CN1545914A - Production method of natural lycopene oleoresin and natural lycopene crystallisate - Google Patents
Production method of natural lycopene oleoresin and natural lycopene crystallisate Download PDFInfo
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- CN1545914A CN1545914A CNA2003101241596A CN200310124159A CN1545914A CN 1545914 A CN1545914 A CN 1545914A CN A2003101241596 A CNA2003101241596 A CN A2003101241596A CN 200310124159 A CN200310124159 A CN 200310124159A CN 1545914 A CN1545914 A CN 1545914A
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- organic solvent
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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 process for producing natural tomatine oleoresin and natural tomatine crystallization substance which comprises, lixiviating catsup with organic solvent, separating and reclaiming organic solvent, removing residual organic solvent by carbon dioxide supercritical method, thus obtaining preliminary level or top-quality level tomatine oleoresin.
Description
Technical field
The present invention relates to put forward production methods of lycopene from tomato, is the production method of a kind of natural lycopene oleo-resinous and natural lycopene crystallisate.
Background technology
Natural lycopene is a kind of in the carotenoid, its antioxidant property is 100 times of vitamin-E, the sickness rate that can suppress multiple cancer, the inducing cell gap junction communication, remove free radical, have very high pharmaceutical use, nourishing function will be widely used in medicines and health protection, makeup, food service industry.
The tomato-sauce content of lycopene height that Xinjiang produces, low mold count, the output height, be subjected to the impact of international market price sales volume too big as the Xinjiang tomato-sauce industry of replenishing the status on the world market, the tomato-sauce sales volume in the time Xinjiang of world's tomato good harvest descends, price glides, and the incident that thousands of tons of tomato-sauce is toppled over Gobi desert once took place.
Chinese patent application number is that 00128226.3 patent documentation discloses the method that a kind of tomato-sauce is produced crystalline lycopene and/or lycopene oleo-resinous, and it provides a tomato deep-processing method; But, because this method production process complexity, investment is big, extraction yield is low, therefore is unfavorable for industrialization.
Summary of the invention
The invention provides the production method of a kind of natural lycopene oleo-resinous and natural lycopene crystallisate, its production method is easy and help industrialization production.
One of technical scheme of the present invention is achieved like this: a kind of production method of natural lycopene oleo-resinous, and it carries out according to the following steps:
The first step is with organic solvent lixiviate tomato-sauce: 1 weight part tomato-sauce is joined 0.5 weight part to 3 weight part organic solvent, be heated with stirring under 30 ℃ to 60 ℃, keep separating obtaining vat liquor after 20 minutes to 50 minutes;
The second step Separation and Recovery organic solvent: 40 ℃ under 80 ℃, with organic solvent Separation and Recovery from the vat liquor that the first step obtains, and obtain the crude product lycopene oleo-resinous;
The 3rd step was slightly taken off residual organic solvent: the ethanolic soln of extraordinarily going into 80% to 99.9% concentration in the crude product lycopene oleo-resinous of the second step gained by 0.3 to 2 of its weight, stir down at 40 ℃ to 80 ℃, and vacuum filtration 0.25 hour to 2 hours, obtain the primary product lycopene oleo-resinous.
Above-mentioned primary product lycopene oleo-resinous can be carried out CO 2 supercritical and remove residual organic solvent, obtain the elaboration lycopene oleo-resinous, its processing parameter is: temperature is 25 ℃ to 40 ℃, and pressure is 6Mpa to 12Mpa, and the time is 20 minutes to 120 minutes.
Two of technical scheme of the present invention is achieved like this: a kind of production method of natural lycopene crystallisate, and it carries out according to the following steps:
The first step is with organic solvent lixiviate tomato-sauce: 1 weight part tomato-sauce is joined 0.5 weight part to 3 weight part organic solvent, be heated with stirring under 30 ℃ to 60 ℃, keep separating obtaining vat liquor after 20 minutes to 50 minutes;
The second step Separation and Recovery organic solvent: 40 ℃ under 80 ℃, with organic solvent Separation and Recovery from the vat liquor that the first step obtains, and obtain the crude product lycopene oleo-resinous;
The 3rd goes on foot coarse crystallization: after the second crude product lycopene oleo-resinous that goes on foot gained is concentrated, under 0 to-20 ℃, carry out crystallization, separate mother liquor and obtain crude product crystal of lycopene thing;
The 4th step was slightly taken off residual organic solvent: the ethanolic soln that adds 80% to 99.9% concentration in the crude product crystal of lycopene thing of the 3rd step gained by 0.3 to 2 times of weight of its weight, stir down at 40 ℃ to 80 ℃, and vacuum filtration 0.25 hour to 2 hours, obtain primary product crystal of lycopene thing.
Above-mentioned primary product crystal of lycopene thing can be carried out CO 2 supercritical and remove residual organic solvent, obtain elaboration crystal of lycopene thing, its processing parameter is: temperature is 25 ℃ to 40 ℃, and pressure is 6Mpa to 12Mpa, and the time is 20 minutes to 120 minutes.
Above-mentioned organic solvent is selected a kind of organic solvent or the mixture of organic solvent more than two kinds in varsol, low boiling ester, ether, the letones for use.
Above-mentioned organic solvent is selected a kind of organic solvent or the mixture of organic solvent more than two kinds in ethane, molten kerosene, ethyl acetate, the acetone for use.
Above-mentioned tomato-sauce can select that solid content is 20% to 50%, natural lycopene content is the tomato-sauce of 30mg/100g to 180mg/100g for use.
The advantage that the present invention has is: production process is easy, invest little, the extraction yield height, Determination of Residual Organic Solvents is little, helps large-scale industrial production.
Embodiment
The present invention is not subjected to the restriction of following embodiment, can determine concrete embodiment according to the technical scheme and the practical situation of the invention described above.
Embodiment 1, and the production method of this natural lycopene oleo-resinous is carried out according to the following steps:
The first step is with organic solvent lixiviate tomato-sauce: 1 weight part tomato-sauce is joined 0.5 weight part or 1.5 weight parts or 3 weight part organic solvents, be heated with stirring under 30 ℃ or 45 ℃ or 60 ℃, keep separating obtaining vat liquor after 20 minutes or 35 minutes or 50 minutes;
The second step Separation and Recovery organic solvent: under 40 ℃ or 50 ℃ or 60 ℃ or 70 ℃ or 80 ℃,, and obtain the crude product lycopene oleo-resinous with organic solvent Separation and Recovery from the vat liquor that the first step obtains;
The 3rd step was slightly taken off residual organic solvent: in the crude product lycopene oleo-resinous of the second step gained by 0.3 times or 2 ethanolic soln of extraordinarily going into 80% or 85% or 90% or 99% concentration of its weight, stir down at 40 ℃ or 50 ℃ or 60 ℃ or 70 ℃ or 80 ℃, and vacuum filtration 0.25 hour or 1 hour or 2 hours, obtain the primary product lycopene oleo-resinous.
Embodiment 2, the foregoing description 1 resulting primary product lycopene oleo-resinous is carried out CO 2 supercritical remove residual organic solvent, just obtain the elaboration lycopene oleo-resinous, its processing parameter is: temperature is 25 ℃ or 30 ℃ or 40 ℃, pressure is 6Mpa or 9Mpa or 12Mpa, and the time is 20 minutes or 40 minutes or 60 minutes or 80 minutes or 100 minutes or 120 minutes.Gained elaboration lycopene oleo-resinous is detected: its Determination of Residual Organic Solvents is less than 25ppm, and content of lycopene is 3-8%, and extraction yield is 75% to 85%.
Embodiment 3, and this natural lycopene crystalline production method is carried out according to the following steps:
The first step is with organic solvent lixiviate tomato-sauce: 1 weight part tomato-sauce is joined 0.5 weight part or 1.5 weight parts or 3 weight part organic solvents, be heated with stirring under 30 ℃ or 45 ℃ or 60 ℃, keep separating obtaining vat liquor after 20 minutes or 35 minutes or 50 minutes;
The second step Separation and Recovery organic solvent: under 40 ℃ or 50 ℃ or 60 ℃ or 70 ℃ or 80 ℃, with organic solvent Separation and Recovery from the vat liquor that the first step obtains, and obtain the crude product lycopene oleo-resinous;
The 3rd goes on foot coarse crystallization: after the second crude product lycopene oleo-resinous that goes on foot gained is concentrated, under 0 ℃ or-10 ℃ or-20 ℃, carry out crystallization, separate mother liquor and obtain crude product crystal of lycopene thing;
The 4th step was slightly taken off residual organic solvent: in the crude product crystal of lycopene thing of the 3rd step gained by 1 times or 2 ethanolic soln of extraordinarily going into 80% or 85% or 90% or 99.9% concentration of its weight, stir down at 40 ℃ or 50 ℃ or 60 ℃ or 70 ℃ or 80 ℃, and vacuum filtration 0.25 hour or 1 hour or 2 hours, obtain primary product crystal of lycopene thing.
Embodiment 4, the foregoing description 3 resulting primary product crystal of lycopene things are carried out CO 2 supercritical remove residual organic solvent, obtain elaboration crystal of lycopene thing, its processing parameter is: temperature is 25 ℃ or 30 ℃ or 40 ℃, pressure is 6Mpa or 9Mpa or 12Mpa, and the time is 20 minutes or 40 minutes or 60 minutes or 80 minutes or 100 minutes or 120 minutes.Gained elaboration crystal of lycopene thing is detected: its Determination of Residual Organic Solvents is less than 25ppm, and content of lycopene is 10% to 80% crystal of lycopene, extraction yield 75% to 85%.
In the foregoing description 1 and embodiment 2: organic solvent can be selected a kind of organic solvent or the mixture of organic solvent more than two kinds in varsol, low boiling ester, ether, the letones for use, organic solvent also can be selected a kind of organic solvent or the mixture of organic solvent more than two kinds in ethane, molten kerosene, ethyl acetate, the acetone for use, determines according to actual needs; Solid-liquid separation can adopt conventional separation method, as: filtering separation, centrifugation, membrane sepn; The Separation and Recovery of organic solvent can adopt thin-film evaporator to carry out; Concentration method can adopt conventional concentration method, as: evaporation concentration, thin film concentration, vacuum concentration; Tomato-sauce can select that solid content is 20% to 50%, natural lycopene content is the tomato-sauce of 30mg/100g to 180mg/100g for use.
Claims (10)
1, a kind of production method of natural lycopene oleo-resinous is characterized in that carrying out according to the following steps:
The first step is with organic solvent lixiviate tomato-sauce: 1 weight part tomato-sauce is joined 0.5 weight part to 3 weight part organic solvent, be heated with stirring under 30 ℃ to 60 ℃, keep separating obtaining vat liquor after 20 minutes to 50 minutes;
The second step Separation and Recovery organic solvent: 40 ℃ under 80 ℃, with organic solvent Separation and Recovery from the vat liquor that the first step obtains, and obtain the crude product lycopene oleo-resinous;
The 3rd step was slightly taken off residual organic solvent: the ethanolic soln of extraordinarily going into 80% to 99.9% concentration in the crude product lycopene oleo-resinous of the second step gained by 0.3 to 2 of its weight, stir down at 40 ℃ to 80 ℃, and vacuum filtration 0.25 hour to 2 hours, obtain the primary product lycopene oleo-resinous.
2, the production method of natural lycopene oleo-resinous according to claim 1, it is characterized in that above-mentioned primary product lycopene oleo-resinous is carried out CO 2 supercritical removes residual organic solvent, obtain the elaboration lycopene oleo-resinous, its processing parameter is: temperature is 25 ℃ to 40 ℃, pressure is 6Mpa to 12Mpa, and the time is 20 minutes to 120 minutes.
3, the production method of natural lycopene oleo-resinous according to claim 1 and 2 is characterized in that organic solvent selects a kind of organic solvent or the mixture of organic solvent more than two kinds in varsol, low boiling ester, ether, the letones for use.
4, the production method of natural lycopene oleo-resinous according to claim 3 is characterized in that organic solvent selects a kind of organic solvent or the mixture of organic solvent more than two kinds in ethane, molten kerosene, ethyl acetate, the acetone for use.
5,, it is characterized in that tomato-sauce selects that solid content is 20% to 50%, natural lycopene content is the tomato-sauce of 30mg/100g to 180mg/100g for use according to the production method of claim 1 or 2 or 4 described natural lycopene oleo-resinouss.
6, a kind of natural lycopene crystalline production method is characterized in that carrying out according to the following steps:
The first step is with organic solvent lixiviate tomato-sauce: 1 weight part tomato-sauce is joined 0.5 weight part to 3 weight part organic solvent, be heated with stirring under 30 ℃ to 60 ℃, keep separating obtaining vat liquor after 20 minutes to 50 minutes;
The second step Separation and Recovery organic solvent: 40 ℃ under 80 ℃, with organic solvent Separation and Recovery from the vat liquor that the first step obtains, and obtain the crude product lycopene oleo-resinous;
The 3rd goes on foot coarse crystallization: after the second crude product lycopene oleo-resinous that goes on foot gained is concentrated, under 0 to-20 ℃, carry out crystallization, separate mother liquor and obtain crude product crystal of lycopene thing;
The 4th step was slightly taken off residual organic solvent: the ethanolic soln that adds 80% to 99.9% concentration in the crude product crystal of lycopene thing of the 3rd step gained by 0.3 to 2 times of weight of its weight, stir down at 40 ℃ to 80 ℃, and vacuum filtration 0.25 hour to 2 hours, obtain primary product crystal of lycopene thing.
7, the production method of natural lycopene oleo-resinous according to claim 6, it is characterized in that above-mentioned primary product crystal of lycopene thing is carried out CO 2 supercritical removes residual organic solvent, obtain elaboration crystal of lycopene thing, its processing parameter is: temperature is 25 ℃ to 40 ℃, pressure is 6Mpa to 12Mpa, and the time is 20 minutes to 120 minutes.
8,, it is characterized in that organic solvent selects a kind of organic solvent or the mixture of organic solvent more than two kinds in varsol, low boiling ester, ether, the letones for use according to the production method of claim 6 or 7 described natural lycopene oleo-resinouss.
9, the production method of natural lycopene oleo-resinous according to claim 8 is characterized in that organic solvent selects a kind of organic solvent or the mixture of organic solvent more than two kinds in ethane, molten kerosene, ethyl acetate, the acetone for use.
10,, it is characterized in that tomato-sauce selects that solid content is 20% to 50%, natural lycopene content is the tomato-sauce of 30mg/100g to 180mg/100g for use according to the production method of claim 6 or 7 or 9 described natural lycopene oleo-resinouss.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2003101241596A CN1545914A (en) | 2003-12-12 | 2003-12-12 | Production method of natural lycopene oleoresin and natural lycopene crystallisate |
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| CNA2003101241596A CN1545914A (en) | 2003-12-12 | 2003-12-12 | Production method of natural lycopene oleoresin and natural lycopene crystallisate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100341427C (en) * | 2005-03-16 | 2007-10-10 | 新疆生命红果蔬制品有限公司 | Emulsified lycopene and its preparing process |
| CN100357358C (en) * | 2005-11-30 | 2007-12-26 | 中国科学院新疆理化技术研究所 | Method for preparing licopin |
| CN101810225A (en) * | 2010-04-09 | 2010-08-25 | 新疆大学 | Method for producing lycopene oil resin and plant oil rich in lycopene |
-
2003
- 2003-12-12 CN CNA2003101241596A patent/CN1545914A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100341427C (en) * | 2005-03-16 | 2007-10-10 | 新疆生命红果蔬制品有限公司 | Emulsified lycopene and its preparing process |
| CN100357358C (en) * | 2005-11-30 | 2007-12-26 | 中国科学院新疆理化技术研究所 | Method for preparing licopin |
| CN101810225A (en) * | 2010-04-09 | 2010-08-25 | 新疆大学 | Method for producing lycopene oil resin and plant oil rich in lycopene |
| CN101810225B (en) * | 2010-04-09 | 2013-01-23 | 新疆大学 | Method for producing lycopene oil resin and plant oil rich in lycopene |
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