CN107384378A - A kind of food-grade fluorescence nano microemulsion and preparation method thereof - Google Patents
A kind of food-grade fluorescence nano microemulsion and preparation method thereof Download PDFInfo
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- CN107384378A CN107384378A CN201710725874.7A CN201710725874A CN107384378A CN 107384378 A CN107384378 A CN 107384378A CN 201710725874 A CN201710725874 A CN 201710725874A CN 107384378 A CN107384378 A CN 107384378A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/02—Polyalkylene oxides
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Abstract
The invention discloses a kind of food-grade fluorescence nano microemulsion and preparation method thereof, preparation method is:(1) oil phase must be mixed by mixing isoamyl acetate and ethanol, add Emulsifier EL-60, stirring;(2) it is kept stirring for, water is added dropwise, obtains homogeneous, transparent food-grade fluorescence nano microemulsion.Oil-in-water (O/W) the food-grade fluorescence nano microemulsion for the appearance transparent that the method for the present invention is prepared has fluorescent characteristic.Belong to the category of nano-luminescent material, and belong to food-grade, there is nontoxic, biodegradable, good biocompatibility.Without mark during as fluorescent nano material, support is not required to.The raw material used is simple and easy to get, wherein isoamyl acetate used, is food preparation aroma class additive, product preparation cost also has peat-reek while low.The method of the present invention is without high temperature high pressure process, and simple and easy, process efficiency is high, meets energy-conserving and environment-protective theory.
Description
Technical field
The present invention relates to a kind of preparation method of fluorescence nano microemulsion, belong to production preparation and the application field of microemulsion.
Background technology
For a long time, the research on function factor in food, medicine is not interrupted, is focused mostly on by cell, animal
Test to assess its physiologically active, the research on its mechanism of action is very difficult to be carried out.The appearance and application of food-grade fluorescence probe,
Can the more intuitively detection function factor some outer changes in vivo, so as to realize the real-time monitoring to function factor.
On the basis of fluorescent material is widely studied, the research of fluorescent nano material has started a new tide.It is glimmering
Body of light is to be based on sensor, and the information that chemistry, physics, biology etc. are difficult to detect is converted into optical information to realize detection and divide
Analysis.Fluorescent nano material is pair can to launch fluorescence, at least one-dimensional in three dimensions be in nano-scale (0.1-100nm)
Material general designation, it has been provided simultaneously with the characteristic of fluorescent material and nano material.Fluorescent nano material can be used as fluorescence probe
Seek the inner or in vitro active component transmission of biology, drug targeting, bio-imaging etc..The fluorescence nano material of common reporter at present
Material is broadly divided into following several:Fluorescent material, fluorescin, inorganic nano fluorescent grain based on labelling strategies etc..Wherein, base
In the fluorescent material of labelling strategies, polymer, the silica of dyestuff doping of such as dye load, it prepares generally relatively more multiple
It is miscellaneous, costly, and the shortcomings that labeling effciency is low be present;Though fluorescin good biocompatibility, be easily quenched, and price compared with
It is expensive;Inorganic nano fluorescent grain, as carbon quantum dot generally can not use separately as probe, and need suitably there is machine support to make
It keeps stable.
Microemulsion is spontaneously formed by components such as surfactant, cosurfactant, oil and water under proper proportion
Stabilization of thermostatic system, its particle diameter between 5-100nm, have colourless, transparent (or translucent), prepare it is easy, through high speed from
The performances such as layering, hypotoxicity, ultralow interfacial tension, emulsification, solubilising, scattered, foaming, lubrication and flexibility do not occur for the heart.Micro emulsion
Liquid, can conduct because above-mentioned unique physicochemical characteristics is widely used in the various fields such as food, medicine, cosmetics, chemistry
Food function factor carrier, active ingredient solubility is improved, increase stability, improve bioavilability;Because of its unique bilayer
Architectural feature, membrane simulation research can be used for;Available for cosmetics are made, promote skin to absorb, effectively extend cosmetics
Shelf-life;Reaction rate etc. can be improved as enzyme and the microreactor of chemical reaction.
At present, the preparation for microemulsion and research are concentrated mainly on its physicochemical characteristics and associated application side
Face, the documents and materials on fluorescence microemulsion and its optical characteristics etc. are not found also.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of food-grade fluorescence nano microemulsion.
Second object of the present invention is to provide a kind of preparation method of food-grade fluorescence nano microemulsion.
Technical scheme is summarized as follows:
A kind of preparation method of food-grade fluorescence nano microemulsion, comprises the following steps:
(1) it is 3 in mass ratio:1-6 ratio, isoamyl acetate and ethanol, which are mixed, must mix oil phase, add mixing
The Emulsifier EL-60 of 1.5-12 times of oil phase quality, under the conditions of temperature is 4-70 DEG C, with 150-400rpm mixing speeds, stir
Mix 10-60min;
(2) 150-400rpm mixing speed is kept, water is added dropwise, the gross mass for adding water is step (1) acquisition
1.5-9 times of liquid gross mass, obtain homogeneous, transparent food-grade fluorescence nano microemulsion.
The mass ratio of isoamyl acetate and ethanol is 3:2.
The mass ratio for mixing oil phase and Emulsifier EL-60 is 1:3.
Step (1) described temperature is 25 DEG C.
Mixing speed is 200rpm.
Step (1) mixing time is 20min.
The gross mass for adding water is 2.33 times of the liquid gross mass that step (1) obtains.
Food-grade fluorescence nano microemulsion prepared by the above method.
Advantages of the present invention:
(1) oil-in-water (O/W) the food-grade fluorescence nano microemulsion tool for the appearance transparent that method of the invention is prepared
There is fluorescent characteristic.
(2) food-grade fluorescence nano microemulsion prepared by the present invention belongs to the category of nano-luminescent material, and belongs to food-grade,
With nontoxic, biodegradable, good biocompatibility.
(3) it need not be marked when food-grade fluorescence nano microemulsion prepared by the present invention is used as fluorescent nano material, be not required to prop up
Frame.
(4) raw material used in the present invention is simple and easy to get, wherein isoamyl acetate used, is food preparation aroma class additive,
Product preparation cost also has peat-reek while low.
(5) method of the invention is without high temperature high pressure process, and simple and easy, process efficiency is high, meets energy-conserving and environment-protective theory.
Embodiment
With reference to specific embodiment, the present invention is further illustrated.
For the present invention using isoamyl acetate as oil phase, Emulsifier EL-60 (CrEL) is surfactant, and ethanol is to help table
Face activating agent.
Embodiment 1
A kind of preparation method of food-grade fluorescence nano microemulsion, comprises the following steps:
(1) take 90mg isoamyl acetates respectively and 30mg absolute ethyl alcohols mix and must mix oil phase, add mixing oil phase matter
1.5 times of amount, i.e. 180mg CrEL are mixed in small beaker, add rotor, adjustment rotating speed is 150rpm, is 4 DEG C of conditions in temperature
Lower stirring 10min;
(2) under 150rpm mixing speed, water is added dropwise, the gross mass for adding water is the liquid that step (1) obtains
1.5 times of gross mass, obtain homogeneous, transparent food-grade fluorescence nano microemulsion.
Gained microemulsion particle diameter is 26.34nm, and PDI (polydispersity Index) is 0.309, and fluorescence intensity is located at
Near 8000.
Embodiment 2
A kind of preparation method of food-grade fluorescence nano microemulsion, comprises the following steps:
(1) take 90mg isoamyl acetates respectively and 60mg absolute ethyl alcohols mix and must mix oil phase, add mixing oil phase matter
3 times of amount, i.e. 450mg CrEL are mixed in small beaker, add rotor, adjustment rotating speed is 200rpm, is 25 DEG C of conditions in temperature
Lower stirring 20min;
(2) under 200rpm mixing speed, water is added dropwise, the gross mass for adding water is the liquid that step (1) obtains
2.33 times of gross mass;Obtain homogeneous, transparent food-grade fluorescence nano microemulsion.
Gained microemulsion particle diameter is 25.62nm, and PDI (polydispersity Index) is 0.323, and fluorescence intensity is located at
Near 8200.
Embodiment 3
A kind of preparation method of food-grade fluorescence nano microemulsion, comprises the following steps:
(1) take 40mg isoamyl acetates respectively and 40mg absolute ethyl alcohols mix and must mix oil phase, add mixing oil phase matter
6 times of amount, i.e. 480mg CrEL are mixed in small beaker, add rotor, adjustment rotating speed is 250rpm, is 50 DEG C of conditions in temperature
Lower stirring 30min;
(2) under 250rpm mixing speed, water is added dropwise, the gross mass for adding water is the liquid that step (1) obtains
4 times of gross mass;Obtain homogeneous, transparent food-grade fluorescence nano microemulsion.
Gained microemulsion particle diameter is 23.24nm, and PDI (polydispersity Index) is 0.378, and fluorescence intensity is located at
Near 7500.Embodiment 4
A kind of preparation method of food-grade fluorescence nano microemulsion, comprises the following steps:
(1) take 30mg isoamyl acetates respectively and 40mg absolute ethyl alcohols mix and must mix oil phase, add mixing oil phase matter
9 times of amount, i.e. 630mg CrEL are mixed in small beaker, add rotor, adjustment rotating speed is 300rpm, is 70 DEG C of conditions in temperature
Lower stirring 40min;
(2) under 300rpm mixing speed, water is added dropwise, the gross mass for adding water is the liquid that step (1) obtains
9 times of gross mass;Obtain homogeneous, transparent food-grade fluorescence nano microemulsion.
Gained microemulsion particle diameter is 20.62nm, and PDI (polydispersity Index) is 0.393, and fluorescence intensity is located at
Near 5700.Embodiment 5
A kind of preparation method of food-grade fluorescence nano microemulsion, comprises the following steps:
(1) take 30mg isoamyl acetates respectively and 50mg absolute ethyl alcohols mix and must mix oil phase, add mixing oil phase matter
12 times of amount, i.e. 960mg CrEL are mixed in small beaker, add rotor, adjustment rotating speed is 350rpm, is 25 DEG C of bars in temperature
50min is stirred under part;
(2) under 350rpm mixing speed, water is added dropwise, the gross mass for adding water is the liquid that step (1) obtains
4 times of gross mass;Obtain homogeneous, transparent food-grade fluorescence nano microemulsion.
Gained microemulsion particle diameter is 18.62nm, and PDI (polydispersity Index) is 0.326, and fluorescence intensity is located at
Near 7600.(transmite slit and exciting slit are located at 2.5nm, and PMT is measured when being 700V by F2500.)
Embodiment 6
A kind of preparation method of food-grade fluorescence nano microemulsion, comprises the following steps:
(1) take 30mg isoamyl acetates respectively and 60mg absolute ethyl alcohols mix and must mix oil phase, add mixing oil phase matter
4 times of amount, i.e. 360mg CrEL are mixed in small beaker, add rotor, adjustment rotating speed is 400rpm, is 25 DEG C of conditions in temperature
Lower stirring 60min;
(2) under 400rpm mixing speed, water is added dropwise, the gross mass for adding water is the liquid that step (1) obtains
2.33 times of gross mass;Obtain homogeneous, transparent food-grade fluorescence nano microemulsion.
Gained microemulsion particle diameter is 15.62nm, and PDI (polydispersity Index) is 0.303, and fluorescence intensity is located at
Near 8000.(transmite slit and exciting slit are located at 2.5nm, and PMT is measured when being 700V by F2500.)
Embodiment 7
A kind of preparation method of food-grade fluorescence nano microemulsion, comprises the following steps:
(1) take 90mg isoamyl acetates respectively and 60mg absolute ethyl alcohols mix and must mix oil phase, add mixing oil phase matter
4 times of amount, i.e. 600mg CrEL are mixed in small beaker, add rotor, adjustment rotating speed is 200rpm, is 25 DEG C of conditions in temperature
Lower stirring 20min;
(2) under 200rpm mixing speed, water is added dropwise, the gross mass for adding water is the liquid that step (1) obtains
4 times of gross mass;Obtain homogeneous, transparent food-grade fluorescence nano microemulsion.
Gained microemulsion particle diameter is 15.62nm, and PDI (polydispersity Index) is 0.203, and fluorescence intensity is located at
Near 7200.(transmite slit and exciting slit are located at 2.5nm, and PMT is measured when being 700V by F2500.)
Claims (8)
1. a kind of preparation method of food-grade fluorescence nano microemulsion, comprises the following steps:
(1) it is 3 in mass ratio:1-6 ratio, isoamyl acetate and ethanol, which are mixed, must mix oil phase, add mixing oil phase
The Emulsifier EL-60 of 1.5-12 times of quality, under the conditions of temperature is 4-70 DEG C, with 150-400rpm mixing speeds, stirring
10-60min;
(2) 150-400rpm mixing speed is kept, water is added dropwise, the gross mass for adding water is the liquid that step (1) obtains
1.5-9 times of gross mass, obtain homogeneous, transparent food-grade fluorescence nano microemulsion.
2. according to the method for claim 1, it is characterized in that the mass ratio of isoamyl acetate and ethanol is 3:2.
3. according to the method for claim 1, it is characterized in that the mass ratio of mixing oil phase and Emulsifier EL-60 is 1:3.
4. according to the method for claim 1, it is characterized in that step (1) described temperature is 25 DEG C.
5. according to the method for claim 1, it is characterized in that the mixing speed is 200rpm.
6. according to the method for claim 1, it is characterized in that step (1) mixing time is 20min.
7. according to the method for claim 1, it is characterized in that the gross mass for adding water is the liquid gross mass that step (1) obtains
2.33 times.
8. food-grade fluorescence nano microemulsion prepared by claim 1-7 method.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109329858A (en) * | 2018-09-06 | 2019-02-15 | 天津大学 | A kind of food-grade water-in-oil-in water microemulsion and preparation method |
CN113368046A (en) * | 2021-06-01 | 2021-09-10 | 中国科学院植物研究所 | Oil-in-water-in-oil nano emulsion and preparation method thereof |
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CN101987070A (en) * | 2009-07-31 | 2011-03-23 | 赢创德固赛(中国)投资有限公司 | Oil-in-water microemulsion with high oil-loading quantity |
WO2013059898A1 (en) * | 2011-10-24 | 2013-05-02 | Universidade Federal De Ouro Preto - Ufop | Pharmaceutical compositions containing sesquiterpene lactones belonging to the class of furan heliangolides for the treatment of parasitic infections and tumours |
CN105748408A (en) * | 2014-12-17 | 2016-07-13 | 北京盈科瑞药物研究院有限公司 | Micro-emulsion and micro-emulsion preparation, and preparation methods thereof |
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2017
- 2017-08-22 CN CN201710725874.7A patent/CN107384378A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101987070A (en) * | 2009-07-31 | 2011-03-23 | 赢创德固赛(中国)投资有限公司 | Oil-in-water microemulsion with high oil-loading quantity |
WO2013059898A1 (en) * | 2011-10-24 | 2013-05-02 | Universidade Federal De Ouro Preto - Ufop | Pharmaceutical compositions containing sesquiterpene lactones belonging to the class of furan heliangolides for the treatment of parasitic infections and tumours |
CN105748408A (en) * | 2014-12-17 | 2016-07-13 | 北京盈科瑞药物研究院有限公司 | Micro-emulsion and micro-emulsion preparation, and preparation methods thereof |
Non-Patent Citations (1)
Title |
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MENGNA HOU等: "Novel Fluorescent Microemulsion: Probing Properties, Investigating Mechanism, and Unveiling Potential Application", 《ACS APPL. MATER. INTERFACES》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109329858A (en) * | 2018-09-06 | 2019-02-15 | 天津大学 | A kind of food-grade water-in-oil-in water microemulsion and preparation method |
CN109329858B (en) * | 2018-09-06 | 2021-12-28 | 天津大学 | Food-grade water-in-oil-in-water microemulsion and preparation method thereof |
CN113368046A (en) * | 2021-06-01 | 2021-09-10 | 中国科学院植物研究所 | Oil-in-water-in-oil nano emulsion and preparation method thereof |
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Application publication date: 20171124 |