CN115429721B - Essential oil nanoemulsion and preparation method thereof - Google Patents
Essential oil nanoemulsion and preparation method thereof Download PDFInfo
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 133
- 239000007908 nanoemulsion Substances 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 240000000560 Citrus x paradisi Species 0.000 claims abstract description 67
- 239000004094 surface-active agent Substances 0.000 claims abstract description 61
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 claims abstract description 24
- 235000011067 sorbitan monolaureate Nutrition 0.000 claims abstract description 24
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims abstract description 23
- 229920000053 polysorbate 80 Polymers 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 235000011187 glycerol Nutrition 0.000 claims abstract description 9
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 229960004063 propylene glycol Drugs 0.000 claims abstract description 6
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims abstract description 3
- 235000013772 propylene glycol Nutrition 0.000 claims abstract description 3
- 230000007547 defect Effects 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 description 47
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- 238000003860 storage Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
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- 239000003921 oil Substances 0.000 description 9
- 230000007774 longterm Effects 0.000 description 8
- 238000000265 homogenisation Methods 0.000 description 7
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- 239000004530 micro-emulsion Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
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- UAHWPYUMFXYFJY-UHFFFAOYSA-N beta-myrcene Chemical compound CC(C)=CCCC(=C)C=C UAHWPYUMFXYFJY-UHFFFAOYSA-N 0.000 description 2
- NEHNMFOYXAPHSD-UHFFFAOYSA-N citronellal Chemical compound O=CCC(C)CCC=C(C)C NEHNMFOYXAPHSD-UHFFFAOYSA-N 0.000 description 2
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- 230000005484 gravity Effects 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- NDVASEGYNIMXJL-UHFFFAOYSA-N sabinene Chemical compound C=C1CCC2(C(C)C)C1C2 NDVASEGYNIMXJL-UHFFFAOYSA-N 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229930006978 terpinene Natural products 0.000 description 2
- 150000003507 terpinene derivatives Chemical class 0.000 description 2
- NDVASEGYNIMXJL-NXEZZACHSA-N (+)-sabinene Natural products C=C1CC[C@@]2(C(C)C)[C@@H]1C2 NDVASEGYNIMXJL-NXEZZACHSA-N 0.000 description 1
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 description 1
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
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- GLZPCOQZEFWAFX-YFHOEESVSA-N Geraniol Natural products CC(C)=CCC\C(C)=C/CO GLZPCOQZEFWAFX-YFHOEESVSA-N 0.000 description 1
- 239000005792 Geraniol Substances 0.000 description 1
- 244000020551 Helianthus annuus Species 0.000 description 1
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- 208000008589 Obesity Diseases 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 229920001213 Polysorbate 20 Polymers 0.000 description 1
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 1
- VYBREYKSZAROCT-UHFFFAOYSA-N alpha-myrcene Natural products CC(=C)CCCC(=C)C=C VYBREYKSZAROCT-UHFFFAOYSA-N 0.000 description 1
- KQAZVFVOEIRWHN-UHFFFAOYSA-N alpha-thujene Natural products CC1=CCC2(C(C)C)C1C2 KQAZVFVOEIRWHN-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 206010006451 bronchitis Diseases 0.000 description 1
- 238000005537 brownian motion Methods 0.000 description 1
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- 235000009508 confectionery Nutrition 0.000 description 1
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- 229940113087 geraniol Drugs 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 229930007744 linalool Natural products 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
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- 239000002105 nanoparticle Substances 0.000 description 1
- 239000012875 nonionic emulsifier Substances 0.000 description 1
- 235000020824 obesity Nutrition 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 229930006696 sabinene Natural products 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/068—Microemulsions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4993—Derivatives containing from 2 to 10 oxyalkylene groups
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/21—Emulsions characterized by droplet sizes below 1 micron
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/596—Mixtures of surface active compounds
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Abstract
The invention relates to an essential oil nanoemulsion and a preparation method thereof, and belongs to the technical field of daily chemical products. The invention relates to a preparation method of grapefruit essential oil nanoemulsion, which is characterized by comprising the following steps of: (1) Uniformly mixing a surfactant to obtain a mixed solution A; the surfactant comprises a surfactant A and a surfactant B, wherein the surfactant A comprises span 20 and Tween 80, and the surfactant B comprises at least one of glycerol and 1, 2-propanediol; (2) Adding essential oil into the mixed solution A in the step (1), and uniformly stirring to obtain a mixed solution B; (3) Adding water into the mixed solution B in the step (2), uniformly stirring, and homogenizing to obtain the essential oil nanoemulsion. The essential oil nanoemulsion prepared by the method effectively solves the defect that essential oil is easy to volatilize, and has good physicochemical property and stability.
Description
Technical Field
The invention relates to the technical field of daily chemical products, in particular to essential oil nanoemulsion and a preparation method thereof.
Background
The grapefruit is cool and sweet in nature, has the effects of clearing heat and quenching thirst, is obtained by squeezing peel, can nourish tissue cells, increase physical strength, relieve bronchitis, improve diseases such as obesity, edema and lymph gland system, has wide medical care effect and a certain beautifying effect, and comprises main chemical components of pinene or pinene, sabinene, myrcene, limonene, geraniol, linalool, citronellal, sunflower acetate and terpinene or terpinene. However, the grapefruit essential oil has high volatility, so that the action time is short, and the effect is difficult to effectively play. In order to prolong the action time of the grapefruit essential oil and strengthen the action effect of the grapefruit essential oil, the preparation of the grapefruit essential oil into emulsion is a main research direction. Nanoemulsions are one of the microemulsion systems and are commonly prepared by a phase inversion emulsification method. The phase inversion emulsification method is to add water/oil type emulsifier into oil phase to make it dissolve or disperse uniformly, and to add water phase under the condition of continuous stirring. Initially, the surfactant-containing oil phase has a small amount of water, and as the system changes to a surfactant-oil-water liquid crystal transition phase, the water phase surrounds the oil phase as the water phase continues to increase, becoming a continuous phase. With the continuous increase of the water adding amount, the continuous phase is changed from the oil phase to the water phase, and the oil/water type microemulsion is formed.
However, the operation of preparing the grapefruit essential oil emulsion by the inversion emulsion method is simple, but the performance of the microemulsion prepared by the method is influenced by factors such as the size of liquid drops, the type and the addition amount of the surfactant, the hydrophilic and hydrophobic balance value and the like. At present, the field has the main problems of harsh requirements of emulsifying agents, unstable physicochemical properties of emulsion and the like. Therefore, there is an urgent need to develop a grapefruit essential oil nanoemulsion that is not volatile, has good physicochemical properties, and still has good stability for long-term storage.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the essential oil nanoemulsion which is not easy to volatilize, has good physicochemical properties and still has good stability after long-term storage.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
In a first aspect, the invention provides a preparation method of an essential oil nanoemulsion, which comprises the following steps:
(1) Uniformly mixing a surfactant to obtain a mixed solution A; the surfactant comprises a surfactant A and a surfactant B, wherein the surfactant A comprises span 20 and Tween 80, and the surfactant B comprises at least one of glycerol and 1, 2-propylene glycol;
(2) Adding essential oil into the mixed solution A in the step (1), and uniformly stirring to obtain a mixed solution B;
(3) Adding water into the mixed solution B in the step (2), uniformly stirring, and homogenizing to obtain the essential oil nanoemulsion.
The inventor of the invention finds that span and tween are taken as small molecular emulsifying agents in a large number of surfactant researches, the span has strong capability of reducing the surface tension of oil-water interface tension, the span has lipophilicity, the tween has hydrophilicity, glycerol or 1, 2-propanediol is added in the emulsification process to form a compound surfactant together with span 20 and tween 80 for emulsification, on one hand, an adsorption layer can be formed on the oil-water interface, the stability of dispersing nonpolar molecules or solvents in aqueous solution can be increased, and the prepared essential oil nanoemulsion has good physicochemical property of emulsion; on the other hand, the glycerol or the 1, 2-propylene glycol can also change the surface activity and the hydrophilic and lipophilic balance of span 20 and tween 80, adjust the polarity of water and oil, and is favorable for preparing the small-particle essential oil nanoemulsion, so that the small-particle essential oil nanoemulsion overcomes the action of gravity, prevents emulsion separation layering phenomenon caused by aggregation or gravity, and enables the essential oil nanoemulsion to form a uniform system and to have better stability. And the product prepared by singly using span or tween surfactant can not have the tyndall effect or has poor physicochemical property and stability. In addition, other surfactants are adopted for compounding, so that the prepared essential oil nanoemulsion has the defects of larger particles, higher polymer dispersion index, lower Zeta potential and the like, and is not beneficial to long-term storage of the essential oil nanoemulsion.
As a preferred embodiment of the method for preparing an essential oil nanoemulsion, in the step (1), the mass ratio of the surfactant a to the surfactant B is surfactant a: surfactant b=1, (3-5).
As a preferred embodiment of the method for preparing an essential oil nanoemulsion, in the step (1), the mass ratio of the surfactant a to the surfactant B is surfactant a: surfactant b=1:4.
As a preferred embodiment of the preparation method of the essential oil nanoemulsion, in the step (1), the mass ratio of span 20 to tween 80 is span 20: tween 80= (2-5): 5.
The research shows that under the condition that the dosage of the surfactant is certain, the mass ratio of span 20 and tween 80 in the range is changed, so that the polydispersion coefficient of the grapefruit essential oil nanoemulsion is reduced and kept below 0.25, and the flocculation phenomenon of the liquid drops caused by the aggregation of brownian motion due to the fact that the liquid drops with different particle sizes in the emulsion are emulsified at different speeds can be effectively avoided due to the fact that the particle size distribution is uniform, so that the grapefruit essential oil nanoemulsion has better stability; the influence of changing the mass ratio of span 20 and tween 80 on the particle size and Zeta potential absolute value of the grapefruit essential oil nanoemulsion is small, and further proves that the grapefruit essential oil prepared by the surfactant compounded by span 20 and tween 80 has good emulsion physicochemical property under a certain dosage condition. The too small amount of span 20 can affect the water-oil balance of the system, and the particle size obtained by emulsification with essential oil is larger and the dispersion is not uniform, which is not beneficial to the long-term storage stability of the essential oil nanoemulsion.
As a preferred embodiment of the preparation method of the essential oil nanoemulsion, in the step (1), the mass ratio of span 20 to tween 80 is span 20: tween 80=3:5.
In the preferred embodiment of the method for preparing an essential oil nanoemulsion according to the present invention, in the step (2), the essential oil is grapefruit essential oil, and the drip rate of the grapefruit essential oil is (40-80) drops/min.
The research shows that the grapefruit essential oil nanoemulsion provided by the invention effectively overcomes the defect of short acting time caused by the easy volatility of the grapefruit essential oil within the dropping speed range of the grapefruit essential oil, prolongs the acting time of the grapefruit essential oil in the essential oil nanoemulsion, and enhances the acting effect of the grapefruit essential oil.
As a preferred embodiment of the method for preparing an essential oil nanoemulsion, in the step (2), the mass ratio of the essential oil to the surfactant a is: surfactant a=1: (4-5).
The inventor researches find that when the mass ratio of the essential oil to the surfactant is adopted, the performance of small particle size and uniform particle distribution can be better realized, and the oil phase component in the essential oil nanoemulsion is harder to separate out from the essential oil nanoemulsion, and the stability of the essential oil nanoemulsion after long-time storage is better; when the dosage of the essential oil is small, although the particle size of the prepared essential oil nanoemulsion is also small, the particle size is nonuniform, so that nonuniform particles in the essential oil nanoemulsion are more likely to undergo polymerization sedimentation, and the stability of the essential oil nanoemulsion in long-term storage is not facilitated; when the dosage of the essential oil is large, the particles of the essential oil nanoemulsion are enlarged, the Zeta potential of the essential oil nanoemulsion is reduced, and the physicochemical property of the essential oil nanoemulsion is poor.
As a preferred embodiment of the preparation method of the essential oil nanoemulsion, in the step (2), the mass ratio of the essential oil to the surfactant a is: surfactant a=1:5.
In a preferred embodiment of the method for producing an essential oil nanoemulsion according to the present invention, in the step (1), the mixing temperature is 70 to 80 ℃.
The inventor finds that the nonionic emulsifier compounded by span 20 and Tween 80 surfactant is beneficial to phase inversion emulsification with the grapefruit essential oil according to the invention when the temperature range reaches the vicinity of the phase inversion temperature, and the prepared grapefruit essential oil nanoemulsion has uniform particles and smaller particle size.
As a preferred embodiment of the method for preparing an essential oil nanoemulsion according to the present invention, in the step (1), the temperature of the mixing is 80 ℃.
In the preferred embodiment of the method for preparing an essential oil nanoemulsion according to the present invention, in the step (3), the homogenizing time is 4 to 6 minutes, and the homogenizing power is 240 to 280W.
As a preferred embodiment of the method for preparing an essential oil nanoemulsion, in the step (3), the homogenizing time is 5min, and the homogenizing power is 240W.
According to the invention, the grapefruit essential oil nanoemulsion with lower particle size and better stability after long-term storage is prepared by combining a phase inversion emulsification method and a homogenization method, and the homogenization time and the homogenization power are controlled within the ranges, so that the complete emulsification reaction of the grapefruit essential oil is facilitated, the incomplete emulsification reaction can be caused by shorter homogenization time or lower homogenization power, the obtained grapefruit essential oil nanoemulsion is more unstable, and the grapefruit essential oil nanoemulsion is unfavorable for long-term storage and poor in stability.
In a second aspect, the present invention provides an essential oil nanoemulsion obtained from a method of preparing an essential oil nanoemulsion.
Compared with the prior art, the invention has the beneficial effects that: the grapefruit essential oil nanoemulsion still has good stability after long-term storage is prepared by combining a phase inversion emulsification method with a homogenization method. The invention adopts span 20, tween 80 and glycerol as surfactants to carry out emulsification reaction, which can effectively reduce aggregation, flocculation and precipitation phenomena of the nano emulsion to a certain extent, and the surfactants form an adsorption layer at an oil-water interface, thereby realizing the increase of emulsion stability. The grapefruit essential oil nanoemulsion prepared by the method effectively solves the defect that grapefruit essential oil is volatile, and has good physicochemical property and stability.
Drawings
FIG. 1 shows particle size values of grapefruit essential oil nanoemulsion of example 1 of the present invention stored at 4deg.C for various times;
FIG. 2 shows particle size values of grapefruit essential oil nanoemulsion of example 1 of the present invention stored at 26℃for various times.
Detailed Description
The technical scheme of the invention is further described below with reference to the embodiment and the attached drawings. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The methods or operations used in the examples, unless specifically indicated, are conventional methods or conventional operations in the art.
Examples 1 to 13 and comparative examples 1 to 12
The components of the essential oil nanoemulsions of grapefruits of examples 1 to 13 and comparative examples 1 to 12 of the present invention and their amounts and reaction conditions are shown in tables 1 and 2, respectively, below.
The preparation method of the grapefruit essential oil nanoemulsion of examples 1 to 13 and comparative examples 1 to 12 of the present invention comprises the following steps:
(1) Uniformly mixing a surfactant A and a surfactant B to obtain a mixed solution A;
(2) Adding essential oil into the mixed solution A in the step (1), uniformly mixing the essential oil with the dropping speed of 60 drops/min, and stirring the mixture for 30min to obtain a mixed solution B;
(3) Adding water into the mixed solution B in the step (2), uniformly mixing, stirring for 15min, homogenizing, and filtering by a microporous filter membrane with the diameter of 0.22 mu m to obtain the grapefruit essential oil nanoemulsion.
TABLE 1
TABLE 2
Effect example 1
To verify the physicochemical properties and stability of the grapefruit essential oil nanoemulsions prepared in the present invention, the grapefruit essential oil nanoemulsions prepared in examples 1 to 13 and comparative examples 1 to 12 of the present invention were respectively subjected to appearance observation and measurement of particle diameters, polydispersity coefficients and Zeta potential values, and the test results are shown in table 3 below.
Appearance observation: and (3) carrying out appearance observation on the obtained grapefruit essential oil nanoemulsion, and observing whether the grapefruit essential oil nanoemulsion has a tyndall effect or not by using laser to directly shoot the grapefruit essential oil nanoemulsion.
Particle size testing: taking 10uL of grapefruit essential oil nanoemulsion to reach 1mL, and measuring the particle size of the grapefruit essential oil nanoemulsion by using a nanometer particle size and Zeta potential analyzer.
Polydisperse coefficient test: taking 10uL of grapefruit essential oil nanoemulsion to reach 1mL, and measuring the polydispersity index of the grapefruit essential oil nanoemulsion by using a nanometer particle size and Zeta potential analyzer.
Zeta potential value test: and taking 10uL of grapefruit essential oil nanoemulsion to reach 1mL, and measuring the Zeta potential of the grapefruit essential oil nanoemulsion by using a nano-particle size and Zeta potential analyzer.
TABLE 3 Table 3
As can be seen from tables 1 to 3, according to comparative examples 1 to 13, the physical and chemical properties and stability of the grapefruit essential oil nanoemulsion can be affected by the selection of different raw materials, the formulation ratio of the raw materials, different heating temperatures, different homogenization time and power, and the grapefruit essential oil nanoemulsion prepared in examples 1 to 13 of the present invention has smaller particle size and smaller polydispersity, which indicates that the particles of the grapefruit essential oil nanoemulsion prepared in examples 1 to 13 of the present invention are uniformly dispersed and have smaller particle size, and the absolute value of the Zeta potential value thereof is more than 10mV, and can reach 17.3mV at most, which indicates that the grapefruit essential oil nanoemulsion of the present invention has good stability, wherein the formulation ratio and reaction conditions of example 1 are adopted, which can make the grapefruit essential oil nanoemulsion simultaneously have good physical and chemical properties and stability.
Comparing examples 1-2 with comparative examples 1-8, it is known that the grapefruit essential oil nanoemulsion prepared by adopting the surfactant A comprising span 20 and Tween 80 and the surfactant B comprising glycerol or 1,2 propylene glycol of the invention has good Tyndall effect, and the grapefruit essential oil nanoemulsion has uniform particles, smaller particle size, larger absolute value of Zeta potential and better stability; the single span 20, span 80 and tween 20 are used as the surfactant A, and the preparation method of the essential oil nanoemulsion is adopted to be emulsified together with glycerol, so that the grapefruit essential oil nanoemulsion cannot be obtained, and the prepared emulsion has no tyndall effect; the single Tween 80 is used as the surfactant A, and the preparation method of the essential oil nanoemulsion is adopted to be emulsified together with glycerol, so that the grapefruit essential oil nanoemulsion is prepared, but the particle size is 109.3nm, and the particles are not uniformly dispersed and have poor stability; and the surfactant A compounded by other span and tween surfactants is used, or the components of the surfactant B are singly changed, so that the prepared grapefruit essential oil nanoemulsion has larger particle size and poorer stability.
As can be seen from comparing example 1, examples 3 to 4 and comparative example 9, the mass ratio of span 20 to tween 80 according to the present invention is span 20: tween 80= (2-5): the grapefruit essential oil nanoemulsion prepared in the step 5 has uniform particles and smaller particle size, and the stability of the emulsion is greatly improved; when the mass ratio of span 20 to tween 80 is lower than 2:5, the absolute value of the Zeta potential of the grapefruit essential oil nanoemulsion prepared in comparative example 9 is only 6.8mV, while the absolute value of the Zeta potential of example 1 is 2.45 times that of comparative example 9, and the stability of the grapefruit essential oil nanoemulsion prepared in example 1 is greatly improved.
As can be seen from comparing example 1, example 5 and comparative examples 10 to 12, the mass ratio of the essential oil and the surfactant a according to the present invention is: surfactant a=1: (4-5), the prepared grapefruit essential oil nanoemulsion has the properties of uniform particles, smaller particle size and better stability; when the dosage of the essential oil in the essential oil nanoemulsion is high or low, the prepared grapefruit essential oil nanoemulsion has the characteristics of non-uniform particles, large particle size and poor stability.
Effect example 2
To further demonstrate the stability of the grapefruit essential oil nanoemulsion particles prepared in accordance with the present invention, the grapefruit essential oil nanoemulsion prepared in example 1 was stored at 4 ℃ and 26 ℃ respectively, and tested for particle size at 0, 0.5, 1, 1.5, 2, and 3 months, and the test results at 4 ℃ and 26 ℃ were shown in fig. 1 and 2.
As can be seen from FIG. 1, the particle size of the grapefruit essential oil nanoemulsion stored for 3.5 months at 4 ℃ is changed, the particle size is at least 36.1nm, the particle size is at most 38nm, and the particle size change range within 3.5 months is 1.9nm, which shows that the grapefruit essential oil nanoemulsion disclosed by the invention has good stability under the condition of low-temperature storage.
As can be seen from FIG. 2, the particle size of the grapefruit essential oil nanoemulsion stored for 3.5 months at 26 ℃ is changed, the particle size is 41.5nm at minimum, the particle size is 44.1nm at maximum, and the particle size change range within 3.5 months is 2.6nm, which shows that the grapefruit essential oil nanoemulsion disclosed by the invention has good stability under the condition of normal-temperature storage.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. The preparation method of the essential oil nanoemulsion is characterized by comprising the following steps of:
(1) Uniformly mixing a surfactant to obtain a mixed solution A; the surfactant comprises a surfactant A and a surfactant B, wherein the surfactant A comprises span 20 and Tween 80, and the surfactant B comprises at least one of glycerol and 1, 2-propanediol;
(2) Adding essential oil into the mixed solution A in the step (1), and uniformly stirring to obtain a mixed solution B;
(3) Adding water into the mixed solution B in the step (2), uniformly stirring, and homogenizing to obtain the essential oil nanoemulsion;
in the step (1), the mass ratio of the surfactant A to the surfactant B is surfactant A: surfactant b=1: 4, the mass ratio of span 20 to tween 80 is span 20: tween 80= (2-5): 5, a step of; the mixing temperature is 70-80 ℃;
In the step (2), the essential oil is grapefruit essential oil, and the mass ratio of the essential oil to the surfactant A is: surfactant a=1: (4-5); the drip speed of the grapefruit essential oil is (40-80) drops/min.
2. The method for preparing the essential oil nanoemulsion according to claim 1, wherein in the step (1), the mass ratio of span 20 to tween 80 is span 20: tween 80=3:5.
3. The method for preparing an essential oil nanoemulsion according to claim 1, wherein in the step (2), the mass ratio of the essential oil to the surfactant a is: surfactant a=1:5.
4. The method of claim 1, wherein in step (1), the temperature of the mixing is 80 ℃.
5. The method for preparing an essential oil nanoemulsion according to claim 1, wherein in the step (3), the homogenizing time is 4-6 min, and the homogenizing power is 240-280 w.
6. The method of claim 5, wherein in the step (3), the homogenizing time is 5min and the homogenizing power is 240W.
7. An essential oil nanoemulsion obtained by the method for preparing an essential oil nanoemulsion according to any one of claims 1-6.
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