CN101381274B - Method for removing dissolvent residual from lycopene oleoresin - Google Patents
Method for removing dissolvent residual from lycopene oleoresin Download PDFInfo
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- CN101381274B CN101381274B CN2008102243074A CN200810224307A CN101381274B CN 101381274 B CN101381274 B CN 101381274B CN 2008102243074 A CN2008102243074 A CN 2008102243074A CN 200810224307 A CN200810224307 A CN 200810224307A CN 101381274 B CN101381274 B CN 101381274B
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Abstract
The invention discloses a method for removing a residual solvent in a lycopene oil resin, which belongs to the technical field of separating and purifying the residual solvent in the food processing. An extraction of the lycopene oil resin to be treated is added into a material bottle; after checking and confirming of an airtight system, a vacuum pump is started to degas the material; after a numerical value of a vacuum degree is stabilized, the procedure of degassing is completed. Scraper rotational speed, feeding velocity, pressure of molecular distillation, distillation temperature and condensing temperature are set, a material valve is opened to allow the material to flow into a distillation body so as to undergo the molecular distillation, impurities contained in the oil resin enter a distillate component, and the remaining residue component, namely the purified lycopene oil resin is collected. Because the molecular distillation technology is adopted, the method can not only remove the residual solvent in the lycopene oil resin and reduce contents of other impurities in the oil resin, but also can improve safety of the lycopene oil resin and density of lycopene, thereby contributing to strengthening the activity of the lycopene.
Description
Technical field
The invention belongs to dissolvent residual separating and purifying technology field in the food-processing, particularly a kind of method that removes dissolvent residual in the lycopene oleo-resinous.
Background technology
Lyeopene be a kind of are a kind of of carrotenoid by 11 conjugated double bonds and 2 straight chain type hydrocarbon polymers that unconjugated double bond is formed, dissolve in fat and lipoid, take on a red color.Lyeopene has physiologic function widely, comprise anti-oxidant, enhance immunity power, anticancer, effectively stop low-density lipoprotein oxidation, anti-ageing, prevent optical radiation damage or the like.
At present, Lyeopene mainly is to adopt organic solvent extraction such as ETHYLE ACETATE, normal hexane, passes through vacuum concentration then, obtains the crude extract of Lyeopene---lycopene oleo-resinous.Because it is residual wherein to contain certain amount of organic solvent, thereby HUMAN HEALTH is caused potential hazard.
Adopt the conventional as easy as rolling off a log destruction of causing Lyeopene of thermal distillation that adds, and organic solvent residual can not be removed fully.At present, the report that adopts supercritical carbon dioxide fluid to remove dissolvent residual in the lycopene oleo-resinous is arranged, but this method still can not thoroughly be removed dissolvent residual.Molecular distillation technique is short-path distillation again; It is a kind of new high-efficiency liquid liquid stripping technique of gentleness; Obtained fast development in recent decades, particularly more and more praised highly the theory of green food and back to nature along with countries in the world, this eco-friendly pure Physical Separation Technology gains great popularity more.Molecular distillation technique is to utilize the difference of molecular motion mfp and the separation that realizes mixture, is particularly suitable for concentrating, purifying or separation of high molecular weight, high boiling point, full-bodied material and the organic mixture of poor heat stability and separating of natural product.It is widely used in industries such as food, medicine, daily use chemicals.Residual solvent and the raising content of lycopene removed in the lycopene oleo-resinous about the applied molecular distillation technique at home and abroad also do not appear in the newspapers.
Exist chemical solvents residual in the lycopene oleo-resinous that the organic solvent extraction method that generally adopts now obtains, these chemical solventss all have neurotoxicity or potential carinogenicity, and HUMAN HEALTH is had potential harm, have limited the widespread use of Lyeopene.Adopt the conventional as easy as rolling off a log destruction of causing Lyeopene of thermal distillation that adds, and organic solvent residual can not be removed fully.At present, the report that adopts supercritical carbon dioxide fluid to remove dissolvent residual in the lycopene oleo-resinous is also arranged, but this method still can not thoroughly be removed dissolvent residual.
Summary of the invention
The purpose of this invention is to provide a kind of method that removes dissolvent residual in the lycopene oleo-resinous, it is characterized in that, step does,
(1) in bottle for material, adds pending lycopene oleo-resinous extract;
(2) inspection affirmation system airtight after, the open vacuum pump carries out the material degassing, treat that vacuum values is stable after, degassing process is accomplished;
(3) setting scraper plate rotating speed 100～150r/min, feeding rate 10～20ml/min, short-path distillation pressure are 0.5～8Pa, 85～130 ℃ of distillation temperatures, water cycle cooling; Condensing temperature need be lower than at least 40 ℃ of short-path distillation temperature; Open Material valve, material flows into distillated subject, carries out short-path distillation; Impurities gets in the overhead product component in the oleo-resinous, collects the lycopene oleo-resinous after remaining residue component is purifying.
Beneficial effect of the present invention is:
(1) conventional distillation is compared; Adopt residual solvent and partial impurities in the molecular distillation technique separation removal lycopene oleo-resinous extract; Can not only improve security of products and active constituent content; And the Lyeopene that can avoid thermo-sensitivity and easy oxidation in the short-path distillation process not recurring structure change, keep its biological activity.Have advantages such as product quality height, energy consumption are little, easy handling.
(2) molecular distillation technique is a kind of high-new stripping technique, has that service temperature is low, low, the heated time of distillation pressure is short, characteristics such as separation degree and product yield height, is specially adapted to the separation of high boiling point, thermo-sensitivity and readily oxidizable substance.
(3) the present invention adopts molecular distillation technique can not only remove the residual solvent in the lycopene oleo-resinous; Can reduce simultaneously the content of other impurity in the oleo-resinous; Can improve the security of lycopene oleo-resinous, can improve the wherein concentration of Lyeopene again, help strengthening its activity.
Embodiment
Below in conjunction with embodiment the present invention is described further:
Embodiment 1
A kind of method that removes dissolvent residual in the lycopene oleo-resinous is a raw material with the lycopene oleo-resinous, and wherein the content of Lyeopene is 7.23%, normal hexane content 2%, and ethyl acetate content 0.8%, step do,
(1) in bottle for material, adds pending lycopene oleo-resinous extract 50ml;
(2) inspection affirmation system airtight after, the open vacuum pump carries out the material degassing, treat that vacuum values is stable after, degassing process is accomplished;
(3) setting scraper plate rotating speed 96r/min, feeding rate 10ml/min, short-path distillation pressure are 6.5Pa, 85 ℃ of distillation temperatures, water cycle cooling; 40 ℃ of condensing temperatures; Open Material valve, material flows into distillated subject, carries out short-path distillation; Impurities gets in the overhead product component in the oleo-resinous, collects the lycopene oleo-resinous after remaining residue component is purifying.
The content of Lyeopene is 9.06% to use efficient liquid-phase chromatography method to record wherein, and normal hexane is 10ppm to use gas chromatography to record wherein, and ETHYLE ACETATE is 19ppm, and the clearance of residual solvent is more than 99%, and Lyeopene purity increases by 25%.
Embodiment 2
A kind of method that removes dissolvent residual in the lycopene oleo-resinous is a raw material with the lycopene oleo-resinous, and wherein the content of Lyeopene is 5.69%, ethanol content 0.6%, and ethyl acetate content 0.4%, step do,
(1) in bottle for material, adds pending lycopene oleo-resinous extract 50ml;
(2) inspection affirmation system airtight after, the open vacuum pump carries out the material degassing, treat that vacuum values is stable after, degassing process is accomplished;
(3) setting scraper plate rotating speed 96r/min, feeding rate 12ml/min, short-path distillation pressure are 2.5Pa, 100 ℃ of distillation temperatures, water cycle cooling; 40 ℃ of condensing temperatures; Open Material valve, material flows into distillated subject, carries out short-path distillation; Impurities gets in the overhead product component in the oleo-resinous, collects the lycopene oleo-resinous after remaining residue component is purifying.
The content of Lyeopene is 7.75% to use efficient liquid-phase chromatography method to record wherein, and ethanol is 5ppm to use gas chromatography to record wherein, and ETHYLE ACETATE is 24ppm, and the clearance of residual solvent is more than 99%, and Lyeopene purity increases by 36%.
Embodiment 3
A kind of method that removes dissolvent residual in the lycopene oleo-resinous is a raw material with the lycopene oleo-resinous, and wherein the content of Lyeopene is 6.14%, ethanol content 1%, and ethyl acetate content 0.9%, step do,
(1) in bottle for material, adds pending lycopene oleo-resinous extract 50ml;
(2) inspection affirmation system airtight after, the open vacuum pump carries out the material degassing, treat that vacuum values is stable after, degassing process is accomplished;
(3) setting scraper plate rotating speed 110r/min, feeding rate 15ml/min, short-path distillation pressure are 0.5Pa, 85 ℃ of distillation temperatures, water cycle cooling; 40 ℃ of condensing temperatures; Open Material valve, material flows into distillated subject, carries out short-path distillation; Impurities gets in the overhead product component in the oleo-resinous, collects the lycopene oleo-resinous after remaining residue component is purifying.
The content of Lyeopene is 7.96% to use efficient liquid-phase chromatography method to record wherein, and ethanol is 5ppm to use gas chromatography to record wherein, and ETHYLE ACETATE is 6ppm, and the clearance of residual solvent is more than 99%, and Lyeopene purity increases by 30%.
Claims (1)
1. a method that removes dissolvent residual in the lycopene oleo-resinous is characterized in that, step does,
(1) in bottle for material, adds pending lycopene oleo-resinous extract;
(2) inspection affirmation system airtight after, the open vacuum pump carries out the material degassing, treat that vacuum values is stable after, degassing process is accomplished;
(3) setting scraper plate rotating speed 100～150r/min, feeding rate 10～20ml/min, short-path distillation pressure are 0.5～8Pa, 85～130 ℃ of distillation temperatures, water cycle cooling; Condensing temperature need be lower than at least 40 ℃ of short-path distillation temperature; Open Material valve, material flows into distillated subject, carries out short-path distillation; Impurities gets in the overhead product component in the oleo-resinous, collects the lycopene oleo-resinous after remaining residue component is purifying.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008102243074A CN101381274B (en) | 2008-10-16 | 2008-10-16 | Method for removing dissolvent residual from lycopene oleoresin |
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| CN2008102243074A CN101381274B (en) | 2008-10-16 | 2008-10-16 | Method for removing dissolvent residual from lycopene oleoresin |
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| CN101381274A CN101381274A (en) | 2009-03-11 |
| CN101381274B true CN101381274B (en) | 2012-05-30 |
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| CN105778555B (en) * | 2014-12-26 | 2017-05-31 | 新疆西域果宝生物科技有限公司 | A kind of preparation method of simple lycopene oleoresin precipitation purification |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1234671C (en) * | 2004-08-11 | 2006-01-04 | 中国林业科学研究院林产化学工业研究所 | Molecular distillation purification method of polyprenol |
| CN1289609C (en) * | 2005-05-25 | 2006-12-13 | 中国科学院新疆理化技术研究所 | Method for preparing crystal of lycopene and concentrate |
| WO2008102032A1 (en) * | 2007-02-22 | 2008-08-28 | Universidad De Cordoba | Method for obtaining squalene |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1234671C (en) * | 2004-08-11 | 2006-01-04 | 中国林业科学研究院林产化学工业研究所 | Molecular distillation purification method of polyprenol |
| CN1289609C (en) * | 2005-05-25 | 2006-12-13 | 中国科学院新疆理化技术研究所 | Method for preparing crystal of lycopene and concentrate |
| WO2008102032A1 (en) * | 2007-02-22 | 2008-08-28 | Universidad De Cordoba | Method for obtaining squalene |
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