CN105686974A - Emulsion gel induced by natural amphiphilic small molecules and quick preparation method thereof - Google Patents
Emulsion gel induced by natural amphiphilic small molecules and quick preparation method thereof Download PDFInfo
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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Abstract
The invention discloses emulsion gel induced by natural amphiphilic small molecules and a quick preparation method thereof. The quick preparation method comprises the following steps of first uniformly dispersing ammonium glycyrrhetate into water, and heating and agitating an obtained mixture to obtain a transparent ammonium glycyrrhetate solution; afterwards, adding sunflower seed oil into the ammonium glycyrrhetate solution, carrying out homogenization treatment on mixed liquor, and standing the mixed liquor to obtain the emulsion gel. An obtained product is high in oil phase content, is in a solid shape, has favorable plasticity and spreadability, can be subjected to drying treatment, and has oil content which can be up to 98 percent after being dried. The emulsion gel induced by the natural amphiphilic small molecules and the quick preparation method thereof are simple and mild in technical condition, and have industrialized and large-scale application value; the quick continuous production can be carried out; an emulsion gel type product applied to food, a medicine and a cosmetic can be prepared by manipulating a process condition.
Description
Technical field
The present invention relates to emulsion gel, particularly relate to emulsion gel and the fast preparation method thereof of the little molecule induction of a kind of natural amphiphilic；Belong to food, medicine and cosmetics processing technique field。
Technical background
Emulsion gel (emulsiongel) is in the presence of a stabilizer by the gel system constituted with continuous phase foreign minister in dispersion phase, and it receives more and more attention in basic research and practical application as an important product system。Emulsion gel has many different effects and range of application in foods and cosmetics field。
Emulsion gel is utilized to prepare plastic fat goods。Plastic fat is by fluid oil and solid-state fat mixture dimerous, in solid-state under room temperature, is the main component of most of lipid food, including spread, margarine, chocolate, ice cream, shortening and all kinds of bakeries etc.。The function of many plastic fat goods and matter structure are all based on liquid fat can be wrapped in interior fatty crystallite gel networks structure, this network provides necessary structure for the application in food of the functional liquid fat, and imparts plastic fat products machinery characteristic, functional characteristic and special quality。But, traditional plastic fat hydrogenation course of processing can introduce trans fats and saturated fat, and often edible saturated fat and trans fats not only can make the increase of low density lipoprotein, LDL, and can cause and metabolism, disease that cardiovascular is relevant。Cardiovascular and cerebrovascular disease is had good health care and a therapeutical effect by polyunsaturated fatty acid, and can play and make cholesterol esterification thus the effect of the cholesterol levels reduced in blood and liver。But, unsaturated fatty acids is present in fluid oil more, and fluid oil does not have the network structure of fat crystallization, it is impossible to for structure, local flavor and processing characteristics that lipid food offer plastic fat can be provided by。Therefore, liquid fat, as a kind of structurized method of liquid fat, can be converted into the gel-like structure with viscoelastic properties as the substitute of plastic fat by emulsion gel, makes to utilize unsaturated fatty acids to replace saturated fat and is possibly realized。
Emulsion gel can as the transmission system of carotenoid, plant sterol, fish oil, quintessence oil isoreactivity material and medicine。Active substance in emulsion gel system or drug main to be dissolved in the interior phase oil droplet of emulsion, diffusion between continuous phase microcell in emulsion system can be passed through, reach the purpose of slow release, and significantly improving stability and the biological activity of active substance, this makes the application of emulsion gel to medical science and cosmetic field。In addition, emulsion gel can also limit or stop in food containing fat mutually between the flowing of liquid fat and the generation of migration and improve emulsion intercalation method。
The stabilizer that emulsion gel is conventional has surfactant, solid micro-nano granules etc.。In recent years, the concern of research worker is increasingly received based on the emulsion gel of little molecular gel agent, it has several advantage: (1) little molecule by intermolecular weak non-covalent bond effect generation self assembly, can be upwardly formed longer threadiness, tubulose or helicoidal structure at one-dimensional square。Disperse medium, again through Mechanical entanglement or the formation space three-dimensional network structure that overlaps each other, is caught in this space structure, is made liquid in microcell be in first valve state by surface tension by these structures；(2) vegetable oil of liquid (≤2wt%) can be carried out structuring and immobilization by little molecular gel system under low concentration；(3) having good gel-sol phase in version reversibility, this reversible phase transition process can pass through the effect induction such as heating, optical, electrical, ultrasonic, shearing stimulation, oxidoreduction or control；(4) dispersed phase volume fraction can without consecutive variations between dispersion phase and dispersion phase maximum volume mark。Monoglyceride is the small-molecule substance with emulsibility and self-assembly property being most commonly used for preparing emulsion gel, Heertje{HeertjeI, HendrickxHA, KnoopsAJ, etal.Useofmesomorphicphasesinfoodproducts:US, US6368652 [P] .2002.} and Batte{BatteHD, WrightAJ, RushJW, etal.Effectofprocessingconditionsonthestructureofmonoste arin oil watergels [J] .FoodResearchInternational, 2007, it has been done a lot of research by 40 (40): 982-988.}, but α-gel phase is thermodynamic instability, denser gel phase can be converted into over time, reduce the space between monoglyceride bilayer, cause that water is discharged, adding sodium stearoyl lactate could stable alpha-gel phase。
Summary of the invention
It is an object of the invention to overcome the shortcoming of prior art, it is provided that a kind of quick preparation is by the method for the emulsion gel of the little molecule induction of natural amphiphilic。
The present invention is from molecular structure angle and nutrition and health perspectives, utilize amphiphilic nature and the gelling ability of natural small molecule glycyrrhizic acid, oil phase content height is prepared by manipulating simple process conditions, the emulsion gel of the characteristics such as shape and good plasticity, the smear with solid, this product property is stable, can be dried process。
Glycyrrhizic acid is a kind of natural small molecule, is the main component of Radix Glycyrrhizae, has high sugariness, low calorie, safety non-toxic and stronger medicinal health care function。The industries such as food, cosmetics, medicine are sold and be applied to glycyrrhizic acid mainly in a salt form in the market, for instance ammonium glycyrrhizinate, it can dissociate after being dissolved in water further, exists in solution with the form of glycyrrhizic acid。Glycyrrhizic acid molecule is made up of a hydrophobic triterpene aglycone (18 β-enoxolone) and two hydrophilic glucuronic acids。Owing to having hydrophilic and hydrophobic part simultaneously, glycyrrhizic acid has amphipathic, has the self assembly behavior of complexity in water。Finding according to the study, the self assembly of glycyrrhizic acid is relevant to concentration, along with the increase of glycyrrhizic acid concentration can gradually form hydrogel。Therefore, the glycyrrhizic acid simultaneously with emulsifying and gelling ability is a kind of ideal lipid structures auxiliary agent。At present, in the research both at home and abroad in this field, do not find the research report utilizing natural glycyrrhizic acid to carry out structured liquid oils and fats。
The purpose of the present invention is achieved through the following technical solutions:
A kind of method of quick emulsion gel preparing the little molecule induction of natural amphiphilic, comprises the steps:
1) ammonium glycyrrhizinate is dispersed in water, after heated and stirred, obtains transparent ammonium glycyrrhizinate solution；
2) Oleum Helianthi is added in ammonium glycyrrhizinate solution, this mixed liquor is carried out homogenizing process, after standing, obtain emulsion gel。
For realizing the object of the invention further, it is preferable that described ammonium glycyrrhizinate solution concentration is 0.5-6wt%。
Preferably, the time of described heated and stirred is 10-30min。
Preferably, the final concentration of 10-60wt% of Oleum Helianthi in emulsion gel。
Preferably, after Oleum Helianthi adds ammonium glycyrrhizinate solution to, before carrying out homogenizing process, also including mixed liquor is carried out heating in water bath process, treatment temperature is 70-90 DEG C, and the process time is 10-30min。
Preferably, the speed of ammonium glycyrrhizinate and Oleum Helianthi mixed liquor homogenizing is 11500-30000rpm, and the time of homogenizing is 2-5min。
Preferably, the temperature of described standing is 4 DEG C-25 DEG C。
Preferably, the time of described standing is 6-24h。
Preferably, the emulsion gel of described acquisition also includes being dried process。The method of described dried is lyophilization。
The emulsion gel of the little molecule induction of a kind of natural amphiphilic, is prepared by said method。The emulsion gel of natural amphiphilic little molecule induction prepared by the present invention is milky white shape, has the cool taste of Oleum Helianthi。Emulsion gel is made to have shape and good plasticity, the smear of solid with ammonium glycyrrhizinate for the three-dimensional net structure that support builds。The viscoelastic properties of emulsion gel can be manipulated by different ammonium glycyrrhizinate concentration, oil content and preparation condition, can application and preparation emulsion gel product in different food products and cosmetics。
The principle of the invention: the present invention it is critical only that the amphiphilic nature that make use of natural small molecule glycyrrhizic acid cleverly and gelling ability are to prepare emulsion gel。First make glycyrrhizic acid molecule spontaneously be adsorbed on oil-water interface by high speed homogenization under glycyrrhizic acid concentration is more than its critical plastic concentration conditions, reduce surface tension, form emulsion oil-in-water；Reduction along with temperature, glycyrrhizic acid in body phase and oil-water interface can pass through non-covalent intermolecular key active force (hydrophobic interaction, hydrogen bond) and orderly self assembly occurs, form long fibre shape micro structure, these micro structures assemble formation space three-dimensional network further, therefore emulsion oil droplets is all fixed in the three-dimensional net structure of formation in an orderly manner, ultimately forms emulsion gel。
Relative to prior art, the invention have the advantages that and beneficial effect:
1, the invention provides the natural material of a kind of novel structured lipid, fluid oil is carried out structuring by the ingenious amphipathic and gelling ability utilizing little molecule glycyrrhizic acid under low concentration, expands emulsion gel practical application in foods and cosmetics field。
2, present invention process condition is simply gentle, is not related to the chemical compositions such as poisonous and hazardous reagent and emulsifying agent, green safety；And quick continuous prodution can be carried out, simple manipulation process condition application and preparation emulsion gel product in different food products and cosmetics can be passed through, there is the using value of industrialization and scale。
3, the emulsion gel product unsaturated fatty acids content that prepared by the present invention is high, the characteristics such as shape and good plasticity, the smear with solid, and can be used for load vitamin E, plant sterol, fish oil, quintessence oil isoreactivity material, make lipid food or cosmetics etc. have corresponding functional characteristic further。
Accompanying drawing explanation
Fig. 1 a is the apparent figure of emulsion gel under the different ammonium glycyrrhizinate concentration of embodiment 1。
Fig. 1 b is the little amplitude dynamic frequency scanning figure of emulsion gel under the different ammonium glycyrrhizinate concentration of embodiment 2。
Fig. 1 c is the smear of emulsion gel under the different ammonium glycyrrhizinate concentration of embodiment 1。
Fig. 2 a is the apparent figure of emulsion gel under the different Oleum Helianthi concentration of embodiment 2。
Fig. 2 b is the little amplitude dynamic frequency scanning figure of emulsion gel under the different Oleum Helianthi concentration of embodiment 2。
Fig. 3 heats before embodiment 3 Oleum Helianthi homogenizing and the little amplitude dynamic frequency scanning figure of not heating condition stimulating milk secretion lyogel。
Fig. 4 is the little amplitude dynamic frequency scanning figure of emulsion gel under the different homogenizing speed of embodiment 4。
Fig. 5 is that embodiment 5 is different places the little amplitude dynamic frequency scanning figure of emulsion gel at temperature。
Fig. 6 is the apparent figure of emulsion gel under embodiment 6 different dry drying method。
Detailed description of the invention
For being more fully understood that the present invention, below in conjunction with drawings and Examples, the invention will be further described, but embodiments of the present invention are not limit so。
In following embodiment, rheol assay method is as follows:
Ftheoloqical measurements: adopt little variable rheology analysis that the rheological property of condensation product is analyzed。Emulsion gel is placed in flow graph sample stage, selects parallel-plate to test。The gap of sample stage and parallel-plate is 1mm。First at record 25 DEG C sample with the elastic modelling quantity (G') of strain variation and viscous modulus value (G ")；It is then determined that strain is positioned at the modulus range of linearity of sample condensation product when being 0.01%, then sample is performed a scan, records G' and G " with the trend of frequency change。
Embodiment 1
Being dispersed in 5 parts of deionized waters respectively by 5 parts of ammonium glycyrrhizinates, at 80 DEG C, heated and stirred 30min obtains the clear solution of concentration respectively 0.5wt%, 1wt%, 2wt%, 4wt% and 6wt%。Oleum Helianthi is added separately in the ammonium glycyrrhizinate solution of variable concentrations, controls Oleum Helianthi concentration and be 60wt%, 80 DEG C of heating in water bath 30min。Mixed liquor is carried out homogenizing process, homogenizing 2min under 20500rpm speed。It is placed at 25 DEG C after 12h to obtain the emulsion gel of the little molecule induction of natural amphiphilic。
From the preparation method of embodiment it will be seen that the present invention is not related to any poisonous and hazardous raw material and reagent, the green safety of product own；And the course of processing is easy and simple to handle, it is not necessary to use large-scale and complicated device, it is simple to carry out quick continuous prodution。
Plasticity is the most basic characteristic of emulsion gel shape fatty foodstuff or cosmetics。In plastic fat product, the factor such as size of solid fats content and crystalline particle determines its plasticity, and in the present invention, liquid fat is carried out structuring as derivant by glycyrrhizic acid molecule, and in the emulsion gel system therefore formed, the content of ammonium glycyrrhizinate decides the plasticity of product。
In embodiment 1, Fig. 1 a is the apparent figure of ammonium glycyrrhizinate concentration respectively 0.5wt%, 1wt%, 2wt%, 4wt% and 6wt% emulsion gel。As seen from the figure when ammonium glycyrrhizinate concentration is lower than 2wt%, system can not form gel, apparent in flowable state。When ammonium glycyrrhizinate concentration is higher than 2wt%, the stable O/w emulsion of ammonium glycyrrhizinate can form emulsion gel under 25 DEG C of conditions, gel is milky white shape, has the cool taste of Oleum Helianthi, illustrates that starting ammonium glycyrrhizinate from 2wt% concentration can catch oil droplet its space structure completely。The vegetable oil of liquid (≤2wt%) can be carried out structuring and immobilization by visible ammonium glycyrrhizinate gel rubber system under low concentration；But owing to ammonium glycyrrhizinate concentration is high during higher than 6wt%, it is easy to gelling in emulsion gel preparation process, is therefore not easy to preparation。
The functional characteristic of emulsion gel shape fatty foodstuff or cosmetics and processing characteristics are mainly reflected in its mechanical performance, and wherein rheological properties (ability of opposing small deformation) is embodied by the viscoelastic modulus of product。G' value represents the storage of energy in each deformation circulation, the elasticity of reaction sample and class solid property, G " viscosity of value then response sample and fluid-like state character。Fig. 1 b is the little amplitude dynamic frequency scanning figure of ammonium glycyrrhizinate concentration respectively 0.5wt%, 1wt%, 2wt%, 4wt% and 6wt% emulsion gel。As seen from the figure, when ammonium glycyrrhizinate concentration is within the scope of 2-6wt%, G' value is all higher than G in frequency sweeping ranges " value, it is seen that emulsion gel is mainly deformed elastically, in solid-state。It addition, elastic modelling quantity improves along with the raising of ammonium glycyrrhizinate concentration, illustrate that the intensity of emulsion gel constantly strengthens。This is because ammonium glycyrrhizinate content is more high in the grease gel of unit volume, it is possible to the molecular amounts participating in three-dimensional net structure structure is also more many, then the structuring degree of this emulsion gel is also more high。
Ammonium glycyrrhizinate concentration owing to ammonium glycyrrhizinate concentration is high higher than 6wt%, being easy to gelling in emulsion gel preparation process, being therefore not easy to preparation, so not detecting。When ammonium glycyrrhizinate concentration is lower than 2wt%, owing to system can not form gel, apparent in flowable state, it is not suitable for when identical rheology and detects。
2% and 4% emulsion gel sample is taken out and carries out smearing the apparent figure obtained on plate by Fig. 1 c。As seen from the figure, product of the present invention is creamy white, and has shape and good plasticity, the smear of solid, can pass through simple manipulation different condition application and preparation emulsion gel product in different food products and cosmetics。
Utilize emulsion gel prepared by ammonium glycyrrhizinate can meet consumer to the demand without satisfied fatty acid and trans fatty acid food, fluid oil structuring is made it have the structure of solid-state and form and there is the trophism of fluid oil, the fatty foodstuff such as spread, chocolate cream can be applied in；And can load vitamin E, carotenoid, plant sterol, fish oil isoreactivity material, be applied in functional food；Simultaneously in cosmetics, medicine and other fields, this emulsion gel also has great application prospect, and its mechanical property shown and functional characteristic can as external facial cream and ointment for these fields。
Key to the invention is that the self assembly characteristic that make use of glycyrrhizic acid dexterously, i.e. amphiphilic nature and gelling ability, prepare emulsion gel type product；As material itself, glycyrrhizic acid is very ripe and is widely used in the industries such as food, cosmetics, medicine: in field of food, can being used safely in sweetmeats made of fruit and sugar, confection, soft drink, canned meat etc. by GB2760 2014 regulation, need appropriate use by producing, safety is high；In cosmetic field, glycyrrhizic acid has compatibility widely in cosmetics, often shared with other activating agents, can accelerate skin potentiation to their absorption, can be used for sun-proof, brighten, nurse one's health, antipruritic and hair-growing and hair care etc.。All with the addition of natural whiting composition in current many whitening and speckle dispelling products, the natural component wherein employed up to is Radix Glycyrrhizae extract and placenta extracting liquid。Added with Radix Glycyrrhizae elite in Nivea whitening and protective day cream；Added with Radix Glycyrrhizae elite, Semen Vitis viniferae extracting solution, Mulberry Roots and natural algae in the white paste formulation of the natural profit of Yue-Sai；Avon whitening series of products also contain Radix Glycyrrhizae extract, Placenta extract；The whitening and skin-protecting dew that Christian Dior (Shanghai) produces vitamin C, arbutin and 3 kinds of whitening compositions of glycyrrhetate have been simultaneously introduced。The present invention is mainly from glycyrrhizic acid molecule structure, utilize its amphipathic structure and in aqueous phase, be self-assembled into the ability of fiber gel, these characteristics are generalized on oil-water interfaces, it has been found that it exists the energy of oil-water interfaces plastic, thus preparing the emulsion gel induced by glycyrrhizic acid first；And it is simple to invent the preparation condition related to, it is easy to carry out industrialized production。
Embodiment 2
Ammonium glycyrrhizinate is dispersed in deionized water, heated and stirred 20min at 70 DEG C, obtain the transparent ammonium glycyrrhizinate solution that concentration is 2wt%。Oleum Helianthi is added in ammonium glycyrrhizinate solution, controls Oleum Helianthi concentration respectively 10wt%, 20wt%, 40wt% and 60wt%, 70 DEG C of heating in water bath 20min。Mixed liquor is carried out homogenizing process, homogenizing 3min under 20500rpm speed。It is placed at 25 DEG C after 24h to obtain the emulsion gel of the little molecule induction of natural amphiphilic。
Fig. 2 a is the apparent figure of Oleum Helianthi concentration respectively 10wt%, 20wt%, 40wt% and 60wt% emulsion gel。As seen from the figure as Oleum Helianthi concentration respectively 10wt%, 20wt%, 40wt%, the stable O/w emulsion of ammonium glycyrrhizinate produces significantly to be separated。This is owing to only part ammonium glycyrrhizinate is adsorbed on the oil droplets of rareness, continuous phase exists the ammonium glycyrrhizinate not adsorbed in a large number, continuous phase is different with dispersion phase density causes that in emulsion, oil droplet overcomes gravity to float, and upper strata forms emulsion gel layer, and lower floor forms ammonium glycyrrhizinate gel layer。When oil concentration increases to 60wt%, O/w emulsion does not produce layering, it is possible to form the emulsion gel of even structure。
Fig. 2 b is the little amplitude dynamic frequency scanning figure of Oleum Helianthi concentration respectively 10wt%, 20wt%, 40wt% and 60wt% emulsion gel。As seen from the figure, when Oleum Helianthi concentration is within the scope of 10-60wt%, along with the raising of oil concentration, elastic modelling quantity also improves。Illustrating that the viscoelasticity of emulsion gel is limited primarily by the impact of implant, the liquid fat concentration as active fillers is more high, and more polydisperse oil droplet is embedded or is integrated into gel network, makes gel strength higher。
Embodiment 3
Being dispersed in deionized water by ammonium glycyrrhizinate, at 90 DEG C, heated and stirred 10min obtains the clear solution that concentration is 2wt%。Be added to by Oleum Helianthi in ammonium glycyrrhizinate solution making oil concentration is after 60wt%, mixed liquor is carried out homogenizing process, homogenizing 4min under 20500rpm speed at once。It is placed at 25 DEG C after 6h to obtain the emulsion gel of the little molecule induction of natural amphiphilic。
Fig. 3 heats before Oleum Helianthi homogenizing and the little amplitude dynamic frequency scanning figure of not heating condition stimulating milk secretion lyogel。As seen from the figure, Oleum Helianthi carries out homogenizing again after heating and can improve the intensity of emulsion gel。Oil carries out homogenizing again after heating can improve the intensity of emulsion gel。Because the formation of ammonium glycyrrhizinate gel is very sensitive to ambient temperature。The reduction of system temperature can promote that the self assembly of ammonium glycyrrhizinate affects the emulsifying capacity in homogenizing process to oils and fats。
Embodiment 4
Being dispersed in deionized water by ammonium glycyrrhizinate, at 80 DEG C, heated and stirred 10min obtains the clear solution that concentration is 2wt%。Be added to by Oleum Helianthi in ammonium glycyrrhizinate solution making oil concentration is 60wt%, 80 DEG C of heating in water bath 10min。Mixed liquor is carried out homogenizing process, homogenizing 2min under speed respectively 11500rpm, 14500rpm, 20500rpm, 30000rpm。It is placed at 25 DEG C after 12h to obtain the emulsion gel of the little molecule induction of natural amphiphilic。
Fig. 4 is the little amplitude dynamic frequency scanning figure of emulsion gel under different homogenizing speed。As seen from the figure, being within the scope of 11500-20500rpm in homogenizing speed, the elastic modelling quantity of emulsion gel increases along with the raising of homogenizing speed。This is that oil droplet can be embedded better or be integrated into gel network, and the emulsion gel structure making formation is tightr owing to the raising of homogenizing speed can make liquid fat more uniformly be dispersed in ammonium glycyrrhizinate solution。
Embodiment 5
Being dispersed in deionized water by ammonium glycyrrhizinate, at 80 DEG C, heated and stirred 20min obtains the clear solution that concentration is 2wt%。Be added to by Oleum Helianthi in ammonium glycyrrhizinate solution making oil concentration is 60wt%, 80 DEG C of heating in water bath 20min。Mixed liquor is carried out homogenizing process, homogenizing 5min under 20500rpm speed。It is respectively placed at 4 DEG C and 25 DEG C after 12h to obtain the emulsion gel of the little molecule induction of natural amphiphilic。
Fig. 5 is the little amplitude dynamic frequency scanning figure of emulsion gel at different placement temperature。As seen from the figure, under 4 DEG C of conditions, the viscoelastic modulus of emulsion gel is above 25 DEG C。The formation of emulsion gel is the process of a thermodynamical equilibrium。Difference between gelling temperature and the melt temperature of gel is more big more is conducive to the formation of gel。
Embodiment 6
Being dispersed in deionized water by ammonium glycyrrhizinate, at 80 DEG C, heated and stirred 30min obtains the clear solution that concentration is 2wt%。Be added to by Oleum Helianthi in ammonium glycyrrhizinate solution making oil concentration is 60wt%, 80 DEG C of heating in water bath 30min。Mixed liquor is carried out homogenizing process, homogenizing 2min under 20500rpm speed。Being placed at 4 DEG C and obtain, after 24h, the emulsion gel that the little molecule of natural amphiphilic is induced, this product can be dried process。
Fig. 6 is the apparent figure of emulsion gel under different dry drying method。As seen from the figure, emulsion gel is after lyophilization, remain in that good structure, oils and fats is not had to precipitate out, although illustrating that, in dehydration, between oil droplet, gap is more and more less, different oil droplets can tightly link together, but ammonium glycyrrhizinate molecule can remain stable all the time, it is ensured that is not polymerized between adjacent oil droplet。The product oil content obtained after dried is up to 98%。
Embodiments of the present invention are also not restricted to the described embodiments, the change made under other any spirit without departing from the present invention and principle, modification, replacement, combination, simplification, all should be the substitute mode of equivalence, are included in protection scope of the present invention。
Claims (10)
1. the method for the quick emulsion gel preparing the little molecule induction of natural amphiphilic, it is characterised in that comprise the steps:
1) ammonium glycyrrhizinate is dispersed in water, after heated and stirred, obtains transparent ammonium glycyrrhizinate solution；
2) Oleum Helianthi is added in ammonium glycyrrhizinate solution, this mixed liquor is carried out homogenizing process, after standing, obtain emulsion gel。
2. the method for the quick emulsion gel preparing the little molecule induction of natural amphiphilic according to claim 1, it is characterised in that described ammonium glycyrrhizinate solution concentration is 0.5-6wt%。
3. the method for the quick emulsion gel preparing the little molecule induction of natural amphiphilic according to claim 1, it is characterised in that the time of described heated and stirred is 10-30min。
4. the method for the quick emulsion gel preparing the little molecule induction of natural amphiphilic according to claim 1, it is characterised in that the final concentration of 10-60wt% of Oleum Helianthi in emulsion gel。
5. the method for the quick emulsion gel preparing the little molecule induction of natural amphiphilic according to claim 1, it is characterized in that, after Oleum Helianthi adds ammonium glycyrrhizinate solution to, before carrying out homogenizing process, also include mixed liquor is carried out heating in water bath process, treatment temperature is 70-90 DEG C, and the process time is 10-30min。
6. the method for the quick emulsion gel preparing the little molecule induction of natural amphiphilic according to claim 1, it is characterised in that the speed of ammonium glycyrrhizinate and Oleum Helianthi mixed liquor homogenizing is 11500-30000rpm, and the time of homogenizing is 2-5min。
7. the method for the quick emulsion gel preparing the little molecule induction of natural amphiphilic according to claim 1, it is characterised in that the temperature of described standing is 4 DEG C-25 DEG C。
8. the method for the quick emulsion gel preparing the little molecule induction of natural amphiphilic according to claim 1, it is characterised in that the time of described standing is 6-24h。
9. the method for the quick emulsion gel preparing the little molecule induction of natural amphiphilic according to claim 1, it is characterised in that the emulsion gel of described acquisition also includes being dried process, and the method for described dried is lyophilization。
10. the emulsion gel of the little molecule induction of natural amphiphilic, it is characterised in that prepared by its method described in any one of claim 1-9。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110507596A (en) * | 2019-09-29 | 2019-11-29 | 华南理工大学 | Using milk as the oil-in-water type gel emulsion and its fast preparation method of matrix |
| CN111840653A (en) * | 2020-05-27 | 2020-10-30 | 华南理工大学 | Glycyrrhetinic acid base slow-release porous foam material capable of embedding hydrophilic functional factors and preparation method and application thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52139710A (en) * | 1976-05-15 | 1977-11-21 | Morita Kagaku Kogyo | Isolation of glycyrrhizin |
| JPS58163429A (en) * | 1982-03-20 | 1983-09-28 | Shiseido Co Ltd | Emulsifier composition |
| CN1068731A (en) * | 1991-07-25 | 1993-02-10 | 蜜丝佛陀株式会社 | Cosmetic gel |
| CN1650877A (en) * | 2004-12-09 | 2005-08-10 | 中国药科大学 | Slow release preparation of diammonium glycyrrhizate |
-
2016
- 2016-01-26 CN CN201610051180.5A patent/CN105686974B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52139710A (en) * | 1976-05-15 | 1977-11-21 | Morita Kagaku Kogyo | Isolation of glycyrrhizin |
| JPS58163429A (en) * | 1982-03-20 | 1983-09-28 | Shiseido Co Ltd | Emulsifier composition |
| CN1068731A (en) * | 1991-07-25 | 1993-02-10 | 蜜丝佛陀株式会社 | Cosmetic gel |
| CN1650877A (en) * | 2004-12-09 | 2005-08-10 | 中国药科大学 | Slow release preparation of diammonium glycyrrhizate |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110507596A (en) * | 2019-09-29 | 2019-11-29 | 华南理工大学 | Using milk as the oil-in-water type gel emulsion and its fast preparation method of matrix |
| CN111840653A (en) * | 2020-05-27 | 2020-10-30 | 华南理工大学 | Glycyrrhetinic acid base slow-release porous foam material capable of embedding hydrophilic functional factors and preparation method and application thereof |
| CN111840653B (en) * | 2020-05-27 | 2021-07-20 | 华南理工大学 | Glycyrrhetinic acid base slow-release porous foam material capable of embedding hydrophilic functional factors and preparation method and application thereof |
| CN112889931A (en) * | 2021-02-23 | 2021-06-04 | 江南大学 | Zero-trans/low-saturated fatty acid fatty emulsion glue and application |
| CN112889931B (en) * | 2021-02-23 | 2023-01-31 | 江南大学 | Zero-trans/low-saturated fatty acid fatty emulsion glue and application |
| CN113349420A (en) * | 2021-07-16 | 2021-09-07 | 山东大学 | Multi-stimulus responsive cigarette blasting bead, preparation thereof and application thereof in controllable release of essence |
| CN114532413A (en) * | 2022-02-15 | 2022-05-27 | 江南大学 | Emulsion gel for 3D printing of fat substitute and preparation method thereof |
| CN114557440A (en) * | 2022-02-15 | 2022-05-31 | 江南大学 | Stable zein-glycyrrhizic acid-chitosan Pickering emulsion gel and preparation method thereof |
| WO2023155933A1 (en) * | 2022-02-15 | 2023-08-24 | 江南大学 | Emulsion gel for 3d printing of fat substitute, and preparation method therefor |
| CN116272699A (en) * | 2023-02-20 | 2023-06-23 | 华南理工大学 | Thermosensitive biphase structured emulsion gel and preparation method and application thereof |
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