercritical CO
2fluid, extracting pressure and temperature are respectively 15-25MPa, 50-70 DEG C; Carry out the second-order separation after every grade of extraction, first step separating pressure and temperature are respectively 7-12MPa and 35-45 DEG C, and second stage separating pressure and temperature are respectively 5-7MPa and 25-35 DEG C.
2. by the method preparing food-grade lutein ester described in claim 1, it is characterized in that: the extraction time of every one-level is 1-2h, and every flash trapping stage time is 1-2h.
3. by the method preparing food-grade lutein ester described in claim 2, it is characterized in that: lutein ester medicinal extract first carries out heating in water bath before extraction, temperature is 50-60 DEG C, and under agitation keeps 30-120 min, or is placed in vacuum degasser by medicinal extract and removes smell; First extraction kettle temperature should be increased to 50-70 DEG C during extraction, then medicinal extract is loaded in still, open air valve door, make whole extracting system pressure equilibrium, and keep 30min, then start pressure extraction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310440374.0A CN104447465A (en) | 2013-09-25 | 2013-09-25 | Food-grade lutein ester preparation technique |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310440374.0A CN104447465A (en) | 2013-09-25 | 2013-09-25 | Food-grade lutein ester preparation technique |
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| CN104447465A true CN104447465A (en) | 2015-03-25 |
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| CN201310440374.0A Pending CN104447465A (en) | 2013-09-25 | 2013-09-25 | Food-grade lutein ester preparation technique |
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Application publication date: 20150325 |