CN102757372A - Method for preparing food-grade lutein ester - Google Patents
Method for preparing food-grade lutein ester Download PDFInfo
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- CN102757372A CN102757372A CN2012102678725A CN201210267872A CN102757372A CN 102757372 A CN102757372 A CN 102757372A CN 2012102678725 A CN2012102678725 A CN 2012102678725A CN 201210267872 A CN201210267872 A CN 201210267872A CN 102757372 A CN102757372 A CN 102757372A
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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 the lutein ester that organic solvent extractionprocess is prepared carries out deep processing, makes lutein ester be applied to food, medicine and nutritious prod etc.
Background technology
Xenthophylls is that a kind of oxygen containing type trailing plants L recklessly is plain, general being present in banana, Kiwifruit, corn and the Flower of Aztec Marigold, have different physiological roles, as anti-oxidant, eliminate functions such as 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 global cultivated area.Extract lutein ester medicinal extract with organic solvent method from Flower of Aztec Marigold and formed industrialization; But contain the fatty acid ester more than 60% in the medicinal extract; Lutein content has only about 15%, because organic solvent and fatty ester combine, low temperature commonly used at present vacuumizes the method for removing solvent; Do not reach food grade to the 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." method of the refining xenthophylls of a kind of supercritical extraction " (application number 201010517156.9) discloses the method for removing the Flos Tagetis Erectae extract peculiar smell in the Chinese patent document; And in overcritical processing and refining process, adding new organic solvent-acetone and propyl carbinol again; Though this method can be removed the Flos Tagetis Erectae extract peculiar smell; And improve the content of xenthophylls to a certain extent, but still residual a large amount of solvent in the product also is difficult to reach the food grade standard.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method for preparing the food grade lutein ester, can improve lutein content, effectively removes impurity free fatty acids, unpleasant odor and residual solvent in the product, reaches food security standard.
Realize that the technical scheme that the object of the invention is taked is: with lutein ester medicinal extract is raw material, supercritical CO
2For the extraction fluid, carry out three grades of extractions, the 2nd, 3 grades of extractions of last round-robin fluid is used as the 1st, 2 grades of extractions of next round-robin fluid, and fresh supercritical CO is used in each round-robin 3rd level extraction
2Fluid, extracting pressure and temperature are respectively 18～28MPa, 55～65 ℃; Carry out secondary after every grade of extraction and separate, first step separating pressure and temperature are respectively 6～10MPa and 30～40 ℃, and second stage separating pressure and temperature are respectively 4～6MPa and 20～30 ℃.
In above-mentioned operation, the extraction time of each grade is 1～2h, and each grade disengaging time is 1～2h.
Lutein ester medicinal extract should carry out heating in water bath earlier before extraction, temperature is 50～60 ℃, and under agitation keeps 30～120 min, perhaps medicinal extract is placed to remove smell in the vacuum degasser; Should earlier the extraction kettle temperature be increased to 55～65 ℃ during extraction, again medicinal extract be packed in the still, open the air valve door, make whole extracting system pressure equilibrium, and keep 30min, begin pressure extraction then.
The useful technique effect of the present invention is following.
(1) lutein content can be increased to 240～280g/kg in the product from about 150g/kg, on average can reach 260g/kg, and lutein content has on average improved 67%, and the active substance recovery reaches more than 90%;
(2) the total residual solvent in the product can be reduced to below the 50ppm from 20000ppm, reaches the requirement of food security standard;
(3) can effectively remove impurity free fatty acids and unpleasant odor in the product, acid value drops to about 10 from 40, more helps the storage and the use of product;
(4) present method is not introduced other organic solvent, and is good to environment.
The present invention uses supercritical extraction technique, adds the counter-current extraction scheme, is divided into three grades to supercutical fluid; Parameters such as variation extraction pressure and temperature can be separated and removed some free fatty acids and organic residual solvent, remove the taste of lutein extract; The more effective content that improves xenthophylls; Do not add additional organic solvents, extend the shelf life, reach the food grade standard.
Embodiment
Embodiment 1
1, get marigold flower and slightly carry lutein extract 120g and place beaker, heating in water bath to 60 ℃ also keeps 30min;
2, open overcritical equipment, treat that the extraction kettle temperature is increased to 55 ℃ after, medicinal extract is transferred in the extraction kettle, build plug, open the air valve door, make whole extracting system pressure equilibrium, and keep 30min, put into the 2nd grade of supercritical CO of last round-robin
2The extraction fluid begins pressure extraction then;
3, extraction conditions is: extracting pressure 26Mpa, and 60 ℃ of extraction temperature, first step separating pressure and temperature are respectively 8MPa and 40 ℃, and second stage separating pressure and temperature are respectively 5MPa and 30 ℃;
4, behind the extraction 2h, emit separated product, and be replaced with last round-robin 3rd level supercritical CO
2The extraction fluid; Keep the constant continuation extraction of last step extraction conditions 1h then, emit separated product, and change fresh supercritical CO
2The extraction fluid; Continue to keep the constant continuation extraction of extraction conditions 1h again, shut down release, from separating still, take out extraction product food grade lutein ester 62.4g;
5, according to corresponding method of detection in the GB, detect lutein content, Determination of Residual Organic Solvents and free fatty acid content in raw material marigold flower medicinal extract and the extraction product food grade lutein ester, detected result is as shown in table 1.
In the step 1, if the medicinal extract smell is overweight, can prolong soaking time to 1～2h as stated, words with good conditionsi can install whipping appts additional, perhaps medicinal extract are placed in the vacuum degasser.
Each the 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 place beaker, heating in water bath to 60 ℃ also keeps 30min;
2, open overcritical equipment, treat that the extraction kettle temperature is increased to 60 ℃ after, medicinal extract is transferred in the extraction kettle, build plug, open the air valve door, make whole extracting system pressure equilibrium, and keep 30min, put into the 2nd grade of supercritical CO of last round-robin
2The extraction fluid begins pressure extraction then;
3, extraction conditions is: extracting pressure 25Mpa, and 60 ℃ of extraction temperature, first step separating pressure and temperature are respectively 10MPa and 36 ℃, and second stage separating pressure and temperature are respectively 5MPa and 26 ℃;
4, behind the extraction 2h, emit separated product, and be replaced with last round-robin 3rd level supercritical CO
2The extraction fluid; Keep the constant continuation extraction of extraction conditions 2h then, emit separated product, and change fresh supercritical CO
2The extraction fluid; Continue to keep the constant continuation extraction of extraction conditions 2h again, shut down release, from separating still, take out extraction product food grade lutein ester 58.3g;
5, according to corresponding method of detection in the GB, detect lutein content, Determination of Residual Organic Solvents and free fatty acid content in raw material marigold flower medicinal extract and the extraction product food grade lutein ester, detected result is as shown in table 2.
Each the 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 place beaker, heating in water bath to 65 ℃ also keeps 30min;
2, open overcritical equipment, treat that the extraction kettle temperature is increased to 65 ℃ after, medicinal extract is transferred in the extraction kettle, build plug, open the air valve door, make whole extracting system pressure equilibrium, and keep 30min, put into the 2nd grade of supercritical CO of last round-robin
2The extraction fluid begins pressure extraction then;
3, extraction conditions is: extracting pressure 20Mpa, and 65 ℃ of extraction temperature, first step separating pressure and temperature are respectively 8MPa and 40 ℃, and second stage separating pressure and temperature are respectively 4MPa and 30 ℃;
4, behind the extraction 2h, emit separated product, and be replaced with last round-robin 3rd level supercritical CO
2The extraction fluid; Keep the constant continuation extraction of extraction conditions 2h then, emit separated product, and change fresh supercritical CO
2The extraction fluid; Continue to keep the constant continuation extraction of extraction conditions 1h again, shut down release, from separating still, take out extraction product food grade lutein ester 55.7g;
5, according to corresponding method of detection in the GB, detect lutein content, Determination of Residual Organic Solvents and free fatty acid content in raw material marigold flower medicinal extract and the extraction product food grade lutein ester, detected result is as shown in table 3.
Each the index contrast of table 3 marigold flower medicinal extract and food grade lutein ester
。
Claims (3)
1. method for preparing the food grade lutein ester, it is characterized in that: with lutein ester medicinal extract is raw material, supercritical CO
2For the extraction fluid, carry out three grades of extractions, the 2nd, 3 grades of extractions of last round-robin fluid is used as the 1st, 2 grades of extractions of next round-robin fluid, and fresh supercritical CO is used in each round-robin 3rd level extraction
2Fluid, extracting pressure and temperature are respectively 18～28MPa, 55～65 ℃; Carry out secondary after every grade of extraction and separate, first step separating pressure and temperature are respectively 6～10MPa and 30～40 ℃, and second stage separating pressure and temperature are respectively 4～6MPa and 20～30 ℃.
2. by the described method for preparing the food grade lutein ester of claim 1, it is characterized in that: the extraction time of each grade is 1～2h, and each grade disengaging time is 1～2h.
3. by the described method for preparing the food grade lutein ester of claim 2; It is characterized in that: lutein ester medicinal extract carries out heating in water bath earlier before extraction; Temperature is 50～60 ℃, and under agitation keeps 30～120 min, perhaps medicinal extract is placed to remove smell in the vacuum degasser; Should earlier the extraction kettle temperature be increased to 55～65 ℃ during extraction, again medicinal extract be packed in the still, open the air valve door, make whole extracting system pressure equilibrium, and keep 30min, begin pressure extraction then.
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| CN201210267872.5A CN102757372B (en) | 2012-07-31 | 2012-07-31 | Method for preparing food-grade lutein ester |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112619202A (en) * | 2020-12-24 | 2021-04-09 | 晨光生物科技集团股份有限公司 | Industrial method for preparing food-grade lutein |
Citations (7)
| 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 |
| CN101693683A (en) * | 2009-09-26 | 2010-04-14 | 美科尔(河北)生物科技有限公司 | Method for preparing high-purity lutein extract from common lutein extract |
| 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 |
| 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 |
-
2012
- 2012-07-31 CN CN201210267872.5A patent/CN102757372B/en active Active
Patent Citations (7)
| 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 |
| 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 |
| 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 |
| CN101693683A (en) * | 2009-09-26 | 2010-04-14 | 美科尔(河北)生物科技有限公司 | 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 |
Non-Patent Citations (2)
| Title |
|---|
| 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.》, vol. 48, 21 October 2000 (2000-10-21) * |
| 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》, vol. 71, 24 November 2009 (2009-11-24) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112619202A (en) * | 2020-12-24 | 2021-04-09 | 晨光生物科技集团股份有限公司 | Industrial method for preparing food-grade lutein |
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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 |