Essential oil nano delivery carrier based on wild soybean extract as well as preparation method and application of essential oil nano delivery carrier

Abstract

The invention belongs to the technical field of skin care products, and particularly relates to a wild soybean extract-based essential oil nano delivery carrier as well as a preparation method and application thereof. The hydroxypropyl-beta-cyclodextrin is used as a wall material, the polysorbate emulsifier and the wild soybean extract are mixed to form the compound emulsifier, and the essential oil is used as a content, so that the defects of poor stability and low solubility of the essential oil are overcome; the prepared essential oil nano delivery carrier is small in particle size, good in high and low temperature stability, high in transparency, low in irritation and remarkable in functional effect. The essential oil nano delivery carrier can be used as an aromatic or a moisturizing and repairing active matter to be widely applied to skin care products, is in a clear and transparent liquid state, and can also be applied to transparent water aqua cosmetics.

Description

Technical Field

[0001] The invention belongs to the technical field of skin care products, and particularly relates to an essential oil nano delivery carrier based on wild soybean extract, and a preparation method and application thereof. Background Art

[0002] Essential oils are natural oily substances composed of various bioactive ingredients such as terpenes, phenols, aldehydes, ethers and other organic compounds. They are usually liquid and have antibacterial, antioxidant and anticancer effects. Encapsulation of essential oils is the key to solving problems such as volatility, unstable chemical properties and low water solubility. The essential oil delivery carrier formed by encapsulating essential oils has the characteristics of good dispersibility, high stability and excellent biological activity. Generally, the smaller the particle size of the delivery carrier, the more it can overcome its own gravity through Brownian motion to make the system dispersed evenly, achieve a certain kinetic stability, and the higher the delivery efficiency of the essential oil content, so nano-scale essential oil delivery carriers have broad prospects in various application fields.

[0003] Hydroxypropyl-β-cyclodextrin is a modified product of β-cyclodextrin. It has the cavity of β-cyclodextrin and improves its poor water solubility. It has the characteristics of anti-oxidation and decomposition, anti-volatilization, and adsorption of odor. Currently, most of the delivery carriers prepared by cyclodextrin and cyclodextrin derivatives that have been studied are in the form of powders. For example, the hydroxypropyl-β-cyclodextrin-apple flavor package finally obtained in patent CN113262743A is in the form of powder. Powder-shaped inclusions need to be post-processed by distillation equipment, freeze drying or spray drying equipment during the preparation process, which is a waste of resources; a small number are in liquid state, but most of the liquid materials are semi-permeable or milky white and opaque in appearance, and the particle size is mostly in the micron level, with poor stability. They are very prone to instability problems such as low-temperature precipitation or high-temperature transparency under extreme conditions, especially when used in cosmetic aqueous products, which will affect their transparency and stability; a very small number of nano-delivery carriers in clear and transparent liquid state usually need to be dissolved by organic reagents or allowed to stand and then self-assemble after preparation. The subsequent elution, drying and storage processes are time-consuming and labor-intensive, resulting in a certain amount of resource waste.

[0004] At present, there are nano-delivery carriers in a clear and transparent liquid state prepared by cyclodextrin and cyclodextrin derivatives. If it is not achieved by adding organic reagents or long-term self-assembly process, it is usually necessary to add a high content of emulsifier to form a thermodynamically stable system. However, the use of a large amount of emulsifier is not conducive to skin care and will bring certain irritation. Therefore, under the premise of ensuring the stability of the system, the amount of emulsifier added is usually as little as possible. In fact, the adsorption strength and intermolecular interaction level of molecules adsorbed on the O / W oil-water interface are important factors affecting the overall kinetic stability and interfacial rheological response of nano-delivery carriers. Non-ionic emulsifiers polysorbates (such as polysorbate-20, polysorbate-60, polysorbate-80, etc.) are commonly used emulsifiers for preparing nano-delivery carriers with cyclodextrin and cyclodextrin derivatives as wall materials. However, the high surface activity and spatial interaction of such emulsifiers at the O / W oil-water interface will weaken over time, and the interfacial oil droplets will gradually accelerate the aggregation, eventually leading to the oil-water stratification of the nano-delivery carrier liquid.

[0005] At present, the stability of the encapsulated delivery vehicle depends largely on the wall material composition and the feed rate, especially the feed rate. The fine emulsion and monodisperse emulsion formed by the appropriate feed rate can prevent the oil droplets from agglomerating during the preparation process, and form a kinetically and thermodynamically stable nano-delivery vehicle through high-energy homogenization and low-energy spontaneous emulsification.

[0006] Most of the existing research on nano delivery carriers is to use them as delivery carriers to deliver the contents. For example, patent CN115381732A only provides a preparation method for hydroxypropyl cyclodextrin-encapsulated retinol. The wall material of the delivery carrier in the article does not have skin care effects and cannot synergistically enhance the effects with the contents in the cosmetic system. Summary of the invention

[0007] In view of the deficiencies in the prior art, the present invention provides an essential oil nano-delivery carrier based on wild soybean extract, which is based on hydroxypropyl-β-cyclodextrin encapsulating essential oil, and uses a combination emulsifier of a non-ionic emulsifier polysorbate emulsifier and a zwitterionic emulsifier wild soybean extract (the active ingredient is mainly soybean lysolecithin). The obtained essential oil nano-delivery carrier has excellent characteristics such as small particle size, good stability, high transparency, low irritation, and significant efficacy. Secondly, the present invention also provides a method for preparing the above-mentioned essential oil nano-delivery carrier based on wild soybean extract, which has the advantages of simple operation, high repeatability, time and labor saving, and strong stability. Finally, the essential oil nano-delivery carrier of the present invention can be widely used in various skin care products as a fragrance or moisturizing and repairing active substance, especially transparent system water-based products.

[0008] The technical solution of the present invention is as follows:

[0009] In a first aspect, the present invention provides an essential oil nano delivery carrier based on wild soybean extract, comprising the following components: essential oil, hydroxypropyl-β-cyclodextrin, polysorbate emulsifier, wild soybean extract, and water.

[0010] Preferably, the mass percentage of the hydroxypropyl-β-cyclodextrin is 4.0-9.0%; the mass percentage of the essential oil is 0.001-2.5%, more preferably 1.0-2.5%; the mass percentage of the polysorbate emulsifier is 1.5-7.0%; the mass percentage of the wild soybean extract is 0.2-2.0%, and the balance is deionized water.

[0011] In the present invention, the essential oil nano delivery carrier is a light yellow to dark yellow transparent liquid, and its microstructure is round or oval under a transmission electron microscope, and its particle size is 10-30 nm.

[0012] The present invention uses hydroxypropyl-β-cyclodextrin as a wall material, polysorbate emulsifiers and wild soybean extracts as a composite emulsifier, and essential oils as contents, solves the shortcomings of poor stability and low solubility of essential oils, and prepares a small particle size, good high and low temperature stability, high transparency, low irritation, and significant functional effect of essential oil nano delivery carriers. The essential oil nano delivery carrier of the present invention is in a clear and transparent liquid state, and ensures that no organic reagent is required as a solvent or long-term static self-assembly during its preparation process, and a clear, transparent and stable system can be quickly achieved within 24 hours after the preparation is completed. It can be widely used in skin care products as a fragrance or moisturizing repair active substance, especially cosmetics transparent water formulations, and can maintain a long-term clear and transparent stable state under high temperature, low temperature, high and low temperature cycle conditions. This may be attributed to the stability of the nano delivery carrier before 24 hours depends on the type and concentration of the emulsifier, and the soybean lecithin contained in the wild soybean extract is easy to form a buffer elastic layer with a small surface tension at the O / W interface. At the same time, another polysorbate emulsifier present in the system can self-assemble in an orderly manner with hydroxypropyl-β-cyclodextrin, building a "channel" between the main hydroxypropyl-β-cyclodextrin and the guest molecule essential oil, forming a three-phase stable system of main body, guest, and emulsifier, promoting the guest molecule essential oil to quickly enter the hydrophobic cavity of the main body, and finally forming a clear, transparent and stable nano delivery carrier.

[0013] One of the emulsifiers of the present invention, wild soybean extract, is of natural origin, green and safe, mild and non-irritating. Under the condition of the same amount of essential oil added in the existing stabilization system, compared with the use of polysorbate emulsifiers alone, the system of wild soybean extract and polysorbate emulsifiers as emulsifiers can reduce the total amount of emulsifier added by about 21%, thereby reducing the risk of irritation caused by the emulsifier.

[0014] Furthermore, compared with the compound products of other common emulsifiers and polysorbate emulsifiers, the essential oil nano-delivery carrier is clear, transparent and stable. This may be attributed to the fact that anionic emulsifier potassium cetyl phosphate, cationic emulsifier hexadecyltrimethylammonium chloride, nonionic emulsifier inulin lauryl carbamate, and zwitterionic emulsifier cocamidopropyl hydroxysulfonobetaine cannot form a buffer elastic layer with low surface tension at the O / W interface like wild soybean extract, and also cannot promote the orderly self-assembly of polysorbate emulsifiers and hydroxypropyl-β-cyclodextrin, and ultimately fail to achieve the ideal effect of maintaining long-term stability.

[0015] Preferably, the types of essential oils include one or more of the essential oils of lavender, rose, rose geranium, damask rose, sandalwood, bergamot, patchouli, clary sage, ylang-ylang, sweet orange, pink grapefruit, mint, organic juniper berry, Atlantic cedar, (bitter) orange blossom, lemongrass, lemon, tea tree, jasmine, rosemary, frankincense, myrrh, thyme, vetiver, benzoin, white rosin, Scots pine, cypress, holly, eucalyptus, oregano, ginger, cinnamon, bay, nutmeg, fennel, clove, eucalyptus and Roman chamomile.

[0016] Preferably, the polysorbate emulsifier is selected from one or more of polysorbate-20, polysorbate-60 and polysorbate-80.

[0017] Preferably, the essential oil nano delivery carrier further comprises a preservative.

[0018] Further preferably, the preservative includes methylparaben, sodium benzoate, chlorphenesin, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, phenoxyethanol, p-hydroxyacetophenone, 1,2-hexanediol, 1,3-propanediol, propylene glycol, 1,2-pentanediol, pentylene glycol, caprylyl glycol, ethylhexylglycerin, methylisothiazolinone, methylchloroisothiazolinone, magnesium nitrate, magnesium chloride, benzalkonium bromide, benzalkonium chloride, glutaraldehyde, isopentyl glycol, o-cymene-5-ol, bis(hydroxymethyl)imidazolidinyl urea, iodopropynyl butylcarbamate, sodium hydroxymethylglycinate, DMDM ​​hydantoin, sorbic acid and its salts, benzoic acid and its salts and esters, and benzyl alcohol. One or more.

[0019] Further preferably, the preservative includes methylpropanediol, caprylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol.

[0020] More preferably, the mass percentage of the preservative is 0.005-1.2%.

[0021] In a second aspect, the present invention provides a method for preparing an essential oil nano delivery carrier based on wild soybean extract, comprising the following steps:

[0022] (a) mixing hydroxypropyl-β-cyclodextrin with water and stirring until completely dissolved to obtain solution a;

[0023] (b) mixing a polysorbate emulsifier and a wild soybean extract, and stirring until the mixed emulsifier is clear and transparent to obtain a solution b;

[0024] (c) adding the essential oil dropwise into solution a at a dropping speed of 0.6-0.8 mL per minute while stirring to obtain solution c;

[0025] (d) adding solution b dropwise into solution c at a dropping rate of 3.0-5.0 mL / min while stirring to obtain solution d;

[0026] (e) subjecting solution d to ultrasonic treatment, controlling the ultrasonic power to 400-500 W, the ultrasonic time to 5-10 min, the ultrasonic on time to 2.0-3.0 s each time, and the ultrasonic off time to 2.0-3.0 s, to prepare an essential oil nano delivery carrier.

[0027] Preferably, in step (a), the stirring speed is 400-600 rpm and the stirring time is 5-10 min.

[0028] Preferably, in step (b), the stirring speed is 100-200 rpm and the stirring time is 5-10 min.

[0029] Preferably, in step (c), the stirring speed is 400-600 rpm and the stirring time is 20-30 min.

[0030] Preferably, in step (d), the stirring speed is 400-600 rpm and the stirring time is 60-120 min.

[0031] Preferably, in step (e), a preservative is added after the ultrasonic treatment is completed.

[0032] In the process of the present invention, the material-liquid ratio, feed rate and ultrasonic treatment parameters all affect whether the state of the essential oil nano delivery carrier is transparent. Among them, the feed rate is one of the most important factors. Controlling the acceleration of the material droplets can ensure that the oil phase just entering the system is completely dispersed, avoid merging and agglomerating with the next oil phase droplets to reduce the contact area between the two phases, and increase the emulsification efficiency.

[0033] The present invention prepares an essential oil nano delivery carrier based on wild soybean extract through the above ultrasonic treatment. The nano delivery carrier has the characteristics of small particle size, strong stability, high transparency, simple operation, high repeatability, time saving and labor saving.

[0034] In the third aspect, the present invention provides the use of the above-mentioned essential oil nano delivery carrier based on wild soybean extract as a fragrance or moisturizing and repairing active ingredient in the preparation of skin care products, the essential oil nano delivery carrier has the effects of moisturizing, barrier repair, skin-friendly penetration and sustained release of fragrance, and in terms of repair, the wild soybean extract and the essential oil have a synergistic effect.

[0035] In a fourth aspect, the present invention provides the use of the above-mentioned essential oil nano delivery carrier based on wild soybean extract in the preparation of transparent aqueous cosmetics.

[0036] Beneficial effects:

[0037] 1. The present invention prepares an essential oil nano delivery carrier based on wild soybean extract by strictly limiting at least three aspects of the type of emulsifier, the ratio of polysorbate emulsifier to wild soybean extract, and the preparation process. The essential oil nano delivery carrier has the characteristics of small particle size, good high and low temperature stability, high transparency, low irritation, significant functional effect, etc., and can be widely used in skin care products as a fragrance or moisturizing and repairing active ingredient.

[0038] 2. The essential oil nano-delivery carrier based on wild soybean extract provided by the present invention is in a clear and transparent liquid state and can also be used in transparent aqueous cosmetics. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] Figure 1 This is a transmission electron microscopy image of the essential oil nanodelivery carrier.

[0040] Figure 2 The surface tension numerical scatter plot and droplet area curve of the essential oil nano delivery carrier of Example 1 / Comparative Example 4 are shown.

[0041] Figure 3 The thermogravimetric analysis curve (solid line) and the derivative thermogravimetric analysis curve (dashed line) of the essential oil nano delivery carrier of Example 2 / Comparative Example 1 are shown.

[0042] Figure 4 The thermogravimetric analysis curve (solid line) and the derivative thermogravimetric analysis curve (dashed line) of the essential oil nano-delivery carrier of Example 1 / 2 / 3 and lavender essential oil.

[0043] Figure 5The figure is a bar graph of the relative IOD / area average values ​​of ex vivo skin tissue under the action of different test solutions; compared with the blank group, the significance is indicated by #, 0.01≤P<0.05 is indicated by #, 0.001≤P<0.01 is indicated by ##, 0.0001≤P<0.001 is indicated by ###, and P<0.0001 is indicated by ####; compared with the negative control group, the significance is indicated by *, 0.01≤P<0.05 is indicated by *, 0.001≤P<0.01 is indicated by **, 0.0001≤P<0.001 is indicated by ***, and P<0.0001 is indicated by ****. DETAILED DESCRIPTION

[0044] The technical scheme of the present invention will be described clearly and completely below. Obviously, the described embodiments are only some embodiments of the present invention, rather than all embodiments. The raw materials involved in the embodiments, unless otherwise specified, are common commercially available products.

[0045] Technical solution summary:

[0046] A nano-delivery carrier of essential oil based on wild soybean extract comprises the following components: essential oil, hydroxypropyl-β-cyclodextrin, polysorbate emulsifier, wild soybean extract, preservative and water. As a further preference, the mass percentage of hydroxypropyl-β-cyclodextrin is 4.0-9.0%; the mass percentage of essential oil is 0.001-2.5%, preferably 1.0-2.5%; the mass percentage of polysorbate emulsifier in the emulsifier is 1.5-7.0%, the mass percentage of wild soybean extract in the emulsifier is 0.2-2.0%, the mass percentage of preservative is 0.005-1.2%, and the balance is deionized water.

[0047] Preferably, the types of essential oils include one or more of lavender, rose, rose geranium, damask rose, sandalwood, bergamot, patchouli, clary sage, ylang-ylang, sweet orange, pink grapefruit, mint, organic juniper berry, Atlantic cedar, (bitter) orange blossom, lemongrass, lemon, tea tree, jasmine, rosemary, frankincense, myrrh, thyme, vetiver, benzoin, white rosin, European red pine, cypress, holly, eucalyptus, oregano, ginger, cinnamon, laurel, nutmeg, fennel, clove, eucalyptus and Roman chamomile.

[0048] Preferably, the polysorbate emulsifier is selected from one or more of polysorbate-20, polysorbate-60 and polysorbate-80.

[0049] The preservatives include one or more of methylparaben, sodium benzoate, chlorphenesin, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, phenoxyethanol, p-hydroxyacetophenone, 1,2-hexanediol, 1,3-propanediol, propylene glycol, 1,2-pentanediol, pentylene glycol, caprylyl glycol, ethylhexylglycerin, methylisothiazolinone, methylchloroisothiazolinone, magnesium nitrate, magnesium chloride, benzalkonium bromide, benzalkonium chloride, glutaraldehyde, isopentyl glycol, o-cymene-5-ol, bis(hydroxymethyl)imidazolidinyl urea, iodopropynyl butylcarbamate, sodium hydroxymethylglycinate, DMDM ​​hydantoin, sorbic acid and its salts, benzoic acid and its salts and esters, and benzyl alcohol.

[0050] Preferably, the preservative includes methylpropanediol, caprylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol.

[0051] Among them: rose essential oil comes from Yaqi Industrial (Shanghai) Co., Ltd., lavender essential oil comes from Xinjiang Yiparhan Spice Co., Ltd., hydroxypropyl-β-cyclodextrin comes from Shanghai McLean Biochemical Technology Co., Ltd., polysorbate-20, polysorbate-60, and polysorbate-80 come from Beijing Solebaugh Technology Co., Ltd., and wild soybean extract comes from Lucas Meyer Cosmetics (the active ingredient is 20% wild soybean (Glycine Soja) seed extract, and the other solvent is glycerin. All embodiments and comparative examples are set according to the content of the active ingredient).

[0052] A method for preparing an essential oil nano delivery carrier based on wild soybean extract comprises the following steps:

[0053] (a) adding hydroxypropyl-β-cyclodextrin to deionized water, stirring until completely dissolved, the stirring speed is 400-600 rpm, and the stirring time is 5-10 min to obtain solution a;

[0054] (b) mixing a nonionic emulsifier polysorbate with a zwitterionic emulsifier soybean extract, stirring and dispersing, the stirring speed is 100-200 rpm, the stirring time is 5-10 min, and the mixed emulsifier is in a clear and transparent state to obtain a solution b;

[0055] (c) adding the essential oil dropwise into solution a at a dropping speed of 0.6-0.8 mL per minute, stirring while dropping, at a stirring speed of 400-600 rpm, and a stirring time of 20-30 min to obtain solution c;

[0056] (d) adding solution b to solution c at a dropping speed of 3.0-5.0 mL per minute, stirring at a stirring speed of 400-600 rpm for 60-120 min, to obtain solution d;

[0057] (e) Solution d is ultrasonically treated by an ultrasonic cell crusher, and the ultrasonic power is controlled to be 400-500 W, the ultrasonic time is 5-10 min, the ultrasonic on time is 2.0-3.0 s each time, and the ultrasonic off time is 2.0-3.0 s. After completion, preservatives methyl propanediol, caprylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol are added to prepare an essential oil nano delivery carrier.

[0058] Embodiment 1:

[0059] A wild soybean extract-based essential oil nano delivery carrier comprises the following components, measured by mass percentage: 1.3% lavender essential oil, 4.6% hydroxypropyl-β-cyclodextrin, 1.7% polysorbate-80, 1.2% wild soybean extract, 0.4785% methylpropanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0060] The preparation method of the essential oil nano delivery carrier based on wild soybean extract comprises the following steps:

[0061] A. Weigh lavender essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 80, soybean extract, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0062] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 400 rpm until completely dissolved for 5 min to obtain solution a;

[0063] C. Mix polysorbate 80 and soybean extract, stir at a stirring speed of 100 rpm until the mixed emulsifier is clear and transparent, and stir for 5 minutes to obtain solution b;

[0064] D. Lavender essential oil was added dropwise into solution a at a dropping speed of 0.6 mL per minute, and stirred while adding dropwise at a stirring speed of 600 rpm for 30 min to obtain solution c;

[0065] E. Add solution b into solution c at a dropping speed of 4.0 mL per minute, stirring at a stirring speed of 400 rpm for 120 min, to obtain solution d;

[0066] F. Ultrasonic treatment of solution d was performed by an ultrasonic cell crusher, with the ultrasonic power controlled at 500 W, the ultrasonic time at 10 min, the ultrasonic on time at 2.0-3.0 s each time, and the ultrasonic off time at 2.0-3.0 s. After completion, preservatives methylpropanediol, caprylylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare an essential oil nano delivery carrier.

[0067] Embodiment 2:

[0068] A wild soybean extract-based essential oil nano delivery carrier comprises the following components, measured by mass percentage: 2.2% lavender essential oil, 7.7% hydroxypropyl-β-cyclodextrin, 6.6% polysorbate-60, 1.3% wild soybean extract, 0.4785% methylpropanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0069] The preparation method of the essential oil nano delivery carrier based on wild soybean extract comprises the following steps:

[0070] A. Weigh lavender essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 60, soybean extract, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0071] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 500 rpm until completely dissolved for 7 min to obtain solution a;

[0072] C. Mix polysorbate 60 and soybean extract, stir at a stirring speed of 150 rpm until the mixed emulsifier is clear and transparent, and stir for 8 minutes to obtain solution b;

[0073] D. Lavender essential oil was added dropwise into solution a at a dropping speed of 0.7 mL per minute, and stirred while adding dropwise at a stirring speed of 500 rpm for 25 min to obtain solution c;

[0074] E. Add solution b into solution c at a dropping speed of 3.0 mL per minute, stirring at a stirring speed of 600 rpm for 80 min to obtain solution d;

[0075] F. Ultrasonic treatment of solution d was performed by an ultrasonic cell crusher, with the ultrasonic power controlled at 450 W, the ultrasonic time at 10 min, the ultrasonic on time at 2.0-3.0 s, and the ultrasonic off time at 2.0-3.0 s. After completion, preservatives such as methylpropanediol, caprylylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare an essential oil nano-delivery carrier.

[0076] Embodiment 3:

[0077] A wild soybean extract-based essential oil nano delivery carrier comprises the following components, measured by mass percentage: 1.6% lavender essential oil, 4.4% hydroxypropyl-β-cyclodextrin, 5.9% polysorbate-20, 0.3% wild soybean extract, 0.4785% methylpropanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0078] The preparation method of the essential oil nano delivery carrier based on wild soybean extract comprises the following steps:

[0079] A. Weigh lavender essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 20, soybean extract, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0080] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 600 rpm until completely dissolved for 10 min to obtain solution a;

[0081] C. Mix polysorbate 20 and soybean extract, stir at a stirring speed of 200 rpm until the mixed emulsifier is clear and transparent, and stir for 10 minutes to obtain solution b;

[0082] D. Lavender essential oil was added dropwise into solution a at a dropping speed of 0.8 mL per minute, and stirred while adding dropwise at a stirring speed of 400 rpm for 20 min to obtain solution c;

[0083] E. Add solution b into solution c at a dropping speed of 4.0 mL per minute, stirring at a stirring speed of 500 rpm for 100 min, to obtain solution d;

[0084] F. Ultrasonic treatment of solution d was performed by an ultrasonic cell crusher, with the ultrasonic power controlled at 400 W, the ultrasonic time at 10 min, the ultrasonic on time at 2.0-3.0 s each time, and the ultrasonic off time at 2.0-3.0 s. After completion, preservatives methylpropanediol, caprylylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare an essential oil nano delivery carrier.

[0085] Embodiment 4:

[0086] A wild soybean extract-based essential oil nano delivery carrier comprises the following components, measured by mass percentage: 1.6% rose essential oil, 4.4% hydroxypropyl-β-cyclodextrin, 5.9% polysorbate-20, 0.3% wild soybean extract, 0.4785% methylpropanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0087] The preparation method of the essential oil nano delivery carrier based on wild soybean extract comprises the following steps:

[0088] A. Weigh rose essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 20, wild soybean extract, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0089] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 600 rpm until completely dissolved for 10 min to obtain solution a;

[0090] C. Mix polysorbate 20 and soybean extract, stir at a stirring speed of 200 rpm until the mixed emulsifier is clear and transparent, and stir for 10 minutes to obtain solution b;

[0091] D. Rose essential oil was added dropwise into solution a at a dropping speed of 0.7 mL per minute, and stirred while adding dropwise at a stirring speed of 400 rpm for 20 min to obtain solution c.

[0092] E. Add solution b into solution c at a dropping speed of 5.0 mL per minute, stirring at a stirring speed of 500 rpm for 100 min to obtain solution d;

[0093] F. Ultrasonic treatment of solution d was performed by an ultrasonic cell crusher, with the ultrasonic power controlled at 400 W, the ultrasonic time at 5 min, the ultrasonic on time at 2.0-3.0 s each time, and the ultrasonic off time at 2.0-3.0 s. After completion, preservatives methylpropanediol, caprylylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare an essential oil nano delivery carrier.

[0094] Comparative Example 1: No wild soybean extract added

[0095] An essential oil nano delivery carrier comprises the following components by mass percentage: 2.2% lavender essential oil, 7.7% hydroxypropyl-β-cyclodextrin, 10.0% polysorbate-60, 0.4785% methylpropanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0096] The preparation method of the essential oil nano delivery carrier comprises the following steps:

[0097] A. Weigh lavender essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 60, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0098] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 500 rpm until completely dissolved for 7 min to obtain solution a;

[0099] C. Add lavender essential oil dropwise into solution a at a dropping speed of 0.7 mL per minute, stirring while dropping, at a stirring speed of 500 rpm, and a stirring time of 25 min to obtain solution b;

[0100] D. Add polysorbate 60 dropwise into solution b at a dropping speed of 3.0 mL per minute, stirring at a stirring speed of 600 rpm for 80 min to obtain solution c;

[0101] E. Ultrasonic treatment of solution c was performed by an ultrasonic cell crusher, with the ultrasonic power controlled at 450 W, the ultrasonic time at 10 min, the ultrasonic on time at 2.0-3.0 s, and the ultrasonic off time at 2.0-3.0 s. After completion, preservatives such as methylpropanediol, caprylylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare an essential oil nano-delivery carrier.

[0102] Comparative Example 2: No Ultrasonic Cell Disintegrator Treatment

[0103] A wild soybean extract-based essential oil nano delivery carrier comprises the following components, measured by mass percentage: 1.6% lavender essential oil, 4.4% hydroxypropyl-β-cyclodextrin, 5.9% polysorbate-20, 0.3% wild soybean extract, 0.4785% methylpropanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0104] The preparation method of the essential oil nano delivery carrier based on wild soybean extract comprises the following steps:

[0105] A. Weigh lavender essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 20, soybean extract, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0106] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 600 rpm until completely dissolved for 10 min to obtain solution a;

[0107] C. Mix polysorbate 20 and soybean extract, stir at a stirring speed of 200 rpm until the mixed emulsifier is clear and transparent, and stir for 10 minutes to obtain solution b;

[0108] D. Lavender essential oil was added dropwise into solution a at a dropping speed of 0.8 mL per minute, and stirred while adding dropwise at a stirring speed of 400 rpm for 20 min to obtain solution c;

[0109] E. Add solution b into solution c at a dropping speed of 4.0 mL per minute, stirring at a stirring speed of 500 rpm for 100 min, to obtain solution d;

[0110] F. Add preservatives methyl propanediol, caprylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol to solution d to prepare an essential oil nano delivery carrier. The obtained essential oil nano delivery carrier is light yellow and translucent, and has stratification and oiling, and is extremely unstable.

[0111] Comparative Example 3: Direct mixing without dripping

[0112] A wild soybean extract-based essential oil nano delivery carrier comprises the following components, measured by mass percentage: 1.3% lavender essential oil, 4.6% hydroxypropyl-β-cyclodextrin, 1.7% polysorbate-80, 1.2% wild soybean extract, 0.4785% methylpropanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0113] The preparation method of the essential oil nano delivery carrier based on wild soybean extract comprises the following steps:

[0114] A. Weigh lavender essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 80, soybean extract, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0115] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 400 rpm until completely dissolved for 5 min to obtain solution a;

[0116] C. Mix polysorbate 80 and soybean extract, stir at a stirring speed of 100 rpm until the mixed emulsifier is clear and transparent, and stir for 5 minutes to obtain solution b;

[0117] D. Add lavender essential oil directly into solution a and stir at a stirring speed of 600 rpm for 30 min to obtain solution c;

[0118] E. Add solution b directly into solution c and stir at a stirring speed of 400 rpm for 120 min to obtain solution d;

[0119] F. Ultrasonic treatment of solution d was performed by an ultrasonic cell crusher, with the ultrasonic power controlled at 500 W, the ultrasonic time at 10 min, the ultrasonic on time at 2.0-3.0 s each time, and the ultrasonic off time at 2.0-3.0 s. After completion, preservatives methylpropanediol, caprylylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare an essential oil nano delivery carrier.

[0120] Comparative Example 4: Replacement of wild soybean extract

[0121] An essential oil nano delivery carrier comprises the following components, measured by mass percentage: 1.3% lavender essential oil, 4.6% hydroxypropyl-β-cyclodextrin, 1.7% polysorbate-80, 1.2% inulin lauryl carbamate, 0.4785% methylpropanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0122] The preparation method of the essential oil nano delivery carrier comprises the following steps:

[0123] A. Weigh lavender essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 80, inulin lauryl carbamate, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0124] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 400 rpm until completely dissolved for 5 min to obtain solution a;

[0125] C. Mixing polysorbate 80 and inulin lauryl carbamate, stirring at a stirring speed of 100 rpm for 5 min to obtain solution b;

[0126] D. Lavender essential oil was added dropwise into solution a at a dropping speed of 0.6 mL per minute, and stirred while adding dropwise at a stirring speed of 600 rpm for 30 min to obtain solution c;

[0127] E. Add solution b into solution c at a dropping speed of 4.0 mL per minute, stirring at a stirring speed of 400 rpm for 120 min, to obtain solution d;

[0128] F. Ultrasonic treatment of solution d was performed by an ultrasonic cell crusher, with the ultrasonic power controlled at 500 W, the ultrasonic time at 10 min, the ultrasonic on time at 2.0-3.0 s each time, and the ultrasonic off time at 2.0-3.0 s. After completion, preservatives methylpropanediol, caprylylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare an essential oil nano delivery carrier.

[0129] Comparative Example 5: Replacement of wild soybean extract

[0130] An essential oil nano delivery carrier comprises the following components, measured by mass percentage: 1.3% lavender essential oil, 4.6% hydroxypropyl-β-cyclodextrin, 1.7% polysorbate-80, 1.2% cocamidopropyl hydroxysulfobetaine, 0.4785% methylpropanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0131] The preparation method of the essential oil nano delivery carrier comprises the following steps:

[0132] A. Weigh lavender essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 80, cocamidopropyl hydroxysulfobetaine, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0133] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 400 rpm until completely dissolved for 5 min to obtain solution a;

[0134] C. Mixing polysorbate 80 and cocamidopropyl hydroxysulfobetaine, stirring at a stirring speed of 100 rpm for 5 min to obtain a solution b;

[0135] D. Lavender essential oil was added dropwise into solution a at a dropping speed of 0.6 mL per minute, and stirred while adding dropwise at a stirring speed of 600 rpm for 30 min to obtain solution c;

[0136] E. Add solution b into solution c at a dropping speed of 4.0 mL per minute, stirring at a stirring speed of 400 rpm for 120 min, to obtain solution d;

[0137] F. The solution d was ultrasonically treated by an ultrasonic cell crusher, the ultrasonic power was controlled to be 500W, the ultrasonic time was 10min, the ultrasonic on time was 2.0-3.0s each time, and the ultrasonic off time was 2.0-3.0s. After completion, preservatives methyl propanediol, caprylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare an essential oil nano delivery carrier. The obtained essential oil nano delivery carrier was white and opaque, and stratification and oiling occurred, and the state was extremely unstable.

[0138] Comparative Example 6: Replacement of wild soybean extract

[0139] An essential oil nano delivery carrier comprises the following components, measured by mass percentage: 1.3% lavender essential oil, 4.6% hydroxypropyl-β-cyclodextrin, 1.7% polysorbate-80, 1.2% potassium cetyl phosphate, 0.4785% methyl propanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0140] The preparation method of the essential oil nano delivery carrier comprises the following steps:

[0141] A. Weigh lavender essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 80, potassium cetyl phosphate, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0142] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 400 rpm until completely dissolved for 5 min to obtain solution a;

[0143] C. Mixing polysorbate 80 and potassium cetyl phosphate, stirring at a stirring speed of 100 rpm for 5 min, to obtain solution b;

[0144] D. Lavender essential oil was added dropwise into solution a at a dropping speed of 0.6 mL per minute, and stirred while adding dropwise at a stirring speed of 600 rpm for 30 min to obtain solution c;

[0145] E. Add solution b into solution c at a dropping speed of 4.0 mL per minute, stirring at a stirring speed of 400 rpm for 120 min, to obtain solution d;

[0146] F. The solution d was ultrasonically treated by an ultrasonic cell crusher, the ultrasonic power was controlled to be 500W, the ultrasonic time was 10min, the ultrasonic on time was 2.0-3.0s each time, and the ultrasonic off time was 2.0-3.0s. After completion, preservatives methyl propanediol, caprylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare an essential oil nano delivery carrier. The obtained essential oil nano delivery carrier was white and opaque, and stratification, oiling and precipitation occurred, and the state was extremely unstable.

[0147] Comparative Example 7: Replacement of wild soybean extract

[0148] An essential oil nano delivery carrier comprises the following components, measured by mass percentage: 1.3% lavender essential oil, 4.6% hydroxypropyl-β-cyclodextrin, 1.7% polysorbate-80, 1.2% cetyltrimethylammonium chloride, 0.4785% methylpropanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0149] The preparation method of the essential oil nano delivery carrier comprises the following steps:

[0150] A. Weigh lavender essential oil, hydroxypropyl-β-cyclodextrin, polysorbate 80, cetyltrimethylammonium chloride, methylpropylene glycol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0151] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 400 rpm until completely dissolved for 5 min to obtain solution a;

[0152] C. Mix polysorbate 80 and cetyltrimethylammonium chloride, and stir at a stirring speed of 100 rpm for 5 min to obtain solution b;

[0153] D. Lavender essential oil was added dropwise into solution a at a dropping speed of 0.6 mL per minute, and stirred while adding dropwise at a stirring speed of 600 rpm for 30 min to obtain solution c;

[0154] E. Add solution b into solution c at a dropping speed of 4.0 mL per minute, stirring at a stirring speed of 400 rpm for 120 min, to obtain solution d;

[0155] F. The solution d was ultrasonically treated by an ultrasonic cell crusher, the ultrasonic power was controlled to be 500W, the ultrasonic time was 10min, the ultrasonic on time was 2.0-3.0s each time, and the ultrasonic off time was 2.0-3.0s. After completion, preservatives methyl propanediol, capryl hydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare an essential oil nano delivery carrier. The obtained essential oil nano delivery carrier was white and opaque, and oil was discharged, and the state was extremely unstable.

[0156] Comparative Example 8: Hollow Nano-Delivery Carrier

[0157] A hollow nano delivery carrier comprises the following components by mass percentage: 4.6% hydroxypropyl-β-cyclodextrin, 1.7% polysorbate-80, 1.2% wild soybean extract, 0.4785% methyl propanediol, 0.066% caprylhydroxamic acid, 0.0055% glyceryl caprylate, 0.55% 1,2-hexanediol, and the balance is deionized water.

[0158] The preparation method of the hollow nano delivery carrier comprises the following steps:

[0159] A. Weigh hydroxypropyl-β-cyclodextrin, polysorbate 80, wild soybean extract, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, 1,2-hexanediol, and deionized water according to the formula;

[0160] B. Mix hydroxypropyl-β-cyclodextrin with deionized water, and stir with a stirrer at 400 rpm until completely dissolved for 5 min to obtain solution a;

[0161] C. Mix polysorbate 80 and soybean extract, stir at a stirring speed of 100 rpm until the mixed emulsifier is clear and transparent, and stir for 5 minutes to obtain solution b;

[0162] D. Add solution b into solution a at a dropping speed of 4.0 mL per minute, stirring at a stirring speed of 400 rpm for 120 min, to obtain solution c;

[0163] E. Solution c was ultrasonically treated with an ultrasonic cell crusher, with the ultrasonic power controlled at 500 W, the ultrasonic time at 10 min, the ultrasonic on time at 2.0-3.0 s each time, and the ultrasonic off time at 2.0-3.0 s. After completion, preservatives methylpropanediol, caprylylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol were added to prepare a hollow nano delivery carrier.

[0164] Comparative Example 9: Lavender Essential Oil

[0165] Comparative Example 10:

[0166] In order to conduct an efficacy comparison test, Comparative Example 10 was set up. Comparative Example 10 was a mixed dilution of the samples of Comparative Example 8 and Comparative Example 9, and the solvent was EpiGrowth culture medium containing 0.1% DMSO, wherein the final concentration of lavender essential oil / hollow nano delivery carrier was consistent with the separate test solution of Comparative Example 8 and the test solution of Comparative Example 9 during the efficacy test.

[0167] Experimental example:

[0168] (I) Particle size test: The particle size is tested and analyzed by a multi-angle particle size analyzer (Omni, Brookhaven, USA); the polydispersity index (PDI) is one of the important parameters to characterize the uniformity of particle distribution. The value is usually measured by dynamic light scattering (DLS), which reflects the width and uniformity of the particle size distribution. The following is a description of the particle size and appearance results of the nano-delivery carriers prepared in various embodiments and comparative examples of the present invention, wherein the test conditions for appearance stability are room temperature: 20-25°C, high temperature: 45°C, low temperature: -18°C and 4°C, high and low temperature cycle: -18°C, 4°C, 45°C hot and cold cycle, 24h at each temperature, and illumination: 4500±500Lux.

[0169] Table 1. Appearance, stability and particle size of nano-delivery vectors

[0170]

[0171]

[0172] Table 1 (Continued). Appearance, stability and particle size results of nano-delivery vectors

[0173]

[0174] From the results in Table 1, it can be seen that the nano-delivery carriers of Examples 1 to 4 have significant advantages in appearance, stability and particle size compared to Comparative Examples 1 to 7. Among them:

[0175] Comparative Example 2 and Comparative Example 1 show that when wild soybean extract is not added, under the same preparation conditions and process, the particle size of the obtained nano delivery carrier becomes larger, the PDI becomes larger, and the initial appearance is white and opaque. After stability inspection, it was also found that it was stratified and oily. This is attributed to the high surface activity and spatial interaction of polysorbate emulsifiers at the O / W interface, which will weaken over time, and the interfacial oil droplets will gradually accelerate aggregation and eventually lead to oil. The above results show that it is impossible to prepare a stable and transparent nano delivery carrier by relying solely on a simple host-guest interaction between polysorbate emulsifiers and hydroxypropyl-β-cyclodextrin.

[0176] Comparative Example 3 and Comparative Example 2 show that when ultrasonic treatment is not carried out in the preparation process of nano delivery carrier, the nano delivery carrier appearance obtained shows a light yellow translucent state, and stratification and oiling occur. This is attributed to the fact that ultrasound can accurately control the intensity and frequency of liquid cavitation by controlling the frequency, thereby controlling the particle size and stability of the nano delivery carrier. Ultrasonic treatment can also improve the solubility and thermal stability of the inclusion formed by essential oil and hydroxypropyl-β-cyclodextrin by improving the complex structure and increasing molecular interactions (such as hydrogen bonds and hydrophobic interactions). Therefore, the ultrasonic assistance of specific parameters is required in the preparation process of the nano delivery carrier of the present invention.

[0177] Comparative Example 1 and Comparative Example 3 show that when the feed rate is not controlled during the preparation of the nano-delivery carrier, the particle size of the nano-delivery carrier finally obtained becomes larger, and the initial appearance is a yellow-white translucent state. This shows that the mini-emulsion and monodisperse emulsion formed by the appropriate feed rate can prevent the oil droplets from agglomerating during the preparation process, so that the oil phase entering the system is fully and evenly dispersed, the two-phase contact area increases, the emulsification rate is increased, and the nano-delivery carrier with dynamic and thermodynamic stability is formed by high-energy homogenization and low-energy spontaneous emulsification. Therefore, transparent and stable nano-delivery carriers need to strictly control the feed rate.

[0178] Comparative Example 1 and Comparative Examples 4 to 7 show that compared with other types of emulsifiers and mixed emulsifiers composed of polysorbate emulsifiers, the nano delivery carrier prepared by the mixed emulsifier of wild soybean extract and polysorbate emulsifier has better emulsification effect and is more thorough, and the obtained nano delivery carrier has a smaller particle size, a smaller PDI value, and a more stable and transparent state. This may be due to the soybean lecithin contained in the wild soybean extract, which is easy to form a buffer elastic layer with a small surface tension at the O / W interface, promotes the polysorbate emulsifier to build a "channel" between the main hydroxypropyl-β-cyclodextrin and the guest molecule essential oil, self-assembles to form a three-phase stable system of the main body, the guest, and the emulsifier, and promotes the guest molecule essential oil to quickly enter the main hydrophobic cavity, and finally prepares a small particle size, strong stability, high transparency, simple operation, high repeatability, and time-saving and labor-saving essential oil nano delivery carrier.

[0179] On the other hand, in comparison with Example 3 and Example 4, the initial appearance is transparent, the particle size is 10-15 nm, and the PDI is 0.160 and 0.084 respectively. This shows that the preparation method of the essential oil nano delivery carrier of the present application is effective for one or more essential oils and has universal applicability.

[0180] The above results show that the particle size of the essential oil nano-delivery carrier of the present invention is 10-30 nm, transparent and stable.

[0181] (II) Morphological Characterization: The following is a microscopic description of the morphology of the essential oil nano-delivery carrier based on wild soybean extract prepared in Example 3 of the present invention:

[0182] The microscopic morphology of the essential oil nano-delivery carrier was characterized by transmission electron microscopy (JEOL JEM-F200, Japan). Figure 1 As shown, from Figure 1 It can be seen that the particle size of the essential oil nano-delivery carrier prepared in Example 3 is about 10-30 nm, and is round or elliptical in shape, which proves that the essential oil has been successfully encapsulated, and also further confirms the accuracy of the particle size test results.

[0183] (III) Surface tension: The following is an explanation of the surface tension of the nano-delivery carriers prepared in Example 1 and Comparative Example 4 of the present invention:

[0184] Surface tension refers to the force per unit length on the interface between a liquid and another phase (which can be a gas or another liquid) generated by the imbalance of molecular attraction on the surface layer of a liquid. It is mainly applicable to liquids. The smaller the surface tension, the more conducive it is to the formation of essential oil nano-delivery carriers, and the stronger the stability of the system. The surface tension is tested using the hanging drop method using a contact angle meter (Biolin Theta flex, Sweden). The basic principle of measuring surface tension by the hanging drop method is that when a droplet is suspended statically at the mouth of a capillary, the shape of the droplet mainly depends on the balance of gravity and surface tension. Therefore, by measuring the shape of the droplet, the surface tension of the liquid can be inferred. During the experiment, the sample volume was set to 8 μL, the droplet was suspended in the air, and the test lasted for 1 minute. A hanging drop of appropriate volume was automatically formed under the control of the software, and the hanging drop was waited for 60 seconds. The corresponding surface tension value was obtained by image analysis and calculation of the formed hanging drop.

[0185] Depend on Figure 2 It can be seen that the emulsifiers in Example 1 and Comparative Example 4 migrated faster on the droplet surface, and quickly reached a state of equilibrium before the droplets were fully formed, and the emulsifier molecules were fully arranged on the surface. This is mainly due to the fact that the emulsifiers in the two are relatively small, and the solvent deionized water has a relatively large content, which is similar to a single liquid and has no obvious content difference. Therefore, there is no process of emulsifier molecules migrating from the inside of the solvent to the surface, so its surface tension curve presents a stable trend. In the first 60s, the overall trend stability of the surface tension value scatter plot of Example 1 is better than that of Comparative Example 4, and the surface tension values ​​of Example 1 are generally smaller than those of Comparative Example 4.

[0186] The above results confirm that soybean lecithin contained in wild soybean extract can easily form a buffer elastic layer with low surface tension at the O / W interface, which further reduces the surface tension of the entire system of essential oil nano-delivery carrier and enhances its stability.

[0187] (IV) Encapsulation efficiency: The following is a description of the thermal stability and sustained-release performance of the essential oil nano-delivery carrier based on wild soybean extract prepared in each embodiment of the present invention:

[0188] The thermal stability and sustained release performance of the essential oil nano-delivery carrier were analyzed by using a thermogravimetric analyzer (Netzsch STA449F3, Germany). About 3 to 5 mg of the sample was heated at a heating rate of 10°C / min in the range of 30 to 800°C under a constant flow of nitrogen to study the thermal stability of Examples 1 / 2 / 3, Comparative Example 1 and lavender essential oil and the sustained release performance of Examples 1 / 2 / 3.

[0189] Thermogravimetric analysis (TG) curve represents the weight change of the sample with temperature during the program temperature process, while the derivative thermogravimetry (DTG) curve is the differential equation of the thermogravimetric curve, which represents the weight change rate with temperature. The peak of the DTG curve corresponds to the inflection point of the TG curve, which is the maximum point of the weight loss rate. The number of peaks in the DTG curve is equal to the number of steps in the TG curve. Figure 3 It can be seen that the thermal decomposition process of the essential oil nano delivery carrier prepared in Example 2 is mainly divided into four processes: 30-100°C is mainly the volatilization of water and a small amount of impurities; the weight loss peak at 180-250°C is mainly due to the gradual carbonization and decomposition of the polysorbate emulsifier, and the essential oil wrapped in the nano delivery carrier also begins to be gradually released at this stage; the small amount of weight loss at 300-350°C is mainly attributed to the decomposition of the wild soybean extract; at a temperature of about 380°C, the wall material hydroxypropyl-β-cyclodextrin is finally carbonized and decomposed. In contrast, the thermogravimetric analysis results of Comparative Example 1 only have two main weight loss peaks, which are around 30-100°C and 350-400°C, respectively, which may be attributed to the decomposition of water and a small amount of impurities and the carbonization decomposition of hydroxypropyl-β-cyclodextrin, respectively. This also confirms the instability of the encapsulation system of Comparative Example 1. When the thermogravimetric analysis test was performed, the sample had already produced oil. The tested sample mainly contained water and hydroxypropyl-β-cyclodextrin, which is consistent with its stability appearance results, further indicating that the nano-delivery carrier containing wild soybean extract has good thermal stability.

[0190] Depend on Figure 4 It can be seen that the thermogravimetric analysis results of Examples 1 / 2 / 3 have basically the same trend. Figure 3The thermogravimetric analysis results of Example 2 are consistent, and the final weight loss rates (wt.%) of Examples 1 / 2 / 3 are 86.90%, 71.65%, and 80.35%, respectively. The difference in weight loss rates among the three is mainly attributed to the volatilization of moisture and a small amount of impurities in the first 100°C, which is also consistent with the order of solid content in the preparation conditions of Examples 1 / 2 / 3. From the thermogravimetric analysis results of lavender essential oil, it can be learned that the essential oil volatilizes rapidly and continuously within 30-200°C until it is basically completely decomposed. In contrast, the essential oil encapsulated in Examples 1 / 2 / 3 is gradually released mainly within the range of 180-400°C, further indicating that the nano delivery carrier delays the release of the essential oil and has a sustained release effect.

[0191] The above results prove that the essential oil nano-delivery carrier has excellent thermal stability and has a long-lasting sustained-release effect.

[0192] (V) Efficacy test: The following is an illustration of the efficacy test of the nano-delivery carriers prepared in the embodiments and comparative examples of the present invention:

[0193] The efficacy test was conducted by the following experimental method: UVA+UVB was used to irradiate the ex vivo skin tissue to establish a skin photoaging model. The experiment set up a blank control group and a negative control group (30J / cm 2 UVA+50mJ / cm 2 UVB) and sample group (30J / cm 2 UVA+50mJ / cm 2 UVB + Example 1 / Comparative Example 3 / 4 / 8 / 9 / 10), 3 replicates per group. After culturing the ex vivo skin tissue for 2 days, the remaining groups, except the blank control group, began to be irradiated and dosed, with a daily irradiation dose of UVA 30 J / cm 2 and UVB 50mJ / cm 2 , the culture medium was discarded during irradiation and replaced with PBS buffer, UVA irradiation was performed first, and then UVB irradiation was performed continuously for 4 days. Fresh culture medium was replaced after each irradiation, and surface drug administration was performed. The test liquids of different groups were added to the surface of the ex vivo skin tissue, and the added volume of the test liquid was 10 μL. After 4 days of continuous irradiation, the ex vivo skin tissue was cultured for another 3 days, and only drug administration was performed without irradiation. After the culture was completed, the test liquid remaining on the surface of the ex vivo skin tissue was cleaned and the residual liquid was removed. 4% paraformaldehyde was used for fixation, followed by tissue embedding and tissue sectioning. After the baked slices were dewaxed, loricrin (LOR) was immunofluorescently stained, and photographed under a microscope within 24 hours. Three pictures of different fields of view were collected, and the target signals in the pictures were analyzed by relative IOD using Ipwin32 image analysis software, and the average value was calculated. The relative IOD / area average value was calculated based on the blank control group to characterize the relative expression of the protein.

[0194] Among them, the test solution is the dilution solution of the samples in Example 1 and Comparative Examples 3 / 4 / 8, the dilution multiple is 10 times, and the dilution solvent is EpiGrowth culture solution; the test solution of Comparative Example 9 is 0.13% lavender essential oil, the solvent is EpiGrowth culture solution containing 0.1% DMSO, and Comparative Example 10 is a stock solution test; the test solution of the blank control group and the negative control group is blank EpiGrowth culture solution.

[0195] Loricrin (LOR) is the main component of the corneum membrane in terminally differentiated keratinocytes. In the stratum corneum, loricrin is cross-linked to the corneum membrane by transglutaminase and plays an important role in the barrier repair function of the epidermis. Figure 5 It can be seen that compared with the blank control group, under ultraviolet irradiation, the LOR content of the negative control group was significantly reduced (P<0.01), indicating that ultraviolet irradiation can damage the skin barrier structure-related proteins and cause skin damage. Compared with the negative control group, the use of Example 1 / Comparative Example 3 / 4 / 8 / 9 / 10 after ultraviolet irradiation can significantly increase the content of LOR (P<0.05), which has a certain repair effect on the skin barrier, but the lifting ability is different. The lifting rates of LOR in Example 1 / Comparative Example 3 / 4 / 8 / 9 / 10 are 267.30%, 159.39, 98.81, 53.03%, 74.83%, and 138.52%, respectively. Comparative Example 8 and Comparative Example 9 are hollow nano delivery carriers and lavender essential oil, respectively, and both have a certain LOR lifting effect, indicating that the use of wild soybean extract and lavender essential oil alone has a certain lifting effect on LOR. The LOR improvement rate of Example 1 is the highest, and the LOR improvement rate of Comparative Example 3 is lower than that of Example 1, mainly because Example 1 has a suitable dripping speed, the nano delivery carrier system after encapsulation is stable and complete, and the repair performance is more significant. The LOR improvement rate of Comparative Example 4 is lower than that of Example 1, which is attributed to the presence of wild soybean extract in Example 1, indicating that the wild soybean extract present in the nano delivery carrier has a good barrier repair effect. The LOR improvement effect of Comparative Example 10 is lower than that of Example 1, which may be attributed to the volatile characteristics of the essential oil itself. The unencapsulated essential oil is easy to dissipate and has a short action time on the skin, which directly affects the barrier repair effect. The LOR improvement rates of Example 1 and Comparative Example 3 / 10 are higher than those of Comparative Example 8 / 9, which shows that the wild soybean extract and lavender essential oil have a synergistic effect in barrier repair.

[0196] Table 2. Effects of the test solutions of Example 1 / Comparative Examples 3 / 4 / 8 / 9 / 10 on the relative content of loricrin

[0197]

[0198] The above results further verify that the essential oil nanodelivery carrier based on wild soybean extract has good barrier repair effect, and the essential oil and wild soybean extract in the essential oil nanodelivery carrier have a synergistic effect in repair.

[0199] (VI) Formulation Application: The following is a description of the transparent aqueous formulation of the essential oil nano-delivery carrier based on wild soybean extract prepared in Example 3 of the present invention:

[0200] The aqueous product was prepared according to the aqueous formulation in Table 3, and the stability of the aqueous product was tested.

[0201] Table 3. Formulation and stability test results of aqueous products

[0202]

[0203] As can be seen from Table 3, the aqueous product prepared by the essential oil nano delivery carrier provided in the present application has the characteristics of good stability and high transparency.

[0204] The above proves that it is feasible to apply the essential oil nano delivery carrier based on wild soybean extract provided in the present application in the formulation of transparent aqueous cosmetics.

Claims

1. An essential oil nano delivery carrier based on wild soybean extract, characterized in that: Includes the following ingredients: essential oils, hydroxypropyl-β-cyclodextrin, polysorbate emulsifier, wild soybean extract, water.

2. The essential oil nano delivery carrier according to claim 1, characterized in that: The mass percentage of the hydroxypropyl-β-cyclodextrin is 4.0-9.0%; the mass percentage of the essential oil is 0.001-2.5%, and more preferably 1.0-2.5%; the mass percentage of the polysorbate emulsifier is 1.5-7.0%; the mass percentage of the wild soybean extract is 0.2-2.0%, and the balance is deionized water.

3. The essential oil nano delivery carrier according to claim 1, characterized in that The essential oils include one or more of lavender, rose, rose geranium, damask rose, sandalwood, bergamot, patchouli, clary sage, ylang-ylang, sweet orange, pink grapefruit, mint, organic juniper berry, Atlantic cedar, (bitter) orange blossom, lemongrass, lemon, tea tree, jasmine, rosemary, frankincense, myrrh, thyme, vetiver, benzoin, galbanum, Scots pine, cypress, holly, eucalyptus, oregano, ginger, cinnamon, bay, nutmeg, fennel, clove, eucalyptus and Roman chamomile.

4. The essential oil nano delivery carrier according to claim 1, characterized in that: The polysorbate emulsifier is selected from one or more of polysorbate-20, polysorbate-60 and polysorbate-80.

5. The essential oil nano delivery carrier according to claim 1, characterized in that: The essential oil nano delivery vehicle also includes a preservative; Preferably, the preservative includes one or more of methylparaben, sodium benzoate, chlorphenesin, methylpropanediol, caprylhydroxamic acid, glyceryl caprylate, phenoxyethanol, p-hydroxyacetophenone, 1,2-hexanediol, 1,3-propanediol, propylene glycol, 1,2-pentanediol, pentylene glycol, caprylyl glycol, ethylhexylglycerin, methylisothiazolinone, methylchloroisothiazolinone, magnesium nitrate, magnesium chloride, benzalkonium bromide, benzalkonium chloride, glutaraldehyde, isopentyl glycol, o-cymene-5-ol, bis(hydroxymethyl)imidazolidinyl urea, iodopropynyl butylcarbamate, sodium hydroxymethylglycinate, DMDM ​​hydantoin, sorbic acid and its salts, benzoic acid and its salts and esters, and benzyl alcohol; Further preferably, the preservative comprises methylpropanediol, caprylhydroxamic acid, glyceryl caprylate and 1,2-hexanediol; More preferably, the mass percentage of the preservative is 0.005-1.2%.

6. The essential oil nano delivery carrier according to claim 1, characterized in that: The essential oil nano delivery carrier is a transparent liquid with a color ranging from light yellow to dark yellow, a microscopic structure showing a round or oval shape, and a particle size of 10-30 nm.

7. A method for preparing an essential oil nano-delivery carrier based on wild soybean extract according to claim 1, characterized in that: The following steps are involved: (a) mixing hydroxypropyl-β-cyclodextrin with water and stirring until completely dissolved to obtain solution a; (b) mixing a polysorbate emulsifier and a wild soybean extract, and stirring until the mixed emulsifier is clear and transparent to obtain a solution b; (c) adding the essential oil dropwise into solution a at a dropping speed of 0.6-0.8 mL per minute while stirring to obtain solution c; (d) adding solution b dropwise into solution c at a dropping rate of 3.0-5.0 mL / min while stirring to obtain solution d; (e) subjecting solution d to ultrasonic treatment, controlling the ultrasonic power to 400-500 W, the ultrasonic time to 5-10 min, the ultrasonic on time to 2.0-3.0 s each time, and the ultrasonic off time to 2.0-3.0 s, to prepare an essential oil nano delivery carrier.

8. The preparation method according to claim 7, characterized in that: Meet one or more of the following conditions: i. In step (a), the stirring speed is 400-600 rpm and the stirring time is 5-10 min; ii. In step (b), the stirring speed is 100-200 rpm and the stirring time is 5-10 min; iii. In step (c), the stirring speed is 400-600 rpm and the stirring time is 20-30 min; iv. In step (d), the stirring speed is 400-600 rpm and the stirring time is 60-120 min; v. In step (e), a preservative is added after the ultrasonic treatment is completed.

9. Use of the essential oil nano delivery carrier based on wild soybean extract as claimed in claim 1 as a fragrance or moisturizing and repairing active ingredient in the preparation of skin care products, wherein the essential oil nano delivery carrier has the effects of moisturizing, repairing the barrier, skin-friendly penetration and sustained release of fragrance, and in terms of repair, the wild soybean extract and the essential oil have a synergistic effect.

10. Use of the essential oil nano delivery carrier based on wild soybean extract according to claim 1 in the preparation of transparent aqueous cosmetics.

Images