CN1365626A - Nano-chalss natural lycopene product and its preparing process - Google Patents

Nano-chalss natural lycopene product and its preparing process Download PDF

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Publication number
CN1365626A
CN1365626A CN02100653A CN02100653A CN1365626A CN 1365626 A CN1365626 A CN 1365626A CN 02100653 A CN02100653 A CN 02100653A CN 02100653 A CN02100653 A CN 02100653A CN 1365626 A CN1365626 A CN 1365626A
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lycopene
oil
nanoscale
preparation
premixed
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CN1258983C (en
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陈焕忠
尤丰
江俊池
赵斌
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Urumqi golden tomato Biotechnology Co., Ltd.
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陈焕忠
尤丰
江俊池
赵斌
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Abstract

A nano matre-class lycopene oil is prepared from lycopene with granulity of less than 50 nm in the form of resin and/or crystal and plant oil through high-speed stirring at 30-60 deg.C, pressure-homogenizing under a pressure more than 18 MPa at least for 2 times, and loading in capsules.

Description

Nano-chalss natural lycopene product and preparation method thereof
Technical field
The present invention relates to the natural lycopene goods, relate in particular to the stabilized nano level natural lycopene goods that are prepared from by natural lycopene oleoresin or highly purified natural lycopene crystallization, comprise lycopene oil and stable lycopene emulsion, also relate to their preparation method simultaneously.
Technical background
Countless medical practices prove that in carotenoid, the antioxidation of lycopene is the strongest, are 3 times of beta carotene, are about 100 times of vitamin E.The physiologically active of lycopene is avoided oxidative damage and is realized that lycopene is high more in the blood of human body by the protection body, and oxide is just few more, makes each tissue of human body, organ keep a kind of state of healthy coordination, thus delaying human body caducity effectively.Result of study proves that lycopene also has the immunologic function of activating human body cells, prevents and treats the effect of prostate cancer, cancer of the stomach, cutaneum carcinoma, breast cancer, cervical carcinoma and angiocardiopathy effectively.Lycopene has so many medicine and health-care efficacy, how to improve the absorption situation when being applied to human body as liposoluble constituent, is that people are concerned about.
In recent years, the superfine nano technology had begun extensive use in fields such as medicine, health foods, it is found that; common Chinese, for example cow-bezoar is worked into nano-scale; surprising variation has all taken place in its physicochemical property and curative effect, can treat difficult and complicated cases, and has extremely strong targeting.Be difficult for the medicine (as estradiol) or the health food that are absorbed by the body, if after making nano powder or suspension, will become absorbs easily, and then has improved bioavailability of medicament in the past.People also find, same medicine is made plaster and is attached to the affected part if be processed into Nano medication, just can directly absorb and need not inject by skin.
Present lycopene product generally all is a soft capsule dosage form, and solvent-extracted lycopene oleoresin is only recorded capsule through general stirring and processing, or adopts the nanoscale product that processes to record capsule.Lycopene degradation reaction by purplish red browning takes place in lycopene oleoresin in the former soft capsule of lycopene easily in placement, the beginning layering, precipitation and the natural gumization that have, and greatly the quality of infringement itself and effect are worth.Use " 10mg adorns the natural lycopene soft capsule " that lycopene oleoresin that the oleoresin of commodity LYC-O-MATO 6% prepared " 5mg adorn natural lycopene " and " 15mg adds 100 μ g selenium lycopenes " and CN1298904A patent of invention produce prepares as the HEALTHY ORIGINS of manufacturer and above-mentioned problem all occurred.Except these quality problems, because dissolvent residual in the lycopene oleoresin also can produce pungent residual solvent smell in process of production and because the oleoresin flowability is bad, the phenomenon of conveying pipeline obstruction, explosion take place when recording soft capsule.
In order farthest to be absorbed by the body, CN1251745A (BASF AG) discloses a kind of " carotenoid formulation that contains the mixture of bata-carotene, lycopene and lutein ", wherein used the superfine technology of the long-time grinding of ball mill, its granular size is (15000 nanometer) about 15 microns.Though the carotenoid formulation that is easily absorbed by the body also is provided, and this carotenoid raw material that wherein requires to use all should preferably use purity to surpass 75% crystal form, more preferably purity surpasses 90%, especially preferably surpass 95% and extremely preferably surpass 98%, can use bata-carotene, lycopene and the lutein of natural origin, preferred especially synthetic preparation bata-carotene and lycopene.Purity is lower than the method that 75% crystalline solid is not suitable for this patent, the mixture of the oleoresin raw material of low-purity (for example below the 3-24% even 75%) or oleoresin and low-purity crystalline solid, do not advise especially using, thereby the use of raw material is restricted, the price of product is height just naturally.
We know that the commercial value of natural lycopene determines that according to purity the high more then price of purity (content) is high more.As U.S. lycopene LYCOPENE, article number L9879, standard is [50Z-65-8] molecular formula C 40H 56Molecular weight 536.9, purity From to tomato 90-95%10mg is 473.7USD, the lycopene commodity valency of amounting to 90-95% content is 380,000 yuan/kg, and domestic production 80-90% crystal of lycopene body price is also at ten thousand yuan/kg of 6-8, yet lycopene purity is at oleoresin and the crystalline mixture of 3-24%, being worth only is ten thousand yuan/kg of 0.15-1.2, and the crystal of lycopene of purity 60-75% and the mixture of its oleoresin are worth the ten thousand yuan/kg into 3-4.
On the composition of product, BASF patent of invention CN1251745A will be when its patented product of preparation, also will add other active materials of 0.01-40% weight, what they selected has: about 9 kinds of other carotenoid, about 26 kinds of vitamins, about 7 kinds of choline amino acid, 5 kinds of polybasic unsaturated fatty acids, 8 kinds of garlic categories, 4 kinds of ester classes, about 5 kinds of antioxidant also has about 5 kinds of solubilizer.This not only increases production cost, and compatibility is bad, also can make deterioration in quality or counterproductive, is not simple lycopene oil formulation so the method according to BASF we can say obtains, and temperature also can cause the color and luster of product and even the change of quality up to 185 ℃ high-temperature process.
Summary of the invention
Therefore, the invention provides a kind of nanoscale lycopene goods, especially a kind of nanoscale lycopene oil, be easy to absorption by human body, on composition, only comprise select lycopene and edible vegetable oil for use, be a kind of fully natural prod, not only batching is simple, and Product Safety is good, also can not produce bad reaction.
On the basis of above-mentioned lycopene oil product, the present invention also provides a kind of nanoscale lycopene emulsion, can be used as the base-material of diet product, health products, cosmetics etc.
The present invention also provides the preparation method of above-mentioned nanoscale lycopene oil and emulsion, except the crystal of lycopene that uses 70-90%, also can use the lycopene oleoresin of 3-24%, the mixture of the lycopene oleoresin of 24-70% and part lycopene crystal, directly be processed into stabilized nano lycopene oil and the nanometer lycopene emulsion of lycopene particles degree less than all size content of 50nm, record edible health and pharmaceutical soft capsule to be applicable to very easily, or and then emulsification prepare cosmetics for health care such as lipstick, facial mask, the face breast, the micro-capsule electuary, beverage, base-material, health foods such as oral liquid also can be used for going in the bakery product.
According to nanoscale lycopene oil provided by the invention, wherein the content of lycopene is 0.1-30wt.%, and is made up of less than the lycopene and the natural edible-plant oil of 50 nanometers granularity, and the granularity of lycopene especially can be less than 50 nanometers.Through recording soft capsule, promptly can be made into stabilized nano level lycopene fat capsule.All technical barriers in the time of can overcoming existing lycopene oleoresin and record soft capsule.
Preparation method according to nanoscale lycopene goods provided by the invention, comprise 1-2 weight portion lycopene crystal and 800-1000 weight portion natural edible-plant oil for raw material, be specially: implement premixed stirring raw material, material after the premixed is filtered, make the nanoscale lycopene oil.
Comprise lycopene oleoresin, lycopene crystal or their mixture and natural edible-plant oil for raw material, the preparation method is: under 30-60 ℃ the high-speed stirred raw material is implemented premixed; Material after the premixed is carried out secondary pressure homogeneous at least, and homogenization pressure is more than the 18Mpa, makes the nanoscale lycopene oil.
Preparation in accordance with the present invention, the raw material that uses is not limited to crystalline solid, can also be the mixture of lycopene oleoresin or oleoresin and crystalline solid, wherein the purity content of lycopene oleoresin can be low to moderate 3%, the mixture of particularly suitable 60-75% oleoresin and crystalline lycopene.
Preparation method provided by the invention, described premixed makes raw material by mixed uniformly effect except reaching, can also tentatively reach the even dispersion of material and the granular purpose of lycopene particles, so, when premixed except that suitable heating, also require to implement simultaneously high-speed stirred, mixing speed does not have strict the qualification, determines because of employed content of lycopene, that is to say, content of lycopene is higher in the raw material that uses, the corresponding raising of mixing speed.
Difference according to employed lycopene raw material, optionally carry out vacuum emulsification for the material after above-mentioned premixed, when especially using the low concentration oleoresin, can further remove the residual solvent in the oleoresin, help the dispersion of impurity component in the oleoresin simultaneously.
In the described homogeneous of secondary pressure at least, at least once homogenization pressure is more than 180Mpa, promptly, for carrying out high pressure and super-high-pressure homogenization through premixed material, for example at first with the pressure more than the 18Mpa, preliminary election 18-60Mpa, carry out high-pressure homogeneous, at least once, implement the above super-high-pressure homogenization of 180Mpa then, be equally at least once.By the homogeneous of high pressure and super-pressure, can realize the nanometer ultra micro of material is handled, wherein homogenizer of Cai Yonging and super-high-pressure homogenization equipment all are the conventional equipments in this field, and is for example listed among the embodiment of back.
The crude vegetal that the present invention uses is food grade natural oil or essential oil, for example corn salad oil, tomato seed salad oil, safflower salad oil, sunflower seeds salad oil, sesame salad oil, evening primrose wet goods, or their mixture.When wherein content of lycopene was very low, for example 0.1-1% directly can be used as edible oil, and for example cooking oil uses, because wherein content of lycopene is lower, adopts common mixer can realize the purpose of emulsification and dispersion.
A further object of the invention is to add demineralized water again after the preparation of nanometer lycopene oil is finished, distilled water for example, deionization, pure water etc., further Q/W (oil-in-water) type emulsion or W/O (Water-In-Oil) type emulsion are made in emulsification again, wherein except that emulsifying agent, can also add various nutritional agents, lecithin for example, PluronicF68, mannitol, glycerine, the vitamin E wet goods, so that lycopene more wide spread except that being used for soft capsule for health care, can also be used for health-related cosmetics, as: lipstick, facial mask, beyond the face breast, can also be used for various cold drinks, base-material, ice cream and bakery product and various the needs go in interpolation natural edible red pigment and the functional health product, are that the operator obtains bigger economic interests.
Can adopt further emulsification on the basis of the lycopene oil that preceding method obtains in the preparation of above-mentioned emulsion, also can finish in a step.
In a word, enforcement of the present invention has following beneficial effect:
1, the applying nano technology has greatly reduced the production cost of various lycopene formulations, but in using in the maximum magnitude, the lycopene oleoresin of low-grade content 3-75% or the mixture of oleoresin and crystal of lycopene, can certainly use the crystalline solid of content of lycopene more than 75-95% is raw material, preparation nanometer lycopene oil and emulsion.Use the present invention, can utilize the lycopene oleoresin and the crystalline solid of various different purity, the saving that the mixture of particularly suitable 60-75% oleoresin and crystalline lycopene, its cost of material provide than patent of invention CN1251745A is more than 6 times.
2, batching is simple, does not add other chemical synthesis materials, and the lycopene consumption can greatly increase, and product content has improved, and just can make people reduce amount, and can reach better effect.Only select lycopene and edible vegetable oil, essential oil for use, the employing pure natural plant extract is a raw material, and by the scientific method preparation, the dissolvent residual in the oleoresin is further reduced, and Product Safety is good, more can not produce bad reaction.
3, owing to adopt the ultra micro nanometer technology, in process, need not be as BASF patent (CN1251745A) narration the sort of with lycopene and oil, be heated to 185 ℃ of high temperature, 25 minutes in oil bath.Though lycopene is subjected to high temperature in oil, the short time influence is little, and it is brown deeply to facts have proved that high temperature lycopene like this color in oil becomes, and loses original cerise.It is influential to the lycopene quality what this illustrates, therefore, all round process of the present invention is when the superfine processing, the temperature of lycopene oil is subjected to the effect of mechanical friction and high speed shear, temperature is no more than 65-70 ℃, and can very fast cooling, this is not only energy-conservation, and helps guaranteeing the potential quality and the exterior quality of product.
4, nanoscale lycopene oil provided by the invention, owing to be a kind of nanometer product, particle has good dispersiveness, thereby stability is high, is particularly suited for recording soft capsule.
Invention embodiment
Below describe enforcement of the present invention in detail by specific embodiment, but the purpose of these embodiment only is to help the reader to understand the solution of the present invention and beneficial effect, can not constitute the qualification to the scope of the present invention.
Embodiment 1:
The preparation method of 0.1%-0.2% nanometer natural lycopene oil:
Natural lycopene crystalline lens and 800-1000 times of corn salad oil with the weight portion of part by weight 1-2, be natural lycopene crystalline lens and the corn salad oil of 50g-80-90%, put into SLR type homogeneous agitator, mixed 10min, filter with 350 orders-450 order nylon filter cloth, remove possible slag, promptly obtaining the limpid natural lycopene that contains of kermesinus is 0.2% nanometer natural lycopene oil 1000-1100g, grain fineness can directly be done edible cooking oil and ready-mixed oil less than 20nm.
Embodiment 2:
The preparation method of another low concentration 0.2% nanometer natural lycopene oil:
Natural lycopene crystalline lens and corn salad oil 800-900g with 250g80-90%, put into general mixer, mixed with the mixed 10min that stirs of 36-802pm, place after 1 hour and filter with 450 order nylon filter clothes, promptly obtaining the limpid translucent natural lycopene that contains of kermesinus is 0.2% nanometer natural lycopene oil 1000-1100g, grain fineness can directly be made edible cooking oil less than 20nm.
Embodiment 3:
The preparation method of the nanometer natural lycopene oil of 3% concentration:
Natural lycopene oleoresin and corn salad oil 400g with 550g6%, evening primrose oil 100g puts into SLR type homogeneous agitator, mixed 10min, put into PVQ-3UN type vacuum emulsification machine again, homogeneous 10min, put into twice of 20Mpa pressure homogeneous of JJ0.1/60 homogenizer then, send in the homogenizer of NCJJ-0.2/20 usefulness>180Mpa pressure homogeneous again twice, promptly obtain the nanometer natural lycopene oil 1000g of 3% purity, grain fineness is less than 20nm, and can be used for directly, preparation contains the soft capsule of lycopene ball of lycopene greater than 15mg/500mg.
Embodiment 4:
The preparation method of the nanometer natural lycopene oil of 6% concentration:
Natural lycopene oleoresin and a small amount of lenticular mixture and 700g tomato seed oil with 300g24%, the 200g evening primrose oil is put into SLR type homogeneous agitator, mixed 10min, put into twice of 30Mpa pressure homogeneous of JJ0.1/60 homogenizer again, send in the homogenizer of NCJJ-0.2/20 usefulness>180Mpa pressure homogeneous again twice, promptly obtain the nanometer natural lycopene oil of 6% purity, grain fineness is less than 20nm, and can be used for directly, preparation contains the soft capsule of lycopene ball of lycopene greater than 30mg/500mg.
Embodiment 5:
The preparation method of the nanometer natural lycopene oil of 10% concentration:
Natural lycopene oleoresin and a small amount of lenticular mixture and 1500g tomato seed salad oil with 300g60%, put into SLR type homogeneous agitator, homogeneous 10min, again this miscella is put into twice of 50Mpa pressure homogeneous of JJ0.1/60 homogenizer, make grain fineness less than 30 μ m, send into again and use twice of 180Mpa pressure homogeneous in the NCJJ-0.20/20 homogenizer, promptly obtain the nanometer natural lycopene oil 1800g of 10% purity, particle diameter can be used for preparing the soft capsule of lycopene ball that contains lycopene 50mg/500mg less than 50nm.
Embodiment 6:
The preparation method of the nanometer natural lycopene oil of 30% concentration:
Mixture and 1166g tomato seed salad oil (or safflower salad oil with the natural lycopene crystalline lens oleo-resins a small amount of of 500g60% with it, the sunflower salad oil, the sesame salad oil) puts into SLR type homogeneous agitator, mix 10min, again this miscella is put into twice of 50Mpa pressure homogeneous of JJ0.1/60 homogenizer, make grain fineness less than 50 μ m, send in the NCJJ-0.20/20 homogenizer usefulness>180Mpa pressure homogeneous again one time, make grain fineness less than 30 μ m, send into again and use 250Mpa pressure homogeneous one time in the homogenizer, make grain fineness less than 20nm, to increase product stability and storage property, this finish mainly with the nanometer natural lycopene emulsion formulations of preparation 20%, can be widely used in water-soluble edible haematochrome additive.
Embodiment 7:
The preparation method of the nanometer natural lycopene emulsion of 10% concentration:
With 300g content 60% natural lycopene oleoresin and a small amount of lenticular mixture and 240g tomato seed salad oil, (or safflower salad oil, the sunflower seeds salad oil, the sesame salad oil) with refine yolk lecithin 15g, PluronicF68,20g, mannitol 60g, glycerine 30g, α vitamin e1 g puts into SLR type homogeneous agitator, add 10% Arabic gum emulsion 1134ml again, heat 60 ℃ and carry out pre-emulsification 1 hour, lower the temperature 30 ℃, deliver to emulsification 10min in the HYT2030A28KHZ ultrasonic emulsification machine then, promptly obtain the O/W nanometer natural lycopene emulsion of 10% purity, grain fineness is after testing less than 20nm, can be used for making the beverage base-material, oral liquid, can be added into ice cream, available bakery product etc.
Embodiment 8:
The preparation method of the nanometer natural lycopene emulsion of 20% concentration:
With 1000g content is 30% nanometer natural lycopene oil and the Arabic glue 500g of refine yolk lecithin 15g, vitamin e1 g and 10%, premixed 10min in SLR type homogeneous agitator, again these mixed liquors are sent into and used twice of 180Mpa pressure homogeneous in the NCJJ-0.20/20 homogenizer, promptly obtain the O/W nanometer natural lycopene emulsion of 20% purity, can be used for making senior base material of cosmetics and oil-soluble natural edible red pigment additives such as lipstick.

Claims (12)

1, a kind of nanoscale lycopene oil be made up of less than the lycopene and the natural edible-plant oil of 50 nanometers granularity, and the content of lycopene is 0.1-30wt.%.
2, the described nanoscale lycopene oil of claim 1, wherein, the granularity of lycopene is less than 20 nanometers.
3, a kind of lycopene emulsion wherein contains described nanoscale lycopene oil of claim 1 and emulsifying agent.
4, the purposes of the described lycopene emulsion of claim 3 in making the diet product.
5, the preparation method of nanoscale lycopene goods, raw material comprises 1-2 weight portion lycopene crystal and 800-1000 weight portion natural edible-plant oil, the preparation method comprises: implement premixed to stirring raw material; Material after the premixed is filtered, make the nanoscale lycopene oil.
6, the described preparation method of claim 5 wherein, also comprises conventional emulsifier and demineralized water in the raw material.
7, claim 5 or 6 described preparation methods, wherein, described nanoscale lycopene oil mixes with demineralized water, makes emulsion through emulsification.
8, the preparation method of nanoscale lycopene goods, raw material comprises lycopene oleoresin, lycopene crystal or their mixture and natural edible-plant oil, the preparation method comprises: under 30-60 ℃ the high-speed stirred raw material is implemented premixed; Material after the premixed is carried out secondary pressure homogeneous at least, and homogenization pressure is more than the 18Mpa, makes the nanoscale lycopene oil.
9, the described preparation method of claim 8 wherein, makes material particles by granular to the raw material high-speed stirred in the described premixed process.
10, the described preparation method of claim 8, wherein, in the described homogeneous of secondary pressure at least, homogenization pressure at least once is more than 180Mpa.
11, the described preparation method of claim 8 wherein carries out vacuum emulsification and selectivity comprises to the material after premixed.
12, any described preparation method among the claim 8-11, it also comprises described nanoscale lycopene oil is mixed with demineralized water, makes emulsion through emulsification.
CNB021006539A 2002-02-08 2002-02-08 Nano-chalss natural lycopene product and its preparing process Expired - Fee Related CN1258983C (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101901637A (en) * 2010-07-29 2010-12-01 重庆大学 Composite of vegetable insulating oil and modified nano powder and application and preparation method thereof
CN102077988A (en) * 2010-11-26 2011-06-01 云南聚恒科技有限公司 Hemp seed oil-lycopene soft capsule
CN102329520A (en) * 2011-07-08 2012-01-25 中国热带农业科学院农产品加工研究所 Method for preparing lutein nanometer liquid
CN105166880A (en) * 2014-06-18 2015-12-23 新疆西域果宝生物科技有限公司 Preparation method of lycopene nutrition and health oral liquid
CN106031507A (en) * 2015-03-17 2016-10-19 张跃华 Lycopene functional beverage and preparation method thereof
CN106580828A (en) * 2016-12-21 2017-04-26 周易 Litchi-flavored lip gloss and preparation method thereof
CN112618426A (en) * 2020-06-29 2021-04-09 昆仑技术研究(广州)有限公司 Preparation method and application of water-in-oil type white tomato freeze-dried powder
CN115844015A (en) * 2022-12-06 2023-03-28 南昌大学 Lycopene oil, lycopene preparation and application thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101901637A (en) * 2010-07-29 2010-12-01 重庆大学 Composite of vegetable insulating oil and modified nano powder and application and preparation method thereof
CN101901637B (en) * 2010-07-29 2012-07-04 重庆大学 Composite of vegetable insulating oil and modified nano powder and application and preparation method thereof
CN102077988A (en) * 2010-11-26 2011-06-01 云南聚恒科技有限公司 Hemp seed oil-lycopene soft capsule
CN102077988B (en) * 2010-11-26 2012-12-19 云南聚恒科技有限公司 Hemp seed oil-lycopene soft capsule
CN102329520A (en) * 2011-07-08 2012-01-25 中国热带农业科学院农产品加工研究所 Method for preparing lutein nanometer liquid
CN102329520B (en) * 2011-07-08 2013-06-12 中国热带农业科学院农产品加工研究所 Method for preparing lutein nanometer liquid
CN105166880A (en) * 2014-06-18 2015-12-23 新疆西域果宝生物科技有限公司 Preparation method of lycopene nutrition and health oral liquid
CN106031507A (en) * 2015-03-17 2016-10-19 张跃华 Lycopene functional beverage and preparation method thereof
CN106580828A (en) * 2016-12-21 2017-04-26 周易 Litchi-flavored lip gloss and preparation method thereof
CN112618426A (en) * 2020-06-29 2021-04-09 昆仑技术研究(广州)有限公司 Preparation method and application of water-in-oil type white tomato freeze-dried powder
CN115844015A (en) * 2022-12-06 2023-03-28 南昌大学 Lycopene oil, lycopene preparation and application thereof

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