CN102924967B - Industrialization method for improving purity of lycopene oil resin - Google Patents
Industrialization method for improving purity of lycopene oil resin Download PDFInfo
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- CN102924967B CN102924967B CN201210446426.0A CN201210446426A CN102924967B CN 102924967 B CN102924967 B CN 102924967B CN 201210446426 A CN201210446426 A CN 201210446426A CN 102924967 B CN102924967 B CN 102924967B
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Abstract
The invention discloses an industrialization method for improving purity of lycopene oil resin. The method comprises process steps of (1) adding an alcohol solvent in the lycopene oil resin for evenly stirring to obtain mixed liquor; (2) adding an alkaline aqueous solution in the mixed liquor to stir, and neutralizing a fatty acid compound in the oil resin to obtain neutralization liquor; (3) adding an alkaline aqueous solution in the neutralization liquor to stir, and saponifying an oil compound in the neutralization liquor to obtain saponification liquor; and (4) adding an alcohol-water solution in the saponification liquor to stir, then adding 6# solvent naphtha, stewing and laying after evenly stirring, collecting a 6# solvent layer, concentrating and obtaining the lycopene oil resin with improved purity. The method firstly neutralizes long-chain fatty acid in the lycopene oil resin, then saponifies the oil, can effectively reduce intensity of saponification, reduces packing of produced saponin on lycopene and obviously improves yiels. The method is simple in process and strong in maneuverability, the yield of the lycopene is higher than 90%, and obtained products are stable in state.
Description
Technical field
The present invention relates to the method for purification of a Plant Extracts, especially a kind of industrial method improving lycopene oleo-resinous purity.
Background technology
Lyeopene is very wide in distributed in nature, and in the red plants of maturation, content is higher, as tomato, watermelon, Radix Dauci Sativae, grape, red grapefruit, strawberry, citrus etc.Its molecular formula is C
40h
56molecular weight is 536.85, it is the one of total carotinoid, in all carotenoid, it has strong elimination singlet oxygen and eliminates the function of free radical, it is 2 times of carotene to the elimination function of singlet oxygen, 100 times of vitamin-E, in removing human body " sources of ten thousand diseases " free radical, the effect of Lyeopene is more powerful than β-carotene.2003, U.S.'s Time was listed in Lyeopene first of " contributing maximum food to human health ", and therefore Lyeopene is also called as " gold in plant ".At present, Lyeopene is widely accepted in American-European, Japanese and China Hong Kong & Taiwan areas.To preventing and treating prostatosis, prostate cancer, lung cancer, cancer of the stomach, breast cancer have special effect, the diffusion of effective anticancer and copying, and has anti-cancer and cancer-preventing effect, simultaneously can Cell protection DNA from free radical damage, prevent cytopathy, sudden change, canceration; Containing powerful antioxidation biology active substance, can impel growth and the regeneration of cell, beautifying wrinkle-removing, delays senility, and maintains skin health, is described as " 21 century healthcare products new lover ".
Current domestic and international most of lycopene product is all that raw material extracts with tomato pulp, but owing to being subject to the impact of raw material tomato price, the production cost of Lyeopene is higher, causes the price of lycopene product to remain high always.In recent years, research shows in tomato skin also containing a large amount of Lyeopenes.Tomato in China skin resource is huge, and tomato skin produces the tankage of tomato-sauce, and price is very cheap, therefore utilizes tomato skin to extract Lyeopene and not only greatly can improve yield of lycopene, can also reduce the production cost of Lyeopene greatly.But in tomato cultivating process, only focus on the local flavor, sugariness, pulp proportion etc. of tomato at present, and ignore the cultivation of Natural Antioxidants " Lyeopene " wherein, cause the Lyeopene in tomato skin and pulp always not high.And in tomato-sauce production process, pulp is separated with pericarp and adopts cold stripping and hot soarfing two kinds of modes.Adopt cold strip, in tomato skin, original Lyeopene should not lose, and content is high; Adopt thermal stripping method, in tomato skin, original Lyeopene loss is more, and content is few.Adopt thermal stripping method to be the most frequently used method of current tomato-sauce manufacturing enterprise, be also the development trend that tomato-sauce is produced, this will reduce the content of Lyeopene in tomato skin greatly, makes original purity in tomato skin become less with regard to not high Lyeopene.These factors directly results in the purity not high (purity is 2 ~ 3%) extracting product lycopene oleo-resinous, cannot sell.
China Patent Publication No. CN 1965693A, title: a kind of method of purification of natural lycopene, the method dissolves Lyeopene with hot edible ethanol, then filters and obtains lycopene crystal.Although the lycopene crystal purity that this method obtains can reach 75 ~ 95%, to the ingredient requirement of Lyeopene also very high (15 ~ 25%); The yield of this method is not high yet simultaneously, only has about 50%; The lycopene oleo-resinous purity used in the market is generally between 5 ~ 10%, and also need oiling and other auxiliary materials to be become oleo-resinous if lycopene crystal will be applied, technique is more loaded down with trivial details.
China Patent Publication No. CN 1687239A, title: the preparation method of a kind of crystal of lycopene and enriched material thereof, the method neutralizes with acid after first carrying out saponification to raw material tomato sauce or tomato skin, adopt low mass molecule alcohol process again, then utilize organic solvent to extract solid part, refrigerate method acquisition lycopene crystal and the lycopene concentrates such as crystallization.This patent, compared with first extracting the method for Lyeopene resaponifying, has: 1), alkali number used is comparatively large, causes the wasting of resources; 2), need larger saponification equipment, processing power is limited, and production capacity is low; 3), due to the impact of plant cell wall, saponification effect is bad.In addition, this patent step is more, more loaded down with trivial details, is unfavorable for large-scale industrial production;
Summary of the invention
The technical problem to be solved in the present invention is to provide the industrial method that a kind of technique simply improves lycopene oleo-resinous purity, to obtain highly purified lycopene oleo-resinous.
For solving the problems of the technologies described above, the processing step that the present invention takes is: (1) adds alcoholic solvent in lycopene oleo-resinous, stirs, and obtains mixed solution;
(2) in mixed solution, add alkaline aqueous solution and stir, in and oleo-resinous in fatty acid compound, obtain neutralizer;
(3) in neutralizer, add alkaline aqueous solution and stir, saponification oil compounds wherein, obtains saponification liquor;
(4) in saponification liquor, add alcohol solution, stir; Then 6# solvent oil is added, stratification after stirring; Collect 6# solvent layer and concentrate, obtaining the lycopene oleo-resinous that purity improves.
Step of the present invention (2) the neutral and alkali aqueous solution is the aqueous solution of KOH or NaOH, and the mass percentage concentration of solution is 10 ~ 30%; Lycopene oleo-resinous: alkaline aqueous solution=1:0.1 ~ 0.3(W/W).Described neutralization reaction temperature is 40 ~ 45 DEG C; The used time that adds of alkaline aqueous solution is 10 ~ 20 minutes, continues reaction 5 ~ 10 minutes after adding.
Step of the present invention (3) the neutral and alkali aqueous solution is the aqueous solution of KOH or NaOH, and the mass percentage concentration of solution is 50 ~ 56%; Lycopene oleo-resinous: alkaline aqueous solution=1:0.6 ~ 1(W/W).Described saponification reaction temperature is 55 ~ 63 DEG C, and saponification time is 90 ~ 120 minutes.
In step of the present invention (1), at 40 ~ 45 DEG C, lycopene oleo-resinous and alcoholic solvent are stirred, lycopene oleo-resinous: alcoholic solvent=1:1 ~ 3(W:W).Described alcoholic solvent is one or more in methyl alcohol, ethanol, propyl alcohol and Virahol.
In described step (4), alcohol solution is the aqueous solution of methyl alcohol, ethanol, propyl alcohol and/or Virahol, and in solution, the concentration expressed in percentage by volume of alcohol is 50%, lycopene oleo-resinous: alcohol solution=1:1(V/V).In described step (4), stir 15 ~ 30 minutes after adding alcohol solution.In described step (4), 6# solvent oil: lycopene oleo-resinous=11 ~ 15:1(V/W).
The purity of the lycopene oleo-resinous in step of the present invention (1) is lower than 3%.
The technological principle of present method: adopt alcoholic solvent first to be disperseed by lycopene oleo-resinous, is beneficial to neutralize, the carrying out smoothly of saponification reaction; And then add the ratio of alcoholic solvent in alcohol solution adjustment solution, be beneficial to follow-up 6# solvent oil Lyeopene process and carry out smoothly.
Adopt the beneficial effect that produces of technique scheme to be: the product that (1) the present invention lower oleo-resinous product that cannot sell of purity can be made to be transformed into purity that national standard requires is qualified, purity brings up to more than 4 times.
(2) containing a large amount of greases and longer chain fatty acid in the lycopene oleo-resinous utilizing tomato skin to extract, the present invention first neutralizes resaponifying grease after longer chain fatty acid wherein, effectively can reduce the severe degree of saponification reaction, the Chinese honey locust reducing generation, to the parcel of Lyeopene, significantly improves yield.
(3) present invention process is simple, workable; Lyeopene yield is greater than 90%, and products obtained therefrom is in stable condition.
Embodiment
Below in conjunction with specific embodiment, the present invention is further detailed explanation.
Embodiment 1: the processing step of the industrial method of this raising lycopene oleo-resinous purity is as described below.
Taking 300 kilograms of Lyeopene purity is the lycopene oleo-resinous of 2.24%, adds the methanol solvate of 450 kilograms wherein, then stirs 40 minutes at 45 DEG C, makes it mix, obtain mixed solution; In mixed solution, slowly add the KOH aqueous solution of 35 kilograms of mass percent concentrations 30%, Keep agitation in adition process, adding the used time is 15 minutes, continues reaction 5 minutes after adding, and adds and maintains 45 DEG C with temperature in reaction process, obtain neutralizer; In neutralizer, add 180 kilograms of mass percent concentrations is the potassium hydroxide aqueous solution of 56%, and under the condition of 55 DEG C, saponification 120 minutes, obtains saponification liquor; In saponification liquor, add the methanol aqueous solution 300L of concentration of volume percent 50%, stir 30 minutes, then add 6# solvent oil 4500L, stir stratification after 30 minutes, obtain 6# solvent oil reservoir; Concentrated 6# solvent oil reservoir, can obtain the lycopene oleo-resinous 67.35 kilograms that purity is 9.13%, Lyeopene yield is 91.5%.
Embodiment 2: the processing step of the industrial method of this raising lycopene oleo-resinous purity is as described below.
Taking 300 kilograms of Lyeopene purity is the lycopene oleo-resinous of 1.97%, adds the alcohol solvent of 600 kilograms wherein, then stirs 40 minutes at 43 DEG C, makes it mix, obtain mixed solution; In mixed solution, slowly add the NaOH aqueous solution of 90 kilograms of 12wt% and stir, adding the used time is 20 minutes, continues reaction 10 minutes after adding, and adds and maintains 43 DEG C with temperature in reaction process, obtain neutralizer; In neutralizer, add the NaOH aqueous solution of 250 kilograms of 56wt%, under the condition of 60 DEG C, saponification 110 minutes, obtains saponification liquor; In saponification liquor, add the aqueous ethanolic solution 300L of 50vol%, stir 30 minutes, then add 6# solvent oil 3300L, stir stratification after 30 minutes, obtain 6# solvent oil reservoir; Concentrated 6# solvent oil reservoir, can obtain the lycopene oleo-resinous 66.13 kilograms that purity is 8.12%, Lyeopene yield is 90.86%.
Embodiment 3: the processing step of the industrial method of this raising lycopene oleo-resinous purity is as described below.
Taking 300 kilograms of Lyeopene purity is the lycopene oleo-resinous of 2.05%, adds the isopropanol solvent of 900 kilograms wherein, then stirs 40 minutes at 40 DEG C, makes it mix, obtain mixed solution; In the lycopene solution mixed, slowly add the KOH aqueous solution of 50 kilograms of 25wt% and stir, adding the used time is 20 minutes, continues reaction 10 minutes after adding, and adds and maintains 40 DEG C with temperature in reaction process, obtain neutralizer; In neutralizer, add the KOH aqueous solution of 300 kilograms of 52wt%, under the condition of 60 DEG C, saponification 90 minutes, obtains saponification liquor; In saponification liquor, add the isopropanol water solution 300L of 50vol%, stir 20 minutes, then add 6# solvent oil 4000L, stir stratification after 30 minutes, obtain 6# solvent oil reservoir; Concentrated 6# solvent oil reservoir, can obtain the lycopene oleo-resinous 66.14 kilograms that purity is 8.48%, Lyeopene yield is 91.20%.
Embodiment 4: the processing step of the industrial method of this raising lycopene oleo-resinous purity is as described below.
Taking 300 kilograms of Lyeopene purity is the lycopene oleo-resinous of 2.16%, adds the propyl alcohol of 300 kilograms and the mixed solvent (propyl alcohol: methyl alcohol=2:1 mass ratio) of methyl alcohol wherein, then stirs at 42 DEG C, obtain mixed solution; In mixed solution, slowly add the NaOH aqueous solution of 30 kilograms of 10wt%, Keep agitation in adition process, adding the used time is 10 minutes, continues reaction 8 minutes after adding, and adds and maintains 42 DEG C with temperature in reaction process, obtain neutralizer; In neutralizer, add the NaOH aqueous solution of 210 kilograms of 50wt%, under the condition of 63 DEG C, saponification 100 minutes, obtains saponification liquor; In saponification liquor, add the propyl alcohol of 50vol% and the aqueous solution 300L of methyl alcohol (propyl alcohol: methyl alcohol=1:1 volume ratio), stir 15 minutes, then add 6# solvent oil 4200L, stratification after stirring, obtain 6# solvent oil reservoir; Concentrated 6# solvent oil reservoir, can obtain the lycopene oleo-resinous 71.05 kilograms that purity is 8.29%, Lyeopene yield is 90.90%.
Claims (5)
1. improve an industrial method for lycopene oleo-resinous purity, it is characterized in that, the processing step of its method is: (1) adds alcoholic solvent in lycopene oleo-resinous, stirs, and obtains mixed solution;
(2) in mixed solution, add alkaline aqueous solution and stir, in and oleo-resinous in fatty acid compound, obtain neutralizer;
(3) in neutralizer, add alkaline aqueous solution and stir, saponification oil compounds wherein, obtains saponification liquor;
(4) in saponification liquor, add alcohol solution, stir; Then 6# solvent oil is added, stratification after stirring; Collect 6# solvent layer and concentrate, obtaining the lycopene oleo-resinous that purity improves;
Described step (2) the neutral and alkali aqueous solution is the aqueous solution of KOH or NaOH, and the mass percentage concentration of solution is 10 ~ 30%; Lycopene oleo-resinous: alkaline aqueous solution=1:0.1 ~ 0.3(W/W);
Described neutralization reaction temperature is 40 ~ 45 DEG C; The used time that adds of alkaline aqueous solution is 10 ~ 20 minutes, continues reaction 5 ~ 10 minutes after adding;
?in described step (4), alcohol solution is the aqueous solution of methyl alcohol, ethanol, propyl alcohol and/or Virahol, and in solution, the concentration expressed in percentage by volume of alcohol is 50%, lycopene oleo-resinous: alcohol solution=1:1(V/V);
?described step (3) the neutral and alkali aqueous solution is the aqueous solution of KOH or NaOH, and the mass percentage concentration of solution is 50 ~ 56%; Lycopene oleo-resinous: alkaline aqueous solution=1:0.6 ~ 1(W/W);
Described saponification reaction temperature is 55 ~ 63 DEG C, and saponification time is 90 ~ 120 minutes;
In described step (1), the purity of lycopene oleo-resinous is lower than 3%.
2. the industrial method of raising lycopene oleo-resinous purity according to claim 1, it is characterized in that: in described step (1), at 40 ~ 45 DEG C, lycopene oleo-resinous and alcoholic solvent are stirred, lycopene oleo-resinous: alcoholic solvent=1:1 ~ 3(W:W).
3. the industrial method of raising lycopene oleo-resinous purity according to claim 2, is characterized in that: described alcoholic solvent is one or more in methyl alcohol, ethanol, propyl alcohol and Virahol.
4. the industrial method of the raising lycopene oleo-resinous purity according to claim 1-3 any one, is characterized in that: in described step (4), stirs 15 ~ 30 minutes after adding alcohol solution.
5. the industrial method of the raising lycopene oleo-resinous purity according to claim 1-3 any one, is characterized in that: in described step (4), 6# solvent oil: lycopene oleo-resinous=11 ~ 15:1(V/W).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103664462B (en) * | 2013-11-19 | 2015-06-17 | 新疆红帆生物科技有限公司 | Secondary recycling method for lycopene in tomato oil |
| CN106280542B (en) * | 2016-08-15 | 2017-11-17 | 晨光生物科技集团股份有限公司 | A kind of production method for improving lycopene oleoresin quality |
| CN111943801A (en) * | 2019-05-17 | 2020-11-17 | 清馨(北京)科技有限公司 | Industrial production method of lycopene oleoresin |
Citations (4)
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| US5858700A (en) * | 1997-04-03 | 1999-01-12 | Kemin Foods, Lc | Process for the isolation and purification of lycopene crystals |
| CN1298904A (en) * | 2000-12-18 | 2001-06-13 | 新疆生命红科技投资开发有限责任公司 | Process for preparing crystal lycopene and/or lycopene oil resin from tomato paste |
| CN1775867A (en) * | 2005-11-30 | 2006-05-24 | 中国科学院新疆理化技术研究所 | Method for preparing licopin |
| CN1807410A (en) * | 2006-02-23 | 2006-07-26 | 上海交通大学 | Lycopene purification preparation method |
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2012
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5858700A (en) * | 1997-04-03 | 1999-01-12 | Kemin Foods, Lc | Process for the isolation and purification of lycopene crystals |
| CN1298904A (en) * | 2000-12-18 | 2001-06-13 | 新疆生命红科技投资开发有限责任公司 | Process for preparing crystal lycopene and/or lycopene oil resin from tomato paste |
| CN1775867A (en) * | 2005-11-30 | 2006-05-24 | 中国科学院新疆理化技术研究所 | Method for preparing licopin |
| CN1807410A (en) * | 2006-02-23 | 2006-07-26 | 上海交通大学 | Lycopene purification preparation method |
Non-Patent Citations (3)
| Title |
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| 周丹红,等.皂化法提取番茄红素及其晶体的表征.《化学与生物工程》.2006,第23卷(第6期),第41-43页. * |
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| 番茄红素的生产与检测研究;李雪雁;《电子科技大学学报》;20031231;第32卷(第6期);第760-763页 * |
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Application publication date: 20130213 Assignee: Xinjiang Chenxi Pepper Industry Co.,Ltd. Assignor: Chengguang Natural Pigment Group Co., Ltd. Contract record no.: 2019990000135 Denomination of invention: Industrialization method for improving purity of lycopene oil resin Granted publication date: 20150107 License type: Common License Record date: 20190430 |
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