CN102757372B - Method for preparing food-grade lutein ester - Google Patents
Method for preparing food-grade lutein ester Download PDFInfo
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- CN102757372B CN102757372B CN201210267872.5A CN201210267872A CN102757372B CN 102757372 B CN102757372 B CN 102757372B CN 201210267872 A CN201210267872 A CN 201210267872A CN 102757372 B CN102757372 B CN 102757372B
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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 discloses a method for preparing food-grade lutein ester. In the method, lutein ester prepared with an organic solvent extracting method is deeply processed by using a supercritical technology, so that lutein ester is applied to foods, medicine, nutrients and the like. The method comprises the following steps of: performing three-stage extraction by taking a lutein ester extract as a raw material and taking supercritical CO2 as an extraction fluid, wherein second-stage and third-stage extraction fluids in a previous cycle are taken as first-stage and second-stage extraction fluids in a next cycle, a fresh supercritical CO2 fluid is used in the third-stage extraction in each cycle, the extraction pressure and temperature are 18-28MPa and 55-65 DEG C respectively; and performing second-stage separation after each stage of extraction, wherein the first-stage separation pressure and temperature are 6-10MPa and 30-40 DEG C respectively, and the second-stage separation pressure and temperature are 4-6MPa and 20-30 DEG C respectively. Due to the adoption of the method, the lutein content can be increased, impurity free fatty acid, objectionable odors and residual solvents in a product can be effectively removed, and a food safety standard can be reached.
Description
Technical field
The present invention utilizes supercritical technology, and lutein ester prepared by organic solvent extractionprocess carries out deep processing, 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, general being present in banana, Kiwifruit, corn and Flower of Aztec Marigold, there is different physiological roles, as anti-oxidant, eliminate free radical, anticancer, the function such as sickness rate and vision protection that reduces cardiovascular diseases.China's plantation marigold flower has reached 40～500,000 mu, accounts for the more than 80% of global cultivated area.Extract lutein ester medicinal extract with organic solvent method from Flower of Aztec Marigold and formed industrialization, but in medicinal extract, contain more than 60% fatty acid ester, lutein content only has 15% left and right, because organic solvent and fatty acid ester combine, conventional low temperature vacuumizes the method for removing solvent at present, 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 process raw material for fodder additives, 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 for removing Flos Tagetis Erectae extract peculiar smell, and adding again new organic solvent-acetone and propyl carbinol in overcritical processing and refining process, although the method can be removed Flos Tagetis Erectae extract peculiar smell, and improve to a certain extent the content of xenthophylls, but residual a large amount of solvent still in product, is also difficult to reach food grade standard.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of preparing food grade lutein ester, can improve lutein content, effectively removes impurity free fatty acids, unpleasant odor and residual solvent in product, reaches food security standard.
Realizing the technical scheme that the object of the invention takes is: taking lutein ester medicinal extract as raw material, and supercritical CO
2for extraction fluid, carry out three grades of extractions, the 2nd, 3 grades of extraction fluids of last circulation are used as the 1st, 2 grades of extraction fluids of next circulation, and the extraction of the 3rd level of each circulation is used fresh supercritical CO
2fluid, extracting pressure and temperature are respectively 18～28MPa, 55～65 DEG C; After every grade of extraction, carry out the second-order separation, 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 should first carry out heating in water bath before extraction, and temperature is 50～60 DEG C, and under agitation keeps 30～120 min, or medicinal extract is placed in and in vacuum degasser, removes smell; When extraction, should first extraction kettle temperature be increased to 55～65 DEG C, then medicinal extract is packed in still, open air valve door, make whole extracting system pressure equilibrium, and keep 30min, then start pressure extraction.
The useful technique effect of the present invention is as follows.
(1) product Lutein content can be increased to 240～280g/kg from 150g/kg left and right, on average can reach 260g/kg, and lutein content has on average improved 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) can effectively remove impurity free fatty acids and the unpleasant odor in product, acid value drops to 10 left and right from 40, is more conducive to storage and the use of product;
(4) present method is not introduced 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 separate and remove some free fatty acids and organic residual solvent, remove the taste of lutein extract, the more effective content that improves xenthophylls, do not add other organic solvent, extend the shelf life, reach food grade standard.
Embodiment
Embodiment 1
1, get marigold flower and slightly carry lutein extract 120g and be placed in beaker, heating in water bath to 60 DEG C also keeps 30min;
2, open overcritical equipment, be increased to after 55 DEG C until extraction kettle temperature, 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 of last circulation
2extraction fluid, then starts pressure extraction;
3, extraction conditions is: extracting pressure 26Mpa, and 60 DEG C of extraction temperature, 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 extraction 2h, emit separated product, and be replaced with the 3rd level supercritical CO of last circulation
2extraction fluid; Then keep the constant continuation extraction of previous step extraction conditions 1h, emit separated product, and change fresh supercritical CO
2extraction fluid; Continue again to keep the constant continuation extraction of extraction conditions 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 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, if medicinal extract smell is overweight, can extend soaking time to 1～2h as mentioned above, words with good conditionsi, can install whipping appts additional, or medicinal extract is placed in vacuum degasser.
The each index contrast of table 1 marigold flower medicinal extract and food grade lutein ester
。
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, be increased to after 60 DEG C until extraction kettle temperature, 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 of last circulation
2extraction fluid, then starts pressure extraction;
3, extraction conditions is: extracting pressure 25Mpa, and 60 DEG C of extraction temperature, 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 extraction 2h, emit separated product, and be replaced with the 3rd level supercritical CO of last circulation
2extraction fluid; Then keep the constant continuation extraction of extraction conditions 2h, emit separated product, and change fresh supercritical CO
2extraction fluid; Continue again to keep the constant continuation extraction of extraction conditions 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 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.
The each index contrast of table 2 marigold flower medicinal extract and food grade lutein ester
。
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, be increased to after 65 DEG C until extraction kettle temperature, 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 of last circulation
2extraction fluid, then starts pressure extraction;
3, extraction conditions is: extracting pressure 20Mpa, and 65 DEG C of extraction temperature, 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 extraction 2h, emit separated product, and be replaced with the 3rd level supercritical CO of last circulation
2extraction fluid; Then keep the constant continuation extraction of extraction conditions 2h, emit separated product, and change fresh supercritical CO
2extraction fluid; Continue again to keep the constant continuation extraction of extraction conditions 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 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.
The each index contrast of table 3 marigold flower medicinal extract and food grade lutein ester
。
Claims (3)
1. a method of preparing food grade lutein ester, is characterized in that: taking lutein ester medicinal extract as raw material, and supercritical CO
2for extraction fluid, carry out three grades of extractions, the 2nd, 3 grades of extraction fluids of last circulation are used as the 1st, 2 grades of extraction fluids of next circulation, and the extraction of the 3rd level of each circulation is used fresh supercritical CO
2fluid, extracting pressure and temperature are respectively 18～28MPa, 55～65 DEG C; After every grade of extraction, carry out the second-order separation, 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.
2. by the method for preparing food grade lutein ester claimed in claim 1, it is characterized in that: the extraction time of every one-level is 1～2h, every flash trapping stage time is 1～2h.
3. by the method for preparing food grade lutein ester claimed 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 medicinal extract is placed in and in vacuum degasser, removes smell; When extraction, should first extraction kettle temperature be increased to 55～65 DEG C, then medicinal extract is packed in still, open air valve door, make whole extracting system pressure equilibrium, and keep 30min, then start pressure extraction.
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| CN112619202B (en) * | 2020-12-24 | 2022-04-12 | 晨光生物科技集团股份有限公司 | Industrial method for preparing food-grade lutein |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4048203A (en) * | 1976-12-06 | 1977-09-13 | Thomas Philip | Purification of lutein-fatty acid esters from plant materials |
| CN1771919A (en) * | 2005-10-28 | 2006-05-17 | 江苏瑞迪生科技有限公司 | Compound soft lutein capsule and its prepn process |
| CN1800325A (en) * | 2006-01-10 | 2006-07-12 | 中国农业大学 | Marigold lutein supercritical CO2 extraction method |
| CN101530447A (en) * | 2009-04-14 | 2009-09-16 | 中国农业大学 | Method for extracting oleoresin rich in lutein in marigold by Supercritical CO2 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101756168A (en) * | 2008-12-25 | 2010-06-30 | 中国科学院兰州化学物理研究所 | Calendula yellow pigment extraction method |
| CN101693683B (en) * | 2009-09-26 | 2012-06-27 | 邯郸市中进天然色素有限公司 | Method for preparing high-purity lutein extract from common lutein extract |
| CN102010357A (en) * | 2010-10-25 | 2011-04-13 | 青岛赛特香料有限公司 | Method for refining lutein by supercritical extraction |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4048203A (en) * | 1976-12-06 | 1977-09-13 | Thomas Philip | Purification of lutein-fatty acid esters from plant materials |
| CN1771919A (en) * | 2005-10-28 | 2006-05-17 | 江苏瑞迪生科技有限公司 | Compound soft lutein capsule and its prepn process |
| CN1800325A (en) * | 2006-01-10 | 2006-07-12 | 中国农业大学 | Marigold lutein supercritical CO2 extraction method |
| CN101530447A (en) * | 2009-04-14 | 2009-09-16 | 中国农业大学 | Method for extracting oleoresin rich in lutein in marigold by Supercritical CO2 |
Non-Patent Citations (4)
| Title |
|---|
| Optimization of supercritical carbon dioxide extraction of lutein esters from marigold (Tagetes erecta L.) with vegetable oils as continuous co-solvents;Yanxiang Gao等;《Separation and Purification Technology》;20091124;第71卷;第214-219页 * |
| Sandra Naranjo-Modad等.Solubility of Purified Lutein Diesters Obtained from Tagetes erecta in Supercritical CO2 and the Effect of Solvent Modifiers.《J. Agric. Food Chem.》.2000,第48卷 |
| Solubility of Purified Lutein Diesters Obtained from Tagetes erecta in Supercritical CO2 and the Effect of Solvent Modifiers;Sandra Naranjo-Modad等;《J. Agric. Food Chem.》;20001021;第48卷;第5640-5642页 * |
| Yanxiang Gao等.Optimization of supercritical carbon dioxide extraction of lutein esters from marigold (Tagetes erecta L.) with vegetable oils as continuous co-solvents.《Separation and Purification Technology》.2009,第71卷 |
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Denomination of invention: Method for preparing food-grade lutein ester Effective date of registration: 20200117 Granted publication date: 20140730 Pledgee: CITIC Futong Finance Leasing Co., Ltd. Kunming Branch Pledgor: Yunnan Honglv Capsaicin Co., Ltd. Registration number: Y2020530000001 |
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