CN106880505B - Antioxidant nanometer ethosome rose essence and preparation method thereof - Google Patents
Antioxidant nanometer ethosome rose essence and preparation method thereof Download PDFInfo
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- 241000220317 Rosa Species 0.000 title claims abstract description 75
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 31
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 121
- WMBWREPUVVBILR-UHFFFAOYSA-N GCG Natural products C=1C(O)=C(O)C(O)=CC=1C1OC2=CC(O)=CC(O)=C2CC1OC(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-UHFFFAOYSA-N 0.000 claims abstract description 29
- WMBWREPUVVBILR-WIYYLYMNSA-N (-)-Epigallocatechin-3-o-gallate Chemical compound O([C@@H]1CC2=C(O)C=C(C=C2O[C@@H]1C=1C=C(O)C(O)=C(O)C=1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-WIYYLYMNSA-N 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- -1 sucrose ester Chemical class 0.000 claims abstract description 14
- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 claims abstract description 13
- 229940083466 soybean lecithin Drugs 0.000 claims abstract description 13
- 229930006000 Sucrose Natural products 0.000 claims abstract description 12
- 239000005720 sucrose Substances 0.000 claims abstract description 12
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims abstract description 9
- 229920000053 polysorbate 80 Polymers 0.000 claims abstract description 9
- 239000000341 volatile oil Substances 0.000 claims abstract description 9
- 239000000232 Lipid Bilayer Substances 0.000 claims abstract description 3
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 3
- 239000003381 stabilizer Substances 0.000 claims abstract description 3
- 235000019441 ethanol Nutrition 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 17
- 238000009210 therapy by ultrasound Methods 0.000 claims description 13
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- JKRWZLOCPLZZEI-UHFFFAOYSA-N alpha-Trichloromethylbenzyl acetate Chemical class CC(=O)OC(C(Cl)(Cl)Cl)C1=CC=CC=C1 JKRWZLOCPLZZEI-UHFFFAOYSA-N 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 6
- 150000003254 radicals Chemical class 0.000 description 6
- 230000001953 sensory effect Effects 0.000 description 5
- 238000013270 controlled release Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
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- 239000012071 phase Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
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- 150000002500 ions Chemical class 0.000 description 3
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- WMBWREPUVVBILR-GHTZIAJQSA-N (+)-gallocatechin gallate Chemical compound O([C@H]1CC2=C(O)C=C(C=C2O[C@@H]1C=1C=C(O)C(O)=C(O)C=1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-GHTZIAJQSA-N 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
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- MGJZITXUQXWAKY-UHFFFAOYSA-N diphenyl-(2,4,6-trinitrophenyl)iminoazanium Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1N=[N+](C=1C=CC=CC=1)C1=CC=CC=C1 MGJZITXUQXWAKY-UHFFFAOYSA-N 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
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- LVJJFMLUMNSUFN-UHFFFAOYSA-N gallocatechin gallate Natural products C1=C(O)C=C2OC(C=3C=C(O)C(O)=CC=3)C(O)CC2=C1OC(=O)C1=CC(O)=C(O)C(O)=C1 LVJJFMLUMNSUFN-UHFFFAOYSA-N 0.000 description 1
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- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
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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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/14—Liposomes; Vesicles
-
- 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
- A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
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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
- A61K8/55—Phosphorus compounds
- A61K8/553—Phospholipids, e.g. lecithin
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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
- A61K8/60—Sugars; Derivatives thereof
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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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/86—Polyethers
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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
- A61K2800/10—General cosmetic use
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Abstract
The invention provides an antioxidant nanometer ethosome rose essence, which comprises a vesicle structure consisting of soybean lecithin, ethanol, water and EGCG and having a lipid bilayer structure, wherein a capsule core is rose essential oil, and is prepared by adding a stabilizer sucrose ester and an emulsifier Tween-80 in the preparation process; the fragrance is stable and lasting, the fragrance is not changed, and the product is suitable for food, health care and skin care products; the preparation process is convenient to operate, does not need expensive and complex instruments, has good stability under low-temperature storage, and greatly delays the volatilization of the aroma during preparation and storage.
Description
Technical Field
The invention belongs to the field of daily chemicals, and particularly relates to an antioxidant nanometer ethosome rose essence and a preparation method thereof.
Background
With the development and extension of microcapsule technology, nano-microcapsules are attracting much attention. Nanotechnology is gradually developing research and application in the fields of food, skin care products and the like. The essence is a volatile additive, is applied to food, cosmetics and other aspects, and can be contacted with different parts of a human body. The rose essence is popular with people, but the common rose essence is a common emulsion, belongs to a thermodynamically unstable system, is easy to generate phenomena such as layering, oil floating and the like, is easy to damage the essence system, does not have an antioxidant function, and is easy to oxidize to cause product quality reduction. Gallocatechin gallate (EGCG) is an antioxidant extracted from tea, has strong antioxidation effect, and thus has various biological activities such as anti-aging, anticancer, etc. If the antioxidant essence can be successfully added into an essence system, the essence with the antioxidant function can be obtained.
Disclosure of Invention
The invention aims to provide an antioxidant nanometer ethosome rose essence which can delay aroma release, increase aroma retention time and simultaneously play an antioxidant effect on food, skin, environment and the like, and also discloses a preparation method of the essence.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
an antioxidant nanometer ethosome rose essence comprises a vesicle structure with a lipid bilayer structure, wherein the vesicle structure consists of soybean lecithin, ethanol, water and EGCG, and a capsule core is rose essential oil and is prepared by adding a stabilizer sucrose ester and an emulsifier Tween-80 in the preparation process; the raw materials comprise the following components in percentage by weight:
preferably, the antioxidant nanometer ethosome rose essence is oil-in-water type soybean lecithin bimolecular spherical nanoparticle solution formed by adding sucrose ester into soybean lecithin bimolecular layers.
The invention also aims to provide a preparation method of the antioxidant nanometer ethosome rose essence, which adopts the following technical scheme:
a preparation method of an antioxidant nanometer ethosome rose essence comprises the following steps:
1) adding EGCG into absolute ethyl alcohol to be dissolved uniformly for later use;
2) dissolving tween-80, rose essential oil, sucrose ester and soybean lecithin in the ethanol solution obtained in the step 1) for later use;
3) putting the ethanol solution obtained in the step 2) into a closed bottle, and fully stirring at a certain temperature and a certain rotating speed;
4) keeping the rotating speed and the temperature unchanged, slowly dripping water into the closed bottle and continuously stirring;
5) after the water is dripped, keeping the rotating speed and the temperature unchanged, and continuously stirring the obtained ethanol solution obtained in the step 4);
6) transferring the ethanol solution obtained in the step 5) into a container suitable for ultrasonic treatment, and performing ultrasonic treatment for a certain time.
Preferably, the temperature in the step 3) is 20-50 ℃, the rotation speed is 500-2000r/min, and the stirring time is 2-5 min.
Preferably, the stirring time of the step 5) is 2-5 min.
Preferably, the ultrasonic frequency of the step 6) is 1-3 times and 5 s/time, wherein the duration is 4s, the interval pause time is 1s, and the ultrasonic time is 2-5 min.
Preferably, the ultrasonic step of step 6) is performed under ice bath conditions.
The ethosome is a nanoparticle with a vesicle structure, is used as a novel nanoscale delivery system, has the advantages of the nanoparticle, delays half-life period, has a slow-release and controlled-release effect in vivo and in air, prolongs the effect of loading functional substances and release time, and can also obviously improve the stability of functional factors.
The ethosome has the excellent characteristics of small particle size, high encapsulation rate, difficult leakage, high skin permeability, first-level safety, no toxic or side effect and the like. The possible reason is that the resulting fusion induced by the high concentration of ethanol in the ethosome results in a tighter binding of the components in the structure of the ethosome vesicles. In the ethanol concentration range of 20% -45%, the particle size of the ethosomes is reduced along with the increase of ethanol, and the particle size of the ethosomes is changed due to the difference of phospholipid concentration.
The antioxidant nanometer ethosome rose essence is an oil-in-water phospholipid bimolecular spherical nanoparticle solution formed by simulating a cell membrane phospholipid bimolecular layer and adding sucrose ester.
Compared with the existing nano essence, the nano essence has the beneficial effects that: has slow release property of aroma components; the ethosome material is simple to prepare, has good permeability and adsorption capacity on human epidermis, and has good biological fusion; has antioxidant effect; the fragrance is stable and lasting, the fragrance is not changed, and the product is suitable for food, health care and skin care products; the preparation process is convenient to operate, does not need expensive and complex instruments, has good stability under low-temperature storage, and greatly delays the volatilization of the aroma during preparation and storage.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
An antioxidant nanometer ethosome rose essence comprises the following components in parts by weight (percentage by weight):
the preparation method of the antioxidant nanometer ethosome rose essence specifically comprises the following preparation steps:
1) dripping 0.8 weight part of tween-80 and 1.5 weight parts of rose essential oil into 30 weight parts of absolute ethyl alcohol to be uniformly dissolved for later use;
2) dissolving 1 weight part of EGCG, 0.2 weight part of sucrose ester and 2.5 weight parts of soybean lecithin in the ethanol solution for later use;
3) putting the absolute ethyl alcohol solution obtained in the step 2) into a closed glass conical flask, and fully stirring for 2min at the rotating speed of 1000r/min at 30 ℃;
4) slowly dripping 64 parts by weight of water into the sealed absolute ethyl alcohol solution at the rotation speed of 1000r/min at the temperature of 30 ℃;
5) after the water is dripped, the ethanol solution is continuously stirred for 5min under the condition of keeping the rotation speed of 1000r/min at 30 ℃;
6) transferring the ethanol solution obtained in the step 5) into a container suitable for ultrasonic treatment, and carrying out ultrasonic treatment for 5 s/time under ice bath condition, wherein the duration is 4s, the interval is 1s, and the ultrasonic treatment is 2 min.
And (3) detection:
the EGCG nano ethosome rose essence obtained is detected by a Malvern laser particle size analyzer to be 87.3 +/-1.7 in particle size and 40.1 +/-0.38 in zeta potential.
The EGCG nanometer ethosome rose essence dripped on the professional fragrance-smelling paper is compared with a control group 1 and a control group 2 through sensory evaluation and GC-MS detection.
Control group 1: 1 part by weight of EGCG is replaced by 1 part by weight of ethanol in the formula (the total amount is 31 parts by weight of ethanol, and common nano ethosomes are formed according to the phase synchronization steps.
Control group 2: the components of the formula are not changed, and the components of the formula are simply mixed, so that the nano ethosome is not formed.
The EGCG nano ethosomes rose essence with the clearance rate of 50 percent of free radicals determined by a DPPH method is 0.9ml, and the common nano ethosomes essence is more than 3 ml.
After being released for 3 hours at 37 ℃, the sensory smell EGCG nano ethosome rose essence and the common nano ethosome rose essence still have higher rose fragrance, but the non-nano ethosome rose essence only has lower rose fragrance; GC-MS analysis shows that (Table 1), the retention rate of the EGCG nano ethosomes rose essence and the reduction of the common nano ethosomes essence are slower, but the retention rate of the rose crystals of the non-nano ethosomes essence is fast.
TABLE 13 retention of rose essence after release of rose crystals on test paper at 37 deg.C
Example 2
A release controlled release type nanometer ethosome rose essence comprises the following components in parts by weight (weight percentage):
the preparation method of the release-controlled nanometer ethosome rose essence specifically comprises the following preparation steps:
1) dripping 0.8 weight part of tween-80 and 3 weight parts of rose essential oil into 29 weight parts of absolute ethyl alcohol to be uniformly dissolved for later use;
2) dissolving 0.5 weight part of EGCG, 0.2 weight part of sucrose ester and 2.5 weight parts of soybean lecithin in the absolute ethanol solution for later use;
3) placing the absolute ethyl alcohol into a closed glass conical flask, and fully stirring for 4min at the rotating speed of 1500r/min at 20 ℃;
4) slowly dripping 64 parts by weight of water into the sealed absolute ethyl alcohol for dissolving under the condition of keeping the rotating speed of 1500r/min at 20 ℃;
5) continuously heating and stirring the mixed ethanol solution for 5min under the condition of keeping the rotation speed of 1500r/min at 20 ℃;
6) the ethanol solution is transferred into a container suitable for ultrasonic treatment, and ultrasonic treatment is carried out for 3 minutes under ice bath conditions for 5 s/time (duration time 4s, interval dwell time 1 s).
And (3) detection:
the particle diameter of the nanometer ethosome rose essence is 86.1 +/-2.01 and the zeta potential is 38.9 +/-0.38 detected by a Malvern laser particle size analyzer.
Control group 1: in the formula, 0.5 weight part of EGCG is replaced by 0.5 weight part of ethanol (the total amount is 29.5 weight parts of ethanol, and common nano ethosomes are formed according to a phase synchronization step.
Control group 2: the components of the formula are not changed, and the components of the formula are simply mixed, so that the nano ethosome is not formed.
The EGCG nano ethosomes rose essence with the clearance rate of 50 percent of free radicals determined by a DPPH method is 1.9ml/L, and the common nano ethosomes essence is more than 3 ml/L.
After being released for 3 hours at 37 ℃, the sensory smell EGCG nano ethosome rose essence and the common nano ethosome rose essence still have higher rose fragrance, but the non-nano ethosome rose essence only has lower rose fragrance; GC-MS analysis shows that (Table 2), the retention rate of the EGCG nano ethosomes rose essence and the reduction of the common nano ethosomes essence are slower, but the retention rate of the rose crystals of the non-nano ethosomes essence is fast.
TABLE 23 Retention of Rose essence after release of Rose crystals on test paper at 37 deg.C
Example 3
A release controlled release type nanometer ethosome rose essence comprises the following components in parts by weight (weight percentage):
the preparation method of the release-controlled nanometer ethosome rose essence specifically comprises the following preparation steps:
1) dripping 1.5 parts by weight of tween-80 and 5 parts by weight of rose essential oil into 33.2 parts by weight of absolute ethyl alcohol to be uniformly dissolved for later use;
2) dissolving 2 parts by weight of EGCG, 0.3 part by weight of sucrose ester and 3.0 parts by weight of soybean lecithin in the absolute ethanol solution for later use;
3) placing the absolute ethyl alcohol into a closed glass conical flask, and fully stirring for 4min at the rotating speed of 1500r/min at 20 ℃;
4) slowly dripping 55 parts by weight of water into the sealed absolute ethyl alcohol for dissolving under the condition of keeping the rotation speed of 1500r/min at 20 ℃;
5) continuously heating and stirring the mixed ethanol solution for 5min under the condition of keeping the rotation speed of 1500r/min at 20 ℃;
6) the ethanol solution is transferred into a container suitable for ultrasonic treatment, and ultrasonic treatment is carried out for 3 minutes under ice bath conditions for 5 s/time (duration time 4s, interval dwell time 1 s).
And (3) detection:
the particle size of the nanometer ethosome rose essence is 76.5 +/-1.81 and the zeta potential is 35.9 +/-0.24 through a Malvern laser particle size analyzer detection.
Control group 1: 2 parts by weight of EGCG was replaced with 2 parts by weight of ethanol (37 parts by weight of ethanol in total) in the formulation, and ordinary nanoethosomes were formed in the same phase.
Control group 2: the components of the formula are not changed, and the components of the formula are simply mixed, so that the nano ethosome is not formed.
The EGCG nano ethosomes rose essence with the clearance rate of 50 percent of free radicals determined by a DPPH method is 0.47ml/L, and the common nano ethosomes essence is more than 3 ml/L.
After being released for 3 hours at 37 ℃, the sensory smell EGCG nano ethosome rose essence and the common nano ethosome rose essence still have higher rose fragrance, but the non-nano ethosome rose essence only has lower rose fragrance; GC-MS analysis shows (Table 3) that the retention rate of the EGCG nano ethosomes rose essence and the common nano ethosomes essence are reduced slowly, but the retention rate of the rose crystals of the non-nano ethosomes essence is fast.
TABLE 33 Retention of Rose essence after release of Rose crystals on test paper at 37 deg.C
Example 4
A release controlled release type nanometer ethosome rose essence comprises the following components in parts by weight (weight percentage):
the preparation method of the release-controlled nanometer ethosome rose essence specifically comprises the following preparation steps:
1) dripping 0.85 weight part of tween-80 and 1 weight part of rose essential oil into 30 weight parts of absolute ethyl alcohol to be uniformly dissolved for later use;
2) dissolving 0.5 weight part of EGCG, 0.15 weight part of sucrose ester and 1.0 weight part of soybean lecithin in the absolute ethanol solution for later use;
3) placing the absolute ethyl alcohol into a closed glass conical flask, and fully stirring for 4min at the rotating speed of 1500r/min at 20 ℃;
4) slowly dripping 66.5 parts by weight of water into the sealed absolute ethyl alcohol for dissolving under the condition of keeping the rotation speed of 1500r/min at 20 ℃;
5) continuously heating and stirring the mixed ethanol solution for 5min under the condition of keeping the rotation speed of 1500r/min at 20 ℃;
6) the ethanol solution is transferred into a container suitable for ultrasonic treatment, and ultrasonic treatment is carried out for 3 minutes under ice bath conditions for 5 s/time (duration time 4s, interval dwell time 1 s).
And (3) detection:
the particle size of the nanometer ethosome rose essence is 76.5 +/-1.81 and the zeta potential is 35.9 +/-0.24 through a Malvern laser particle size analyzer detection.
Control group 1: in the formula, 0.5 weight part of EGCG is replaced by 0.5 weight part of ethanol (30.5 weight parts of ethanol in total), and common nano ethosomes are formed according to a phase synchronization step.
Control group 2: the components of the formula are not changed, and the components of the formula are simply mixed, so that the nano ethosome is not formed.
The EGCG nano ethosomes rose essence with the clearance rate of 50 percent of free radicals determined by a DPPH method is 0.45ml/L, and the common nano ethosomes essence is more than 3 ml/L.
After being released for 3 hours at 37 ℃, the sensory smell EGCG nano ethosome rose essence and the common nano ethosome rose essence still have higher rose fragrance, but the non-nano ethosome rose essence only has lower rose fragrance; GC-MS analysis shows (Table 4) that the retention rate of the EGCG nano ethosomes rose essence and the common nano ethosomes essence are reduced slowly, but the retention rate of the rose crystals of the non-nano ethosomes essence is fast.
TABLE 43 Retention of Rose essence after release of Rose crystals on test paper at 37 deg.C
Determination of the ability to scavenge free radicals:
1mL of 1.625X10 were added to the tube in sequence-4mixing mol/L DPPH solution and 3.0mL of 50% ethanol with a total volume of 4.0mL for 20min, and measuring D (517nm) in a 1cm cuvette as D0(ii) a Adding 1mL1.625x10-4The volume of the solution is adjusted to 4mL by 50% ethanol, and the measured value is marked as Ds(ii) a Adding 1mL of ethanol with 50 percent of volume fractionAnd 1.0-3mL of sample solution to be measured, and using 50% ethanol to fix the volume to 4mL, and recording the measured value as Dr. DPPH radical clearance was calculated according to equation (1).
The antioxidant's ability to scavenge free radicals is expressed as 50% value for DPPH scavenging. Preparing antioxidant to be measured into a series of solutions, measuring the quality of the antioxidant and the DPPH free radical clearance, drawing a curve, reading the required antioxidant quality when the DPPH free radical clearance is 50% from the curve, and calculating IC according to the formula (2)50The value is obtained. The measurement was repeated 3 times, and the average value was the measurement result. Thus, IC50The physical meaning is the mass of DPPH scavenged per unit mass of antioxidant when 50% clearance is achieved.
The evaluation method of the fragrance retention effect comprises the following steps:
the fragrance retention effect was evaluated by measuring the retention amount of rose crystals on the fragrance retaining paper by GC-MS.
The solid phase microextraction condition of rose crystal is as follows: the balance time is 30min, the extraction time is 30min, the resolution temperature is 230 ℃, and no flow distribution is carried out. And after extraction is finished, taking the extraction head out of the headspace bottle, and manually putting the extraction head into a gas chromatography-mass spectrometer by a solid phase microextraction handle to perform analytic detection on the aroma substances.
Chromatographic conditions are as follows: column type of chromatographic column: rxi-5ms column (30 m.times.0.25 mm, 0.25um), column flow: 1ml/min, the injection port temperature is 250 ℃, and the temperature rise program is as follows: the initial temperature was 40 ℃ for 5min, then increased to 250 ℃ at 6 ℃/min. The carrier gas is high-purity helium (99.999%), the total flow rate is 15mL/min, and split-flow sample injection is not carried out.
Mass spectrum conditions: EI source temperature 230 ℃, electron energy 70eV, interface temperature 250 ℃, ion monitoring mode (sim mode) was selected, ion: 62. 74, 89, quantification of ions 62, solvent retardation: 3 min.
The calculation method comprises the following steps:
Claims (7)
1. an antioxidant nanometer ethosome rose essence is characterized by comprising a vesicle structure with a lipid bilayer structure, wherein the vesicle structure consists of soybean lecithin, ethanol, water and EGCG, and the vesicle core is rose essential oil and is prepared by adding a stabilizer sucrose ester and an emulsifier Tween-80 in the preparation process; the raw materials comprise the following components in percentage by weight:
the sum of the components is equal to 100%.
2. The antioxidant nanoethosome rose essence of claim 1, wherein the antioxidant nanoethosome rose essence is an oil-in-water type soybean lecithin bimolecular spherical nanoparticle solution formed by adding sucrose ester to soybean lecithin bimolecular layers.
3. A method for preparing the antioxidant nanoethosome rose essence of claim 1 or 2, which is characterized by comprising the following steps:
1) adding EGCG into absolute ethyl alcohol to be dissolved uniformly for later use;
2) dissolving tween-80, rose essential oil, sucrose ester and soybean lecithin in the ethanol solution obtained in the step 1) for later use;
3) putting the ethanol solution obtained in the step 2) into a closed bottle, and fully stirring at a certain temperature and a certain rotating speed;
4) keeping the rotating speed and the temperature unchanged, slowly dripping water into the closed bottle and continuously stirring;
5) after the water is dripped, keeping the rotating speed and the temperature unchanged, and continuously stirring the obtained ethanol solution obtained in the step 4);
6) transferring the ethanol solution obtained in the step 5) into a container suitable for ultrasonic treatment, and performing ultrasonic treatment for a certain time;
4. the method for preparing the antioxidant nanoethosome rose essence according to claim 3, wherein the temperature in the step 3) is 20-50 ℃, the rotation speed is 500-2000r/min, and the stirring time is 2-5 min.
5. The method for preparing the antioxidant nanoethosome rose essence according to claim 3, wherein the stirring time of the step 5) is 2-5 min.
6. The method for preparing antioxidant nanoethosome rose essence according to claim 3, wherein the ultrasonic frequency of step 6) is 1-3 times, 5 s/time, wherein the duration is 4s, the interval pause time is 1s, and the ultrasonic time is 2-5 min.
7. The method for preparing antioxidant nanoethosome rose essence according to claim 3, wherein the ultrasonic step of step 6) is performed under ice bath condition.
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