CN114796023A - Oil-in-water snake oil microemulsion and preparation method thereof - Google Patents
Oil-in-water snake oil microemulsion and preparation method thereof Download PDFInfo
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- CN114796023A CN114796023A CN202210174731.2A CN202210174731A CN114796023A CN 114796023 A CN114796023 A CN 114796023A CN 202210174731 A CN202210174731 A CN 202210174731A CN 114796023 A CN114796023 A CN 114796023A
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- 241000270295 Serpentes Species 0.000 title claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000000593 microemulsion method Methods 0.000 title description 2
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 45
- 239000006184 cosolvent Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 13
- 230000010355 oscillation Effects 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 5
- 239000003921 oil Substances 0.000 claims description 88
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 11
- 229920000053 polysorbate 80 Polymers 0.000 claims description 11
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 10
- HIQIXEFWDLTDED-UHFFFAOYSA-N 4-hydroxy-1-piperidin-4-ylpyrrolidin-2-one Chemical compound O=C1CC(O)CN1C1CCNCC1 HIQIXEFWDLTDED-UHFFFAOYSA-N 0.000 claims description 5
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 5
- -1 sorbitan fatty acid ester Chemical class 0.000 claims description 5
- PGMYKACGEOXYJE-UHFFFAOYSA-N anhydrous amyl acetate Natural products CCCCCOC(C)=O PGMYKACGEOXYJE-UHFFFAOYSA-N 0.000 claims description 4
- 239000004359 castor oil Substances 0.000 claims description 4
- 235000019438 castor oil Nutrition 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 4
- XUGNVMKQXJXZCD-UHFFFAOYSA-N isopropyl palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC(C)C XUGNVMKQXJXZCD-UHFFFAOYSA-N 0.000 claims description 4
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 4
- NEOZOXKVMDBOSG-UHFFFAOYSA-N propan-2-yl 16-methylheptadecanoate Chemical compound CC(C)CCCCCCCCCCCCCCC(=O)OC(C)C NEOZOXKVMDBOSG-UHFFFAOYSA-N 0.000 claims description 4
- 229940090181 propyl acetate Drugs 0.000 claims description 4
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 4
- FFJCNSLCJOQHKM-CLFAGFIQSA-N (z)-1-[(z)-octadec-9-enoxy]octadec-9-ene Chemical compound CCCCCCCC\C=C/CCCCCCCCOCCCCCCCC\C=C/CCCCCCCC FFJCNSLCJOQHKM-CLFAGFIQSA-N 0.000 claims description 3
- 229940072049 amyl acetate Drugs 0.000 claims description 3
- DTPCFIHYWYONMD-UHFFFAOYSA-N decaethylene glycol Polymers OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO DTPCFIHYWYONMD-UHFFFAOYSA-N 0.000 claims description 3
- MNWFXJYAOYHMED-UHFFFAOYSA-M heptanoate Chemical compound CCCCCCC([O-])=O MNWFXJYAOYHMED-UHFFFAOYSA-M 0.000 claims description 3
- 229940093629 isopropyl isostearate Drugs 0.000 claims description 3
- 229940074928 isopropyl myristate Drugs 0.000 claims description 3
- 229940075495 isopropyl palmitate Drugs 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 9
- 238000005119 centrifugation Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 32
- 239000011521 glass Substances 0.000 description 6
- 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 4
- 238000005516 engineering process Methods 0.000 description 4
- QYOVMAREBTZLBT-KTKRTIGZSA-N CCCCCCCC\C=C/CCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO Chemical compound CCCCCCCC\C=C/CCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO QYOVMAREBTZLBT-KTKRTIGZSA-N 0.000 description 3
- 239000002537 cosmetic Substances 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000007957 coemulsifier Substances 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 2
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 2
- 238000013329 compounding Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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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
- A61K8/925—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of animal 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
- A61K8/062—Oil-in-water emulsions
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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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/068—Microemulsions
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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
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
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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
- A61K8/4973—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
- 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
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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
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/26—Optical properties
- A61K2800/262—Transparent; Translucent
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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
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/413—Nanosized, i.e. having sizes below 100 nm
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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
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
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Abstract
The invention discloses an oil-in-water snake oil microemulsion and a preparation method thereof. The oil-in-water snake oil microemulsion comprises an oil phase, an emulsifier, a cosolvent and a water phase. The preparation method comprises the following steps: the emulsifier adopts a single-phase emulsifier or a compound emulsifier; mixing the oil phase and the cosolvent, transferring the mixture into another container, performing ultrasonic treatment under the condition of water bath, and uniformly mixing to obtain a mixed oil phase A; mixing the mixed oil phase A with an emulsifier, transferring to another container, and placing on a constant temperature oscillator for oscillation to obtain a mixed phase B; and (3) dropwise adding distilled water into the mixed phase B, and placing on a constant-temperature oscillator for oscillation until the system is clear to obtain the oil-in-water snake oil microemulsion. The snake oil microemulsion prepared by the method still keeps a clear and transparent stable state under the extreme conditions of centrifugation, high salinity and the like. Therefore, the utility model has higher practical value. Particle size tests show that the snake oil microemulsion prepared by the method has the particle size of less than 25nm and relatively uniform particle size distribution.
Description
Technical Field
The invention relates to an oil-in-water snake oil microemulsion and a preparation method thereof, belonging to the technical field of cosmetics.
Background
The microemulsion is an isotropic, transparent or semitransparent, thermodynamically stable dispersion system formed spontaneously after mixing a certain proportion of water, oil, emulsifier and co-emulsifier (cosolvent). Usually between 0.01 and 0.20 micron, and is stabilized by emulsifier and co-emulsifier (co-solvent).
The snake oil is rich in trace elements and unsaturated fatty acids required by human bodies, has good permeability, and can detoxify, detumescence, moisten skin and prevent chapping. However, because the unsaturated fatty acid in the snake oil contains a plurality of unsaturated bonds, is sensitive to sunlight, heat and air, and is easy to generate oxidation reaction to lose activity, the current method for improving the antioxidant capacity of the snake oil mainly depends on adding an antioxidant. In addition, the snake oil is not easy to dissolve in water and is solid at normal temperature, which also greatly limits the application of the snake oil. The current application of the snake oil does not effectively solve the problem that the snake oil is easy to be oxidized and unstable, so that the search of a proper method for embedding (protecting) the snake oil is very necessary.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to apply the micro-emulsification technology to the snake oil to solve the problems of low solubility, poor stability, low utilization rate and the like; meanwhile, the problem that the snake oil is easy to oxidize and unstable can be solved.
In order to solve the technical problems, the invention provides an oil-in-water snake oil microemulsion, which comprises an oil phase, an emulsifier, a cosolvent and an aqueous phase, wherein the oil phase is snake oil, the emulsifier is at least one of ethoxylated hydrogenated castor oil (PEG-40), polyoxyethylene sorbitan monooleate (Tween 80), sorbitan fatty acid ester (Span 80) and polyoxyethylene (10) oleyl ether (Brij97), the cosolvent is at least one of ethyl acetate, propyl acetate, n-butyl acetate, amyl acetate, isopropyl myristate, isopropyl palmitate and isopropyl isostearate, and the aqueous phase is distilled water.
The invention also provides a preparation method of the oil-in-water snake oil microemulsion, which comprises the following steps:
step 1): the emulsifier adopts one emulsifier as a single-phase emulsifier or adopts more than one emulsifier as a compound emulsifier; when the compound emulsifier is adopted, putting different emulsifiers into a container, performing ultrasonic treatment under the condition of water bath, and uniformly mixing;
step 2): mixing the oil phase and the cosolvent, transferring the mixture into another container, performing ultrasonic treatment under the condition of water bath, and uniformly mixing to obtain a mixed oil phase A;
step 3): mixing the mixed oil phase A with the emulsifier prepared in the step 1), transferring the mixture into another container, and placing the container on a constant temperature oscillator for oscillation to obtain a mixed phase B;
step 4): and (3) dripping distilled water into the mixed phase B, and placing the mixed phase B on a constant-temperature oscillator for oscillation until the system is clear to obtain the oil-in-water snake oil microemulsion.
Preferably, two emulsifiers are adopted in the step 1), and the mass ratio of the two emulsifiers is 9: 1-1: 9.
Preferably, the conditions of the ultrasound in the step 1) are as follows: the frequency is 30Hz, the power is 50W, the temperature is 37 ℃, and the ultrasonic time is 1 h.
Preferably, the mass ratio of the oil phase to the cosolvent in the step 2) is 1: 3-3: 1.
Preferably, the conditions of the ultrasound in step 2) are: the frequency is 30Hz, the power is 50W, the temperature is 37 ℃, and the ultrasonic time is 1 h.
Preferably, the mass ratio of the mixed oil phase A to the emulsifier in the step 3) is 9: 1-1: 9.
Preferably, the temperature of the constant temperature oscillator in the step 3) is 25-30 ℃, and the oscillation time is 24 hours.
Preferably, the temperature of the constant temperature oscillator in the step 4) is 25-30 ℃, and the oscillation time is 12-24 hours.
According to the invention, the water solubility of the snake oil is obviously improved by adding the cosolvents such as ethyl acetate, propyl acetate, n-butyl acetate, amyl acetate, isopropyl myristate, isopropyl palmitate, isopropyl isostearate and the like. The oil-in-water snake oil microemulsion presents a clear and transparent appearance, effectively improves the performances of low temperature resistance, high temperature resistance and the like, and improves the stability of the snake oil.
The microemulsion technology enables the particle size of a snake oil system to reach a nanometer level, has wetting, high permeability and good solubilization, and enables the snake oil to be solubilized in each phase system. According to the invention, the snake oil is deeply modified by adopting a micro-emulsification technology, and a novel nano-grade carrier of the snake oil which is non-toxic, low in cost, simple in process and excellent in physicochemical property is searched, so that the great improvement of the stability of the snake oil is the key point of the research, the bioavailability of the snake oil is expected to be improved, and a certain theoretical basis and practical reference are provided for the fine and further processing of the snake oil.
The microemulsion prepared by the invention still keeps a clear and transparent state under the extreme conditions of centrifugation and high salinity. The particle size test shows that the prepared oil-in-water snake oil microemulsion has the particle size of less than 25nm and relatively uniform particle size distribution.
The preparation method of the invention improves the water solubility of the snake oil, greatly improves the stability and oxidation resistance of the snake oil, can be quickly absorbed by human bodies, has clear and transparent appearance and high stability, and can be widely applied to the fields of cosmetics and the like. The invention is prepared at normal temperature, and has the characteristics of high safety and low energy consumption.
Compared with the prior art, the invention has remarkable technical progress. The invention aims to research and prepare the stable and safe snake oil microemulsion by utilizing the microemulsion technology, thereby overcoming the easy oxidation and hydrophobic characteristics of the snake oil microemulsion and leading the snake oil microemulsion to be applied to cosmetic products as an excellent carrier.
Drawings
FIG. 1 is a graph showing the particle size distribution of the snake oil microemulsion prepared in example 1.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
The main reagents and apparatus used in the examples are shown in tables 1 and 2, respectively.
TABLE 1
| Reagent | Specification of | Manufacturer of the product |
| Polyoxyethylene sorbitan monooleate (Tween 80) | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Sorbitan fatty acid ester (Span 80) | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Ethoxylated hydrogenated castor oil (PEG-40) | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Polyoxyethylene (10) oleyl ether (Brij97) | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Ethyl acetate | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Propyl acetate | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Acetic acid n-butyl ester | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Acetic acid pentyl ester | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Isopropyl myristate | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Palmitic acid isopropyl ester | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Isostearic acid isopropyl ester | Analytical purity | SINOPHARM CHEMICAL REAGENT Co.,Ltd. |
| Snake oil | Analytical purity | Dalian Fang Biochemical Limited |
| Distilled water | Homemade laboratory of Shanghai applied technology university |
TABLE 2
Example 1
An oil-in-water snake oil microemulsion is prepared by compounding polyoxyethylene sorbitan monooleate (Tween-80) and sorbitan fatty acid ester (Span-80) as emulsifier, using snake oil as oil phase, and using ethyl acetate as cosolvent.
The preparation method of the oil-in-water snake oil microemulsion specifically comprises the following steps:
(1) at room temperature, the mass ratio of Tween-80: span-80 ═ 9:1, mixing, fully mixing, transferring to a container, and placing on a water bath ultrasonic instrument under the conditions of: the frequency is 30Hz, the power is 50W, the temperature is 37 ℃, and the time is 1h, so that the compound emulsifier is obtained.
(2) At room temperature, according to the mass ratio: ethyl acetate ═ 1: 1, fully mixing, transferring to a container, and placing on a water bath ultrasonic instrument under the following conditions: the frequency is 30Hz, the power is 50W, the temperature is 37 ℃, and the time is 1h, so that the mixed oil phase A is obtained.
(3) Mixing the mixed oil phase A with a compound emulsifier, wherein the mass ratio of the emulsifier to the mixed oil phase A is 9:1, transferring the mixture into a glass bottle, placing the glass bottle on a constant-temperature oscillator, and continuously shaking for 24 hours at the temperature of 25 ℃ to obtain a mixed phase B;
(4) adding distilled water dropwise into the phase B, placing the phase B on a constant temperature oscillator for oscillation, and continuously shaking under the conditions that: the temperature is 25 ℃ and the time is 12 h. Fully mixing until the system is clear to obtain oil-in-water snake oil microemulsion; FIG. 1 is a particle size distribution diagram of the snake oil microemulsion prepared in the example.
Example 2
An oil-in-water snake oil microemulsion is prepared from oil of snake as emulsifier, and isopropyl myristate as cosolvent by using Brij97 as emulsifier and snake oil as oil phase.
The preparation method of the oil-in-water snake oil microemulsion specifically comprises the following preparation steps:
(1) at room temperature, according to the mass ratio: cosolvent is 1: 1, fully mixing, transferring to a container, and placing on a water bath ultrasonic instrument under the following conditions: the frequency is 30Hz, the power is 50W, the temperature is 37 ℃, and the time is 1h, so that the mixed oil phase A is obtained.
(2) Mixing the mixed oil phase A with an emulsifier, wherein the mass ratio of the emulsifier to the oil phase A is 8:2, transferring the mixture into a glass bottle, placing the glass bottle on a constant-temperature oscillator, and continuously shaking for 24 hours at the temperature of 25 ℃ to obtain a mixed phase B;
(3) dropwise adding distilled water into the phase B, placing the mixture on a constant-temperature oscillator for oscillation, and continuously oscillating under the conditions that: fully mixing at 25 ℃ for 12h until the system is clear to obtain the oil-in-water snake oil microemulsion;
example 3
An oil-in-water snake oil microemulsion is prepared by using ethoxyl hydrogenated castor oil (PEG-40) and polyoxyethylene sorbitan monooleate (Tween-80) as a compound emulsifier, using snake oil as an oil phase, and using n-butyl acetate as a cosolvent.
The preparation method of the oil-in-water snake oil microemulsion specifically comprises the following steps:
(1) at room temperature, the mass ratio of Tween-80: PEG-40 ═ 1: 1, mixing, transferring to a container after fully mixing, and placing on a water bath ultrasonic instrument under the conditions of: the frequency is 30Hz, the power is 50W, the temperature is 37 ℃, and the time is 1h, so that the compound emulsifier is obtained.
(2) At room temperature, according to the mass ratio: cosolvent is 1: 1, fully mixing, transferring to a container, and placing on a water bath ultrasonic instrument under the following conditions: the frequency is 30Hz, the power is 50W, the temperature is 37 ℃, and the time is 1h, so that the mixed oil phase A is obtained.
(3) Mixing the mixed oil phase A with a compound emulsifier, wherein the ratio of the emulsifier to the oil phase A is 7:3, transferring the mixture into a glass bottle, placing the glass bottle on a constant temperature oscillator, and continuously shaking for 24 hours at the temperature of 25 ℃ to obtain a mixed phase B;
(4) adding distilled water dropwise into the phase B, placing the phase B on a constant temperature oscillator for oscillation, and continuously shaking under the conditions that: fully mixing at 25 ℃ for 12h until the system is clear to obtain the oil-in-water snake oil microemulsion;
samples of the microemulsions prepared in examples 1-3 were selected. Centrifugal stability (injecting: a snake oil microemulsion sample is centrifuged at 3000r/min, 2000r/min and 1000r/min for 30min respectively in a centrifugal stability test, and then whether the microemulsion is clear and transparent and is not layered after centrifugation) and a salinity stability test (injecting: a NaCl solution with the concentration of 0.2mol/L and 0.5mol/L is respectively configured in the salinity stability test to replace pure water to investigate the influence of different salinity on the stability of the microemulsion, and the influence is judged according to the state of the microemulsion). The experimental result shows that the snake oil micro-emulsion with different formulas is stable under the conditions of high-speed centrifugation or high salinity, and the appearance is clear, transparent or semitransparent.
Claims (9)
1. The oil-in-water snake oil microemulsion is characterized by comprising an oil phase, an emulsifier, a cosolvent and a water phase, wherein the oil phase is snake oil, the emulsifier is at least one of ethoxylated hydrogenated castor oil, polyoxyethylene sorbitan monooleate, sorbitan fatty acid ester and polyoxyethylene (10) oleyl ether, the cosolvent is at least one of ethyl acetate, propyl acetate, n-butyl acetate, amyl acetate, isopropyl myristate, isopropyl palmitate and isopropyl isostearate, and the water phase is distilled water.
2. The method for preparing the oil-in-water snake oil microemulsion of claim 1, which comprises the following steps:
step 1): the emulsifier adopts one emulsifier as a single-phase emulsifier or adopts more than one emulsifier as a compound emulsifier; when the compound emulsifier is adopted, putting different emulsifiers into a container, performing ultrasonic treatment under the condition of water bath, and uniformly mixing;
step 2): mixing the oil phase and the cosolvent, transferring the mixture into another container, performing ultrasonic treatment under the condition of water bath, and uniformly mixing to obtain a mixed oil phase A;
step 3): mixing the mixed oil phase A with the emulsifier prepared in the step 1), transferring the mixture into another container, and placing the container on a constant temperature oscillator for oscillation to obtain a mixed phase B;
step 4): and (3) dripping distilled water into the mixed phase B, and placing the mixed phase B on a constant-temperature oscillator for oscillation until the system is clear to obtain the oil-in-water snake oil microemulsion.
3. The method for preparing the oil-in-water snake oil microemulsion according to claim 2, wherein two emulsifiers are used in the step 1), and the mass ratio of the two emulsifiers is 9: 1-1: 9.
4. The method for preparing the oil-in-water snake oil microemulsion according to claim 2, wherein the ultrasonic conditions in the step 1) are as follows: the frequency is 30Hz, the power is 50W, the temperature is 37 ℃, and the ultrasonic time is 1 h.
5. The method for preparing the oil-in-water snake oil microemulsion according to claim 2, wherein the mass ratio of the oil phase to the cosolvent in the step 2) is 1: 3-3: 1.
6. The method for preparing the oil-in-water snake oil microemulsion according to claim 2, wherein the ultrasonic conditions in the step 2) are as follows: the frequency is 30Hz, the power is 50W, the temperature is 37 ℃, and the ultrasonic time is 1 h.
7. The method for preparing the oil-in-water snake oil microemulsion according to claim 2, wherein the mass ratio of the mixed oil phase A and the emulsifier in the step 3) is 9: 1-1: 9.
8. The method for preparing the oil-in-water snake oil microemulsion according to claim 2, wherein the temperature of the constant temperature oscillator in the step 3) is 25-30 ℃, and the oscillation time is 24 h.
9. The method for preparing the oil-in-water snake oil microemulsion according to claim 2, wherein the temperature of the constant temperature oscillator in the step 4) is 25-30 ℃ and the oscillation time is 12-24 h.
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