CN105778555A - Desolventizing purification method of lycopene oil resin - Google Patents
Desolventizing purification method of lycopene oil resin Download PDFInfo
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- CN105778555A CN105778555A CN201410823965.0A CN201410823965A CN105778555A CN 105778555 A CN105778555 A CN 105778555A CN 201410823965 A CN201410823965 A CN 201410823965A CN 105778555 A CN105778555 A CN 105778555A
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Abstract
The invention discloses a desolventizing purification method of lycopene oil resin. The method consists of: putting lycopene crystals in an interlayer equipped desolventizing kettle, adding vegetable oil and performing stirring heating; then introducing the heated material into a desolventizing pot, opening a vacuum valve to perform pressure reduction on the desolventizing pot, extracting the residual solvent in non-desolventized lycopene oil resin, at the same time introducing nitrogen to the bottom of the desolventizing kettle, and conducting desolventizing for 8-24h. The method provided by the invention has the advantages of simplicity, short time and low cost, and can ensure lycopene oil resin no peculiar smell. As no water-containing alcohol is added, the desolventized lycopene oil resin is difficult to deteriorate, the purity is high, the quality of lycopene oil resin is enhanced, and the product safety is high. Therefore, the method is suitable for industrial production.
Description
Technical field
The present invention relates to the synthesis of a kind of lycopene, the preparation method that specifically a kind of simple and easy lycopene oleo-resinous precipitation purifies, belong to the synthesis field of lycopene.
Background technology
Lycopene is a kind of natural pigment contained in plant.It is primarily present in the mature fruit of plant of Solanaceae Fructus Lycopersici esculenti.It is one of most powerful antioxidant of being found in the plant of nature at present.Science proves, singlet oxygen and oxygen-derived free radicals in human body are the arch-criminals encroaching on human body self immune system.Effect of lycopene scavenging free radicals outclass other carotenoid and vitamin E, and its singlet-oxygen quenching speed constant is 100 times of vitamin E.Lycopene is very unstable, it is again water-insoluble, current maximally effective extracting method still carries out with organic solvent, but, owing in Fructus Lycopersici esculenti, water content is significantly high, lycopene is in the cellular environment that water content is significantly high, and organic solvent not easily penetrates into, causing that the consumption of organic solvent is big, extraction efficiency is not high yet.
Summary of the invention
In order to solve the problems referred to above, the present invention devises the preparation method that a kind of simple and easy lycopene oleo-resinous precipitation purifies, adopting present invention process to carry out precipitation purification, the time is short, cost is low, it is possible to ensure lycopene oleo-resinous free from extraneous odour, owing to not adding moisture ethanol, lycopene oleo-resinous after precipitation is unlikely to deteriorate, and purity is high, improves lycopene oleo-resinous quality, the safety of product is high, is suitable for industrialized production.
The technical scheme is that
The preparation method that a kind of simple and easy lycopene oleo-resinous precipitation purifies, comprises the following steps:
(1) crystal of lycopene is placed in precipitation still with dissection, and the vegetable oil added is stirred heating up, by adding vegetable oil, it is not only able to dilution lycopene oleo-resinous, increase mobility, whipping process can also increase the surface area that oleoresin contacts with vacuum gas-phase, reduce the resistance that in oleoresin, residual dissolved goes out, be conducive to residual molten precipitation；
Ethanol precipitation technique is added relative to tradition, due to ethanol inherently solvent, if de-unclean, it is possible to stay new residual molten-ethanol is residual molten, and the vegetable oil that the present invention adopts is the composition that lycopene oleo-resinous inherently contains, it is not necessary to elimination, just do not have ethanol residual molten yet；It addition, ethanol in the market much all contains plasticiser residue, plasticiser is likely brought to remain the risk exceeded standard with ethanol precipitation.
(2) material after step (1) being heated up imports in precipitation tank, opens vacuum valve and precipitation tank is reduced pressure, and extracts the residual solvent in non-precipitation lycopene oleo-resinous, is filled with nitrogen in precipitation bottom portion simultaneously, precipitation 8-24 hour.Residual molten in lycopene oleo-resinous can be maintained at below 50ppm after adopting above-mentioned steps of the present invention, meet the requirement of relative national standards.And precipitation purifies, the time is short, cost is low, it is possible to ensure lycopene oleo-resinous free from extraneous odour, owing to not adding moisture ethanol, the lycopene oleo-resinous after precipitation is unlikely to deteriorate, and purity is high, improving lycopene oleo-resinous quality, the safety of product is high, is suitable for industrialized production.
Wherein, the vegetable oil of described step (1) includes safflower oil, certain herbaceous plants with big flowers salad or Oleum Brassicae campestris, and the addition of described vegetable oil is the 10%-30% of gross weight.
Temperature after described step (1) intensification is maintained between 30-50 DEG C.
The vacuum of described step (2) precipitation tank is≤-0.08MPa.
Described step (2) passes into the pressure≤0.1MPa of nitrogen.
It is an advantage of the current invention that: adopt present invention process to carry out precipitation purification, method is easy, time is short, cost is low, ensure that lycopene oleo-resinous free from extraneous odour, owing to not adding moisture ethanol, the lycopene oleo-resinous after precipitation is unlikely to deteriorate, purity is high, improving lycopene oleo-resinous quality, the safety of product is high, is suitable for industrialized production.
Below in conjunction with drawings and Examples, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is the process chart of the embodiment of the present invention.
Detailed description of the invention
Hereinafter the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred embodiment described herein is merely to illustrate and explains the present invention, is not intended to limit the present invention.
Except as otherwise noted, the percent adopted in the present invention is percetage by weight.
Embodiment 1
As it is shown in figure 1, the preparation method that a kind of simple and easy lycopene oleo-resinous precipitation purifies, comprise the following steps:
(1) crystal of lycopene made is placed in precipitation still with dissection, and the vegetable oil added is stirred heating up, by adding vegetable oil, it is not only able to dilution lycopene oleo-resinous, increase mobility, whipping process can also increase the surface area that oleoresin contacts with vacuum gas-phase, reduce the resistance that in oleoresin, residual dissolved goes out, be conducive to residual molten precipitation；
Ethanol precipitation technique is added relative to tradition, due to ethanol inherently solvent, if de-unclean, it is possible to stay new residual molten-ethanol is residual molten, and the vegetable oil that the present invention adopts is the composition that lycopene oleo-resinous inherently contains, it is not necessary to elimination, just do not have ethanol residual molten yet；It addition, ethanol in the market much all contains plasticiser residue, plasticiser is likely brought to remain the risk exceeded standard with ethanol precipitation；
(2) material after step (1) being heated up imports in precipitation tank, open vacuum valve precipitation tank is reduced pressure, extract the residual solvent in non-precipitation lycopene oleo-resinous, it is filled with nitrogen in precipitation bottom portion simultaneously, prevent the lycopene purified oxidized, the precipitation time closed precipitation tank vacuum valve after 8-24 hour, opened exhaust-valve.
Adopt after above-mentioned steps and residual molten in lycopene oleo-resinous can be maintained at below 50ppm, meet the requirement of relative national standards.And precipitation purifies, the time is short, cost is low, it is possible to ensure lycopene oleo-resinous free from extraneous odour, owing to not adding moisture ethanol, the lycopene oleo-resinous after precipitation is unlikely to deteriorate, and purity is high, improving lycopene oleo-resinous quality, the safety of product is high, is suitable for industrialized production.
Wherein, the vegetable oil of described step (1) includes safflower oil, certain herbaceous plants with big flowers salad, Oleum Brassicae campestris, and the addition of described vegetable oil is the 10%-30% of gross weight.
Temperature after described step (1) intensification is maintained between 30-50 DEG C.
The vacuum of described step (2) precipitation tank is≤-0.08MPa；Nitrogen pressure≤0.1MPa.
In the present invention, raw materials used being during this area produces commonly uses raw material, all can obtain from market, and will not produce impact for producing result；The various equipment adopted in the present invention, the conventional equipment being in the production technology of this area to use, and the operation of each equipment, parameter etc. all conventionally operate and carry out, and there is no special feature.
Claims (6)
1. the preparation method that a simple and easy lycopene oleo-resinous precipitation purifies, it is characterised in that comprise the following steps:
(1) crystal of lycopene is placed in precipitation still with dissection, and the vegetable oil added is stirred heating up；
(2) material after step (1) being heated up imports in precipitation tank, opens vacuum valve and precipitation tank is reduced pressure, and extracts the residual solvent in non-precipitation lycopene oleo-resinous, is filled with nitrogen in precipitation bottom portion simultaneously, precipitation 8-24 hour.
2. preparation method according to claim 1, it is characterised in that: the vegetable oil of described step (1) includes safflower oil, certain herbaceous plants with big flowers salad or Oleum Brassicae campestris.
3. preparation method according to claim 1 and 2, it is characterised in that: the addition of described vegetable oil is the 10%-30% of gross weight.
4. preparation method according to claim 1, it is characterised in that: the temperature after described step (1) intensification is maintained between 30-50 DEG C.
5. preparation method according to claim 1, it is characterised in that: the vacuum of described step (2) precipitation tank is≤-0.08MPa.
6. preparation method according to claim 1, it is characterised in that: described step (2) passes into the pressure≤0.1MPa of nitrogen.
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| CN201410823965.0A CN105778555B (en) | 2014-12-26 | 2014-12-26 | A kind of preparation method of simple lycopene oleoresin precipitation purification |
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| CN201410823965.0A CN105778555B (en) | 2014-12-26 | 2014-12-26 | A kind of preparation method of simple lycopene oleoresin precipitation purification |
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| CN105778555A true CN105778555A (en) | 2016-07-20 |
| CN105778555B CN105778555B (en) | 2017-05-31 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380009A (en) * | 2002-05-29 | 2002-11-20 | 北京普瑞孚天然药物现代纯化和分离研究所有限公司 | Preparation method of lycopene richly containing cis-isomer |
| WO2008032006A1 (en) * | 2006-09-11 | 2008-03-20 | Overseal Natural Ingredients Ltd. | Naturally derived colours with bioactive compounds |
| CN101148631A (en) * | 2007-11-09 | 2008-03-26 | 天津商业大学 | Method for preparing lycopene-enriched vegetable oil |
| CN101184543A (en) * | 2005-04-19 | 2008-05-21 | 爱德华多·萨维奥雷伊 | Method of preparing lycopene-enriched formulations that are free of organic solvents, formulations thus obtained, compositions comprising said formulations and use of same |
| CN101248861A (en) * | 2007-02-22 | 2008-08-27 | 刘洪涛 | Tomato deep-processing method |
| CN101381274A (en) * | 2008-10-16 | 2009-03-11 | 中国农业大学 | Method for removing dissolvent residual from lycopene oleoresin |
-
2014
- 2014-12-26 CN CN201410823965.0A patent/CN105778555B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380009A (en) * | 2002-05-29 | 2002-11-20 | 北京普瑞孚天然药物现代纯化和分离研究所有限公司 | Preparation method of lycopene richly containing cis-isomer |
| CN101184543A (en) * | 2005-04-19 | 2008-05-21 | 爱德华多·萨维奥雷伊 | Method of preparing lycopene-enriched formulations that are free of organic solvents, formulations thus obtained, compositions comprising said formulations and use of same |
| WO2008032006A1 (en) * | 2006-09-11 | 2008-03-20 | Overseal Natural Ingredients Ltd. | Naturally derived colours with bioactive compounds |
| CN101248861A (en) * | 2007-02-22 | 2008-08-27 | 刘洪涛 | Tomato deep-processing method |
| CN101148631A (en) * | 2007-11-09 | 2008-03-26 | 天津商业大学 | Method for preparing lycopene-enriched vegetable oil |
| CN101381274A (en) * | 2008-10-16 | 2009-03-11 | 中国农业大学 | Method for removing dissolvent residual from lycopene oleoresin |
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