Rose essential oil liposome emulsion as well as preparation method and application thereof
By combining sucrose or sodium chloride solid phase particles with lecithin with no-loaded liposomes and coated with rose essential oil, the existing liposome preparation process is solved, and efficient and simple preparation of rose essential oil liposome emulsion is achieved, improving the stability and use effect of the drug.
Patent Information
- Application Number
- CN202510111692.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-24
- Publication Date
- 2025-04-29
AI Technical Summary
The existing liposome preparation process is complicated, the production cost is high, the amount of organic solvents is large, and it is difficult to achieve large-scale preparation, resulting in problems in the storage and use of rose essential oil.
Sucrose or sodium chloride solid phase particles are used as carriers, combined with lecithin and other encapsulation materials, and no-loaded liposomes are prepared by impregnation and film formation method, and rose essential oil is coated on its surface to form a rose essential oil liposome emulsion.
The preparation process is simplified, the amount of organic solvent is reduced, the encapsulation rate and drug loading is improved, and it is easy to prepare on a large scale, extending the stability and service life of rose essential oil.
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Figure CN119896640A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of essences and fragrances, and in particular to a rose essential oil nanoliposome emulsion, a preparation method and application thereof. Background Art
[0002] Rose essential oil has a unique rose fragrance and has biological activities such as anti-mutagenicity, anti-oxidation, antibacterial and anti-inflammatory. Its main components are phenylethanol, citronellol, linalool and geraniol, etc. It is widely used as a natural additive in the food, cosmetics and pharmaceutical industries. However, some effective ingredients in rose essential oil are easy to oxidize and volatilize, causing problems during storage and use.
[0003] Liposomes are small vesicles composed of lipid layers that can encapsulate water-soluble or fat-soluble drugs. Liposomes are not only used to deliver drugs, but also to improve their stability by encapsulating bioactive ingredients. Common methods for preparing liposomes include ethanol injection, thin film dispersion, ultrasonic dispersion, melting, reverse evaporation, etc. However, the existing preparation process of liposomes also has certain defects, such as the preparation process is too complicated, the production cost is too high, a large amount of organic solvents are used, and it is difficult to achieve large-scale preparation, resulting in inapplicability. Summary of the invention
[0004] Aiming at the problems of complicated existing liposome preparation process, high production cost, large amount of organic solvent, and difficulty in large-scale preparation, the present invention combines sucrose and sodium chloride solid phase particles as carriers with encapsulation materials for the first time to prepare empty liposomes, and then encapsulates rose essential oil to prepare rose essential oil liposome emulsion. The present invention constructs a new process for preparing rose essential oil liposome emulsion with simple process, small amount of organic solvent, high encapsulation rate, and easy large-scale preparation.
[0005] In order to solve the above problems, the present invention adopts the following technical scheme, a method for preparing rose essential oil liposome emulsion, comprising the following steps:
[0006] (a) adding a wrapping material into an anhydrous ethanol solution to prepare a wrapping material solution;
[0007] (b) immersing the solid phase particles in a coating material solution, removing the anhydrous ethanol, and combining the solid phase particles with the coating material to obtain empty liposomes;
[0008] (c) mixing the empty liposomes with the aqueous dispersion of rose essential oil to obtain a rose essential oil liposome emulsion.
[0009] The encapsulating material is one of lecithin and lecithin-cholesterol;
[0010] In the lecithin-cholesterol, the mass ratio of lecithin to cholesterol is (4-8):1, preferably 6:1.
[0011] The solid phase particles are one of sucrose and sodium chloride. The mechanism of action of the solid phase particles is to utilize the excellent specific surface area of the solid phase particles to make the coating material solution volatilize on the surface of the solid phase particles to form a film.
[0012] The particle size of the solid phase particles is 150-1250 μm.
[0013] Preferably, when the solid phase particles are sucrose, the particle size of the solid phase particles is 300 to 900 μm;
[0014] Preferably, when the solid phase particles are sodium chloride, the particle size of the solid phase particles is 500 to 1250 μm.
[0015] The method for removing the anhydrous ethanol is one of evaporating in a high-temperature water bath, blowing dry, and standing at room temperature.
[0016] Preferably, in step (c), the mixing method of the empty liposomes and the rose essential oil aqueous dispersion includes: vortex oscillation and shaking.
[0017] The mass concentration of the coating material in the coating solution is 0.0189 to 0.2 g / mL, preferably 0.02363 to 0.2 g / mL.
[0018] The mass ratio of the solid phase particles to the encapsulating material is (1.39-6.25):1;
[0019] Preferably, when the solid phase particles are sucrose, the mass ratio of the solid phase particles to the encapsulating material is (1.39-4.17):1;
[0020] Preferably, when the solid phase particles are sodium chloride, the mass ratio of the solid phase particles to the packaging material is (3.125-6.25):1.
[0021] The ratio of the volume of the rose essential oil to the mass of lecithin is (2.3-7.25): 100 mL / g;
[0022] Preferably, when the solid phase particles are sucrose, the ratio of the volume of the rose essential oil to the mass of lecithin is (2.3-3.5): 100 mL / g;
[0023] Preferably, when the solid phase particles are sodium chloride, the ratio of the volume of the rose essential oil to the mass of lecithin is (3.5-7.25): 100 mL / g.
[0024] In the water dispersion of rose essential oil, the volume fraction of rose essential oil is 0.025-0.1%.
[0025] Preferably, when the solid phase particles are sucrose, the volume fraction of the rose essential oil is 0.025-0.05%;
[0026] Preferably, when the solid phase particles are sodium chloride, the volume fraction of the rose essential oil is 0.05-0.1%.
[0027] The present invention also provides a rose essential oil liposome prepared by the above preparation method.
[0028] When the solid phase particles are sucrose, the 18h permeability of the rose essential oil liposome is not less than 21.67%;
[0029] When the solid phase particles are sodium chloride, the 18h permeability of the rose essential oil liposome is not less than 22.63%;
[0030] When the solid phase particles are sucrose, the encapsulation efficiency of the rose essential oil liposome is 73.2-97.5%;
[0031] When the solid phase particles are sodium chloride, the encapsulation efficiency of the rose essential oil liposome is 80.1-93.8%.
[0032] Furthermore, the rose essential oil liposomes were measured for encapsulation efficiency by HPLC-ultrafiltration centrifugation method;
[0033] The ultrafiltration centrifugal speed is 6000-12000 rpm, and the centrifugal time is 10-20 min.
[0034] After granulation, the rose essential oil liposome has a particle size of 106-128 nm and an aggregation degree index (PDI) of 0.171-0.293.
[0035] In the granulation method, the drug-loaded liposome emulsion can be processed in one of the following ways: high-speed shearing, ultrasound, shearing, homogenization, and extrusion. Extrusion is preferred, and microfiltration extrusion is more preferred.
[0036] The present invention also provides a use of the rose essential oil liposome emulsion prepared by the preparation method in preparing an external preparation with the effects of promoting qi and relieving depression, regulating blood, relieving pain and moisturizing the skin.
[0037] Beneficial Effects
[0038] 1. The present invention adopts sucrose or sodium chloride solid phase particles as carriers for the first time, forms empty liposomes by combining with a coating material solution, and prepares rose essential oil liposome emulsion by coating rose essential oil. Due to the excellent specific surface area of the solid phase particles, the film thickness formed by the coating material on the surface of the solid phase particles is thin and uniform, which greatly increases the drug loading while rapidly encapsulating the drug.
[0039] 2. Compared with the spraying method of spraying the coating material solution onto the surface of the solid phase particles to form a spot film with uneven thickness and discontinuousness, the present invention adopts the immersion film-forming method to immerse the solid phase particles in a high concentration of the coating material solution. The obtained film thickness is uniform, resulting in a smaller and more uniform particle size of the formed liposomes, thereby increasing the drug loading capacity.
[0040] 3. The present invention prepares the empty liposomes and then mixes them with the rose essential oil aqueous dispersion, which not only avoids the influence of anhydrous ethanol on the rose essential oil, but also reduces the heating time of the rose essential oil generated by removing ethanol.
[0041] 4. In the actual application process, empty liposomes can be prepared first, and the rose essential oil liposomes can be prepared immediately without considering the influence of storage and transportation conditions on the rose essential oil drug. BRIEF DESCRIPTION OF THE DRAWINGS
[0042] Figure 1 is the HPLC spectrum of linalool reference substance;
[0043] Figure 2 HPLC spectra of the rose essential oil liposome emulsion permeate and concentrate of Examples 1-4 and Comparative Example 1;
[0044] Figure 3 HPLC spectra of the rose essential oil liposome emulsion permeate and concentrate of Examples 5-7;
[0045] Figure 4 This is a particle size distribution diagram of the rose essential oil liposome particles after microfiltration in Example 1. DETAILED DESCRIPTION
[0046] The present invention will be further described in detail below through specific implementation examples, but it should not be understood that the present invention is limited to the following examples, and all technologies realized based on the above content of the present invention belong to the scope of the present invention.
[0047] The lecithin described in the examples was purchased from Beijing Aoboxing Biological Co., Ltd.; rose essential oil was provided by Jinan Rose Garden Brewing Co., Ltd.; artificial skin was Strat-MTM Membrane purchased from Merck Millipore Ltd; cholesterol was purchased from Sinopharm Chemical Reagent Co., Ltd.; anhydrous ethanol was purchased from Tianjin Fuyu Fine Chemical Co., Ltd.; sucrose and sodium chloride were both conventional commercial products.
[0048] Embodiment 1:
[0049] In this embodiment, sucrose (average particle size of 600 μm) is used as the solid phase particles.
[0050] Weigh lecithin and add anhydrous ethanol solution to prepare a 0.2g / mL lecithin solution, ultrasonicate for 10 minutes, and store in dark conditions. Place the lecithin solution in an evaporating dish, heat it in a water bath at 50°C, then add sucrose to the lecithin solution at a mass ratio of 1.39:1 of sucrose solid phase particles to lecithin, stir while adding, evaporate in a water bath to obtain empty liposomes. Take the empty liposomes, add a 0.025% volume fraction of rose essential oil aqueous dispersion according to a ratio of 2.389:100mL / g of rose essential oil volume to lecithin mass, shake for 10 minutes, and obtain a rose essential oil liposome emulsion.
[0051] Embodiment 2:
[0052] In this embodiment, sucrose (average particle size of 600 μm) is used as the solid phase particles.
[0053] Weigh lecithin and add anhydrous ethanol solution to prepare a 0.2g / mL lecithin solution, ultrasonicate for 10 minutes, and store in dark conditions. Place the lecithin solution in an evaporating dish, heat it in a water bath at 50°C, then add sucrose to the lecithin solution at a mass ratio of sucrose solid phase particles to lecithin of 6.25:1, stir while adding, evaporate in a water bath to obtain empty liposomes. Take the empty liposomes, add a 0.025% volume fraction of rose essential oil aqueous dispersion according to a ratio of rose essential oil volume to lecithin mass of 7.25:100mL / g, shake for 10 minutes, and obtain a rose essential oil liposome emulsion.
[0054] Embodiment 3:
[0055] In this embodiment, sucrose (average particle size of 600 μm) is used as the solid phase particles.
[0056] Weigh lecithin and add anhydrous ethanol solution to prepare a 0.2g / mL lecithin solution, ultrasonicate for 10 minutes, and store in dark conditions. Place the lecithin solution in an evaporating dish, heat it in a water bath at 50°C, then add sucrose to the lecithin solution at a mass ratio of sucrose solid phase particles to lecithin of 1.39:1, stir while adding, evaporate in a water bath to obtain empty liposomes. Take the empty liposomes, add a 0.1% volume fraction of rose essential oil aqueous dispersion according to a ratio of rose essential oil volume to lecithin mass of 2.389:100mL / g, shake for 10 minutes, and obtain a rose essential oil liposome emulsion.
[0057] Embodiment 4:
[0058] The preparation conditions of this example are the same as those of Example 1, except that the lecithin in Example 1 is replaced by lecithin-cholesterol.
[0059] The mass ratio of lecithin to cholesterol is 6:1.
[0060] Embodiment 5:
[0061] In this embodiment, sodium chloride (average particle size of 650 μm) is used as the solid phase particles.
[0062] Weigh lecithin and add anhydrous ethanol solution to prepare a 0.2g / mL lecithin solution, ultrasonicate for 10 minutes, and store in dark conditions. Place the lecithin solution in an evaporating dish, heat it in a water bath at 50°C, then add sodium chloride solid phase particles at a mass ratio of 1.39:1 of sodium chloride to lecithin, stir while adding, evaporate in a water bath to obtain empty liposomes. Take the empty liposomes, add a 0.025% volume fraction of rose essential oil aqueous dispersion according to the ratio of rose essential oil volume to lecithin mass of 2.39:100mL / g, shake for 10 minutes, and obtain a rose essential oil liposome solution.
[0063] Embodiment 6:
[0064] In this embodiment, sodium chloride (average particle size of 650 μm) is used as the solid phase particles.
[0065] Weigh lecithin and add anhydrous ethanol solution to prepare a 0.2g / mL lecithin solution, ultrasonicate for 10 minutes, and store in dark conditions. Place the lecithin solution in an evaporating dish, heat it in a water bath at 50°C, then add sodium chloride solid phase particles at a mass ratio of 6.25:1 of sodium chloride to lecithin, stir while adding, evaporate in a water bath to obtain empty liposomes. Take the empty liposomes, add a 0.025% volume fraction of rose essential oil aqueous dispersion according to the ratio of rose essential oil volume to lecithin mass of 7.25:100mL / g, shake for 10 minutes, and obtain a rose essential oil liposome solution.
[0066] Embodiment 7:
[0067] In this embodiment, sodium chloride (average particle size of 650 μm) is used as the solid phase particles.
[0068] Weigh lecithin and add anhydrous ethanol solution to prepare a 0.2g / mL lecithin solution, ultrasonicate for 10 minutes, and store in dark conditions. Place the lecithin solution in an evaporating dish, heat it in a water bath at 50°C, then add sodium chloride solid phase particles at a mass ratio of 1.39:1 to lecithin, stir while adding, evaporate in a water bath to obtain empty liposomes. Take the empty liposomes, add a 0.1% volume fraction of rose essential oil aqueous dispersion according to the ratio of rose essential oil volume to lecithin mass of 2.39:100mL / g, shake for 10 minutes, and obtain a rose essential oil liposome solution.
[0069] Comparative Example 1:
[0070] In this comparative example, no sucrose solid phase particles were added.
[0071] Weigh lecithin and add anhydrous ethanol solution to prepare a solution with a lecithin concentration of 0.2g / mL, ultrasonicate for 10 minutes, and store in dark conditions. Add lecithin solution to an evaporating dish, heat in a water bath at 50°C to evaporate, and obtain a lecithin film. Take rose essential oil aqueous dispersion, add 0.025% rose essential oil aqueous dispersion according to the ratio of rose essential oil volume to lecithin mass 2.389:100mL / g, ultrasonicate for 10min, and obtain rose essential oil liposome emulsion.
[0072] Comparative Example 2:
[0073] The preparation conditions of this comparative example are the same as those of Example 1, except that rose essential oil is replaced by hydroxytyrosol.
[0074] Comparative Example 3:
[0075] The experimental conditions of this comparative example refer to Example 1, where rose essential oil is added to an anhydrous ethanol solution of lecithin (in the anhydrous ethanol solution of lecithin, the concentration of lecithin is 0.2 mg / mL), and the ratio of the volume of the rose essential oil to the mass of lecithin is 2.389:100 mL / g.
[0076] Sucrose was placed in a rotary evaporator, and under heating at 50° C., the sucrose solid phase particles were added to the lecithin solution containing rose essential oil at a mass ratio of 1.39:1 to lecithin, the solvent was evaporated, and deionized water was added to obtain a rose essential oil liposome emulsion (wherein the volume ratio of deionized water to rose essential oil was 100:0.025).
[0077] Comparative Example 4:
[0078] The experimental conditions of this comparative example are as follows: with reference to Example 1, lecithin is weighed and added to anhydrous ethanol solution, a lecithin solution containing 0.2g / mL lecithin is prepared, ultrasonicated for 10 minutes, and kept in dark. Sucrose is taken and placed in a rotary evaporation bottle, and then the lecithin solution is sprayed in the rotary evaporation bottle according to the mass ratio of sucrose solid phase particles and lecithin 1.39:1, the rotary evaporation temperature is 50 DEG C, and the vacuum degree is -0.098MPa to obtain empty liposomes. Take empty liposomes, according to the ratio of rose essential oil volume to lecithin mass being 2.389:100mL / g, add a rose essential oil aqueous dispersion having a volume fraction of rose essential oil of θ.025%, shake for 10min, and obtain a rose essential oil liposome emulsion.
[0079] Test example 1: Encapsulation efficiency test
[0080] Take 0.1mL of rose essential oil liposome emulsion in a common centrifuge tube, centrifuge at 6000rpm for 20min, take out the supernatant and add it to an ultrafiltration centrifuge tube, then add 0.3mL of pure water, ultrafiltration centrifuge for 20min (wherein, the ultrafiltration membrane pore size is 30KD, and the centrifugal speed is 6000rmp), take the permeate solution as the test solution for detecting free essential oil (defined as permeate). Take the centrifugal sediment of common centrifugation and add 0.4mL of anhydrous ethanol, ultrasonically dissolve, add the solution to an ultrafiltration centrifuge tube, ultrafiltration centrifuge for 20min (wherein, the ultrafiltration membrane pore size is 30KD, and the centrifugal speed is 6000rmp), take the permeate solution and supplement the lost weight with anhydrous ethanol as the test solution for detecting the encapsulated essential oil (defined as concentrate). According to the HPLC method, the amount of linalool in the free essential oil and the encapsulated essential oil is detected, and the encapsulation efficiency is calculated as follows:
[0081] Encapsulation rate (100%) = amount of essential oil encapsulated / (amount of free essential oil + amount of essential oil encapsulated) × 100%.
[0082] Chromatographic conditions: bonded silica gel C 18 (4.6mm*150mm, 5μm), with 0.2% phosphoric acid water (A)-acetonitrile (B) as the mobile phase, gradient elution (0-30min, B 35%-80%; 30-35min, B 100%; 35-40min, B 35%), flow rate 1.0ml / min, column temperature 30℃, detection wavelength 203nm, injection volume: 20μL.
[0083] Table 1 Rose essential oil liposome encapsulation efficiency (%)
[0084]
[0085]
[0086] Table 1 shows the encapsulation efficiency of the rose essential oil liposomes prepared in Examples 1-7. Each example examines the effects of the type of solid phase particles, the amount of lecithin, the volume fraction and volume of rose essential oil, and the amount of empty liposomes on the encapsulation efficiency.
[0087] Compared with Example 1, the amount of lecithin used in Example 2 is less, resulting in a smaller number of liposomes formed, resulting in a poor encapsulation efficiency; compared with Example 6, the amount of lecithin used in Example 5 is less, resulting in the adhesion of the encapsulating materials to each other, and the inability to form a spherical shape with a good shape, and the small capacity for rose essential oil or the large thickness of the liposome shell formed, making it difficult for a small amount of drug to enter, and the encapsulation efficiency is low.
[0088] The volume fraction of rose essential oil has a certain influence on the encapsulation rate. When other conditions remain unchanged and within a certain range of rose essential oil volume fraction, when the volume fraction of rose essential oil is too large, it is difficult to disperse well in the aqueous solution. During oscillation, the rose essential oil is in the upper layer and is difficult to fully contact with the empty liposomes, resulting in a low encapsulation rate.
[0089] Compared with the prior art, the present application has significant advantages in that a higher embedding rate can be obtained within a wider parameter range, and the preparation process is simple, the amount of organic solvent used is small, the preparation time is short, and large-scale preparation is possible.
[0090] like Figure 1 As shown, this is the liquid chromatogram of the linalool standard, the main component of rose essential oil. The retention time of linalool is about 15 minutes.
[0091] like Figure 2 , 3 As shown, the HPLC spectra of the rose essential oil liposome emulsion permeate and the concentrated solution prepared in Examples 1 to 4, Comparative Example 1 and Examples 5 to 7 are respectively shown. It can be seen from the figure that the rose essential oil liposome emulsion permeate and the concentrated solution of Examples 1 to 7 have peaks at the linalool chromatographic peak (the retention time of the linalool chromatographic peak is about 15 minutes), but the peak of the permeate is smaller and close to a straight line, while the concentrated solution has a strong peak, indicating that the encapsulated drug leaks little and the encapsulation effect is ideal.
[0092] Test Example 2: Determination of Particle Size
[0093] 0.1 mL of the rose essential oil liposome emulsion prepared in Examples 1 and 5 was taken and diluted to 1 mL with water. The average particle sizes of the rose essential oil liposomes were 160.9 nm and 174.567 nm, respectively, and the average PDIs were 0.290 and 0.361, respectively, and the average potentials were -60.4 mV and -36.6 mV, respectively, by three measurements using a laser particle size analyzer Zetasizer Nano ZS90.
[0094] The rose essential oil liposome emulsions prepared in Examples 1 and 5 were filtered through a microfiltration membrane, 0.1 mL of the filtrate was taken and diluted to 1 mL with water, and the average particle sizes of the rose essential oil liposomes after microfiltration were 114.2 nm and 115.36 nm, respectively, and the average PDIs were 0.188 and 0.171, respectively. The detection showed that the average potential of the rose essential oil liposome emulsion prepared in Example 1 after microfiltration was -0.489 mV.
[0095] like Figure 4The particle size distribution diagram of the rose essential oil liposome emulsion prepared in Example 1 after microfiltration is shown. It can be seen from the analysis that the liposome particle size after microfiltration is small, about 110nm, and the dispersion coefficient is small, relatively stable, and evenly dispersed. The average potential of the liposome is measured to be negative, the surface of the liposome particles is negatively charged, and the stability is good.
[0096] The particle size detection method of the rose essential oil liposome emulsion prepared in other embodiments and comparative examples after granulation is the same as that of Examples 1 and 5. The detection results are shown in Table 2.
[0097] Test Example 3: Transdermal Diffusion Experiment
[0098] Using a transdermal diffusion test device, a PEG400 solution with a mass concentration of 40% was added to the diffusion cell, 0.3 mL of each of the rose essential oil liposome emulsion and rose essential oil aqueous dispersion (volume fraction of 0.025%) prepared in each embodiment and comparative example was taken, uniformly dispersed on the smooth surface of the artificial skin, and permeated at room temperature. After 18 hours, the sample solution (the rose essential oil liposome emulsion permeated solution and the rose essential oil aqueous dispersion permeated solution prepared in each embodiment and comparative example) was taken out from the diffusion cell, and liquid chromatography was performed after microfiltration to calculate the skin permeability. The sample solution was further extracted with an equal volume of cyclohexane, the extract was evaporated, and dissolved with 0.1 mL of anhydrous ethanol as the sample solution for enzyme activity detection.
[0099] Table 2 Transmission rate and average particle size of rose essential oil liposomes
[0100]
[0101] As can be seen from Table 2, the rose essential oil liposome emulsions prepared in Examples 5-7 (sodium chloride as a carrier) have comparable particle sizes and slightly lower permeabilities than those prepared in Examples 1-4 (sucrose as a carrier). The permeabilities of Examples 1-7 are significantly higher than those of Comparative Examples 1-4 and the rose essential oil aqueous dispersion, indicating that the transdermal absorption effect of rose essential oil can be significantly improved by encapsulating to form liposomes, especially by using the liposomes prepared by the method of the present invention.
[0102] Test Example 4: Determination of the Antioxidant Activity of Rose Essential Oil Using the DPPH Method
[0103] 1. Solution preparation
[0104] DPPH-ethanol solution: Weigh 9 mg of DPPH and dissolve it in 200 mL of ethanol. Dissolve it by ultrasonication to prepare a 0.045 mg / mL DPPH-ethanol solution.
[0105] Rose essential oil sample solution: Take an appropriate amount of rose essential oil, dissolve it in anhydrous ethanol and make up to volume to prepare a rose essential oil sample solution with a volume fraction of 0.0625%.
[0106] Vitamin C solution: Dissolve and dilute with anhydrous ethanol to prepare a vitamin C solution with a concentration of 0.0056 mg / mL.
[0107] 2. Detection
[0108] Sample group: Take 40 μL of sample solution into a 96-well plate, add 60 μL of DDPPH free radical solution, shake well, and stand at room temperature (25°C) away from light for 10 min. Measure its absorbance, which is recorded as A1;
[0109] The sample solutions are respectively: the enzyme activity detection sample solutions of the embodiments and comparative examples and the rose essential oil water dispersion obtained in Detection Example 3, the rose essential oil sample solution, and the vitamin C solution.
[0110] Control group: According to the above method, the DPPH free radical solution was replaced by an equal volume of 60% (volume fraction) ethanol, and its absorbance was measured and recorded as A2;
[0111] Blank control group: Pipette 40 μL of 60% (volume fraction) ethanol into a 96-well plate, add 60 μL of DPPH free radical solution, shake well, and stand at room temperature in the dark for 10 min. Measure the absorbance, which is recorded as A0;
[0112] The scavenging rate of DPPH free radical was calculated as follows. The results are shown in Table 3.
[0113]
[0114] Table 3 DPPH free radical scavenging rate
[0115]
[0116]
[0117] Vitamin C was used as a positive control, indicating that the experimental results of the DPPH clearance rate of each embodiment and comparative example were reliable.
[0118] The results in Table 3 show that the 24h skin permeability of Examples 1-7 is significantly increased compared with Comparative Examples 1-4 and the rose essential oil aqueous dispersion, indicating that the rose essential oil liposomes prepared by the present invention can significantly enhance the skin permeability of the rose essential oil aqueous dispersion, and the experimental results of the scavenging rate of DPPH free radicals also confirm this result.
Claims
1. A method for preparing a rose essential oil liposome emulsion, characterized in that: The steps include: (a) adding a wrapping material into an anhydrous ethanol solution to prepare a wrapping material solution; (b) immersing the solid phase particles in a coating material solution, removing the anhydrous ethanol, and combining the solid phase particles with the coating material to obtain empty liposomes; (c) mixing the empty liposome with the aqueous dispersion of Flos Rosae Rugosae essential oil to obtain Flos Rosae Rugosae essential oil liposome emulsion; The solid phase particles are one of sucrose and sodium chloride.
2. The method for preparing the rose essential oil liposome emulsion according to claim 1, wherein The packaging material is one of lecithin and lecithin-cholesterol.
3. The preparation method of rose essential oil liposome emulsion according to claim 2, characterized in that, In the lecithin-cholesterol, the mass ratio of lecithin to cholesterol is (4-8):1, preferably 6:
1.
4. The method for preparing the rose essential oil liposome emulsion according to claim 1, wherein The particle size of the solid phase particles is 150-1250 μm. Preferably, when the solid phase particles are sucrose, the particle size of the solid phase particles is 300 to 900 μm; Preferably, when the solid phase particles are sodium chloride, the particle size of the solid phase particles is 500 to 1250 μm.
5. The method for preparing the rose essential oil liposome emulsion according to claim 1, characterized in that: The mass concentration of the coating material in the coating solution is 0.0189 to 0.2 g / mL, preferably 0.02363 to 0.2 g / mL.
6. The method for preparing the rose essential oil liposome emulsion according to claim 1, characterized in that: The mass ratio of the solid phase particles to the encapsulating material is (1.39-6.25):1; Preferably, when the solid phase particles are sucrose, the mass ratio of the solid phase particles to the encapsulating material is (1.39-4.17):1; Preferably, when the solid phase particles are sodium chloride, the mass ratio of the solid phase particles to the packaging material is (3.125-6.25):
1.
7. The method for preparing the rose essential oil liposome emulsion according to claim 2, characterized in that: The ratio of the volume of the rose essential oil to the mass of lecithin is (2.3-7.25): 100 mL / g; Preferably, when the solid phase particles are sucrose, the ratio of the volume of the rose essential oil to the mass of lecithin is (2.3-3.5): 100 mL / g; Preferably, when the solid phase particles are sodium chloride, the ratio of the volume of the rose essential oil to the mass of lecithin is (3.5-7.25): 100 mL / g.
8. The method for preparing the rose essential oil liposome emulsion according to claim 1, characterized in that: In the water dispersion of rose essential oil, the volume fraction of rose essential oil is 0.025-0.1%. Preferably, when the solid phase particles are sucrose, the volume fraction of the rose essential oil is 0.025-0.05%; Preferably, when the solid phase particles are sodium chloride, the volume fraction of the rose essential oil is 0.05-0.1%.
9. A rose essential oil liposome emulsion prepared by the preparation method according to any one of claims 1 to 8, characterized in that: When the solid phase particles are sucrose, the 18h permeability of the rose essential oil liposome is not less than 21.67%, and the encapsulation efficiency of the rose essential oil liposome is 73.2-97.5%; When the solid phase particles are sodium chloride, the 18h permeability of the rose essential oil liposome is not less than 22.63%, and the encapsulation efficiency of the rose essential oil liposome is 80.1-93.8%.
10. Use of the rose essential oil liposome emulsion prepared by the preparation method according to any one of claims 1 to 8, or the rose essential oil liposome emulsion according to claim 9 in preparing an external preparation with the effects of promoting qi and relieving depression, harmonizing blood, relieving pain, and moisturizing the skin.