Compound massage essential oil for warming uterus and preparation method thereof
By nano-encapsulating rose essential oil and supercritical CO2 extraction of angelica volatile oil, combined with high-pressure homogenization technology, the problems of low stability and low bioavailability of active ingredients in compound massage essential oils have been solved, achieving a highly effective warming and uterine care effect.
Patent Information
- Application Number
- CN202511176718.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-21
- Publication Date
- 2026-01-06
AI Technical Summary
Existing compound massage oils suffer from poor stability of active ingredients, low bioavailability, and insufficient synergistic effects, resulting in limited warming effects on the uterus.
Rose essential oil is encapsulated using nano-encapsulation technology, and angelica volatile oil and ferulic acid are extracted using supercritical CO2 extraction technology. By optimizing the component ratio and high-pressure homogenization process, a multi-dimensional synergistic effect is formed to ensure uniform dispersion and penetration of the components.
It significantly improves the stability and bioavailability of the compound massage oil, achieving an effective warming effect on the uterus, relieving menstrual discomfort, promoting pelvic blood circulation, and providing a safe and gentle care experience.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of natural plant essential oil technology, specifically to a compound massage essential oil for warming the uterus and its preparation method. Background Technology
[0002] In traditional feminine hygiene, massage oils, with their aromatic and soothing properties and localized penetration from natural plant ingredients, are often used to relieve menstrual discomfort and promote pelvic blood circulation, addressing needs such as warming the uterus. Commercially available products are mostly single or simple blends of essential oils, using the natural aromas of plants like lavender and rose to regulate mood, combined with carrier oils (such as sweet almond oil) to reduce skin irritation. However, these products rely heavily on the physical effects of single ingredients, making them less adaptable to complex physiological environments. Furthermore, the active ingredients (such as volatile components in rose essential oil and ferulic acid in angelica) are easily degraded by light and oxygen, leading to unstable efficacy and difficulty in meeting long-term care needs.
[0003] Further analysis of existing technological limitations reveals that while some compound essential oils attempt to add plant extracts (such as angelica and ginger root) to enhance their conditioning effects, two prominent problems exist: First, the bioavailability of active ingredients is low. For example, ferulic acid in angelica is highly polar and poorly lipid-soluble, making it difficult to dissolve directly in the essential oil matrix and affecting its transdermal absorption. Terpenes in rose essential oil are prone to oxidation and deterioration, which not only reduces the aroma quality but may also produce irritating byproducts. Second, the formulation design does not fully optimize the synergistic effect between ingredients. Each raw material is simply mixed as an independent functional unit, failing to form a progressive conditioning mechanism of "promoting penetration - releasing activity - sustained effect," resulting in limited overall warming effect on the uterus and difficulty in meeting the differentiated needs of users with different constitutions.
[0004] Based on this, this invention proposes a compound massage essential oil and its preparation method. Rose essential oil is encapsulated within a β-cyclodextrin cavity using nano-encapsulation technology, significantly improving its stability and sustained-release capacity. Supercritical CO2 extraction technology is employed to simultaneously extract volatile oil and ferulic acid from Angelica sinensis, preserving the integrity and high bioavailability of the active ingredients. Furthermore, it innovatively blends soothing essential oils such as Australian sandalwood and Somali frankincense with warming essential oils such as Indian ginger root oil and Vietnamese cinnamon oil, combined with the gentle base of food-grade sweet almond oil, forming a multi-dimensional synergistic uterine warming system. Simultaneously, the preparation process parameters (such as ultrasonic dispersion conditions and freeze-drying parameters) are optimized to ensure uniform dispersion of all components and absence of impurities, ultimately yielding a compound massage essential oil with high stability, good permeability, and strong safety. This oil can effectively improve menstrual discomfort, promote pelvic blood circulation, and meet the needs of modern women for efficient and gentle uterine warming care products. Summary of the Invention
[0005] The purpose of this invention is to provide a compound massage oil for warming the uterus and its preparation method, which solves the problems of poor stability, low bioavailability and insufficient synergy of active ingredients (such as rose essential oil and angelica extract) in existing compound massage oils, resulting in limited warming effect on the uterus.
[0006] The present invention achieves the above objectives through the following technical solutions:
[0007] A compound massage oil, by weight percentage, comprises the following ingredients:
[0008] Australian sandalwood essential oil: 2-5%;
[0009] Somali frankincense essential oil: 3-8%;
[0010] Modified rose essential oil nano-inclusion complex: 5-10%;
[0011] Indian ginger root oil: 2-4%;
[0012] Vietnamese cinnamon oil: 1-3%;
[0013] Angelica sinensis extract: 3-7%;
[0014] α-Tocopherol: 0.5-1.5%;
[0015] Food-grade sweet almond oil: Balance;
[0016] The preparation method of the rose essential oil nano-inclusion complex includes: adding β-cyclodextrin to deionized water, heating to 60°C and stirring to dissolve, and cooling to room temperature for later use; mixing rose essential oil with anhydrous ethanol and ultrasonically dispersing; adding the rose essential oil ethanol solution dropwise to the β-cyclodextrin aqueous solution while magnetically stirring, and reacting at 40°C until the inclusion rate reaches more than 90% as monitored by fluorescence spectroscopy; transferring the reaction solution to a dialysis bag, dialyzing in deionized water to remove unincluded essential oil and ethanol; and freeze-drying the dialysate.
[0017] According to a preferred embodiment of the present invention, the Australian sandalwood essential oil was purchased from Guangzhou Keran Trading Co., Ltd.
[0018] According to a preferred embodiment of the present invention, the Somali frankincense essential oil was purchased from Dongguan Dongfangyang Biotechnology Co., Ltd.
[0019] According to a preferred embodiment of the present invention, the β-cyclodextrin was purchased from Shaanxi Haoyun Pharmaceutical Technology Co., Ltd.
[0020] According to a preferred embodiment of the invention, the rose essential oil was purchased from Oshadhio.
[0021] According to a preferred embodiment of the present invention, the anhydrous ethanol was purchased from Jinan Century Tongda Chemical Co., Ltd.
[0022] According to a preferred embodiment of the present invention, the dialysis bag was purchased from Shanghai Hanhong Technology Co., Ltd.
[0023] According to a preferred embodiment of the present invention, the Indian ginger root oil was purchased from Guangzhou Hongli Biotechnology Co., Ltd.
[0024] According to a preferred embodiment of the present invention, the Vietnamese cinnamon oil was purchased from Bestman Biotechnology Co., Ltd. in Ji'an City.
[0025] According to a preferred embodiment of the present invention, the α-tocopherol was purchased from Zhengzhou Best Food Additives Co., Ltd.
[0026] According to a preferred embodiment of the present invention, the food-grade sweet almond oil was purchased from Shenzhen Antai Biotechnology Co., Ltd.
[0027] The reaction mechanism of each component in this invention is based on a multi-dimensional physicochemical interaction and synergistic mechanism, specifically as follows: In the preparation of the modified rose essential oil nano-inclusion complex, β-cyclodextrin is dissolved in deionized water at 60℃ to form a homogeneous colloidal solution. Due to hydrophobicity, its molecular cavity can spontaneously include rose essential oil (containing hydrophobic components such as terpenes and linalool) through van der Waals forces and hydrophobic interactions; ultrasonic dispersion (40kHz, 10min) promotes uniform contact between rose essential oil and β-cyclodextrin molecules through cavitation effect, accelerating the inclusion reaction; magnetic stirring (800rpm) further enhances molecular collisions, allowing the inclusion reaction to proceed more rapidly. The reaction was continued at 40℃ until fluorescence spectroscopy showed an inclusion rate of over 90% (indicating that most of the rose essential oil was encapsulated within the β-cyclodextrin cavity). The reaction solution was then transferred to a dialysis bag with a molecular weight cutoff of 10 kDa. Unencapsulated small molecule essential oils and ethanol (molecular weight less than 10 kDa) were separated using a semi-permeable membrane. The solution was dialyzed with deionized water for 24 hours to thoroughly remove impurities. The dialysate was then freeze-dried at -50℃ (vacuum degree 10 Pa, sublimation drying for 24 hours). The stable structure of the β-cyclodextrin inclusion complex was preserved through low-temperature freeze-drying, ultimately forming nano-inclusion complexes with a particle size of 50-100 nm, which significantly improved the stability and sustained-release capacity of the rose essential oil.
[0028] According to a preferred embodiment of the present invention, the ultrasonic dispersion frequency is 40 kHz and the time is 10 min; the dropping rate of the rose essential oil ethanol solution is 1 mL / min; the magnetic stirring speed is 800 rpm; the reaction time at 40°C is 2 h; the molecular weight cutoff of the dialysis bag is 10 kDa; the dialysis time in deionized water is 24 h; the freeze-drying temperature of the dialysis solution is -50°C, the freezing time is 2 h, the vacuum degree is 10 Pa, and the sublimation drying time is 24 h; the particle size of the rose essential oil nanocomplex is 50-100 nm.
[0029] According to a preferred embodiment of the present invention, the Angelica extract comprises volatile oil and ferulic acid.
[0030] According to a preferred embodiment of the present invention, the preparation steps of the Angelica sinensis extract include: taking dried Angelica sinensis root, crushing it with a pulverizer, placing it in the extraction vessel of a supercritical CO2 extraction device, sealing it, and introducing high-pressure CO2. The extraction pressure is set to 30 MPa and the temperature to 45°C. At the same time, an ethanol aqueous solution is injected as an entrainer through an entrainer pump to maintain the above parameters for continuous extraction. After extraction, the mixed fluid is introduced into a separation vessel, and CO2 is volatilized by depressurization and heating. The mixed extract containing volatile oil and ferulic acid is collected. The extract is filtered through an organic filter membrane to remove impurities, and then residual ethanol is recovered by vacuum distillation using a rotary evaporator.
[0031] According to a preferred embodiment of the present invention, the Angelica sinensis root was purchased from Shanghai Yubo Biotechnology Co., Ltd.
[0032] According to a preferred embodiment of the present invention, the pulverizer was purchased from Changzhou Xiaochang Drying Equipment Co., Ltd.
[0033] According to a preferred embodiment of the present invention, the supercritical CO2 extraction device was purchased from Nantong Duxin New Energy Technology Co., Ltd.
[0034] According to a preferred embodiment of the present invention, the separation vessel was purchased from Weihai Huixin Chemical Machinery Co., Ltd.
[0035] According to a preferred embodiment of the present invention, the rotary evaporator was purchased from Zhengzhou Keda Machinery Instrument Equipment Co., Ltd.
[0036] In this invention, the preparation of Angelica sinensis extract relies on supercritical CO2 extraction technology: high-pressure CO2 (30MPa, 45℃) can penetrate the cell wall of Angelica sinensis due to its high permeability and low surface tension, destroying its dense structure and promoting the dissolution of volatile oils (such as α-pinene) and fat-soluble ferulic acid; an ethanol-water solution (volume to raw material ratio 1:5, injection rate 0.5mL / min) acts as an entrainer to increase the polarity of the system and improve the solubility of polar components such as ferulic acid; after continuous extraction for 2 hours, the mixed fluid enters the separation vessel, and CO2 is volatilized into gas and escaped by depressurization (from 30MPa to 8MPa) and heating (from 45℃ to 35℃), retaining the mixed extract of volatile oil and ferulic acid; the extract is filtered through a 0.45μm organic filter membrane to remove plant residues and other impurities, and then residual ethanol is recovered by rotary evaporator (-0.09MPa, 40℃ vacuum distillation), finally obtaining high-purity Angelica sinensis extract (containing volatile oil and ferulic acid).
[0037] According to a preferred embodiment of the present invention, the dried Angelica sinensis root is pulverized to a particle size of 40-60 mesh; the flow rate of the high-pressure CO2 is 20 L / h; the injection rate of the ethanol-water solution is 0.5 mL / min; the mass ratio of the ethanol-water solution to the raw material is 1:5; the continuous extraction time is 2 h; the primary separation pressure in the separation vessel is 8 MPa and the temperature is 35 °C, and the secondary separation pressure is 5 MPa and the temperature is 25 °C; the filtration pore size of the organic filter membrane is 0.45 μm; and the vacuum degree of the rotary evaporator is -0.09 MPa and the temperature is 40 °C.
[0038] This invention also provides a method for preparing the compound massage oil, comprising the following steps:
[0039] S1. Pre-treatment of each raw material: Australian sandalwood essential oil, Somali frankincense essential oil, ginger root oil, and cinnamon oil were filtered to remove impurities after the main component content was confirmed by GC-MS detection; Angelica extract was extracted by supercritical CO2 extraction to obtain a complex of volatile oil and ferulic acid, which was then dried at low temperature, pulverized, and sieved.
[0040] S2. Add food-grade sweet almond oil to the reactor, heat in a water bath to 40°C and stir until homogeneous; add Australian sandalwood essential oil, Somali frankincense essential oil, ginger root oil and cinnamon oil in sequence, and stir at low speed to form an oil phase mixture; add angelica extract and continue stirring; add modified rose essential oil nano-inclusion complex and ultrasonically disperse until homogeneous; finally add α-tocopherol and stir.
[0041] S3. Pass the mixture through a high-pressure homogenizer; after cooling to 25°C, filter it through a microporous membrane for sterilization.
[0042] In the preparation of the compound massage oil in this invention, food-grade sweet almond oil serves as a fat-soluble base, and its gentle skin-friendly and extensible properties provide stable support for the system. Monoterpenes and sesquiterpenes in Australian sandalwood and Somali frankincense essential oils relax pelvic smooth muscles through volatilization and penetration. The warming components (such as gingerol and cinnamaldehyde) in Indian ginger root oil and Vietnamese cinnamon oil promote local vasodilation and accelerate blood circulation by activating skin temperature receptors. Modified rose essential oil nano-encapsulation compounds, due to the sustained-release properties of β-cyclodextrin, continuously release linalool and citronellol from rose essential oil, exerting anti-inflammatory and soothing effects. Volatile oils (such as α-pinene) in angelica extract further reduce skin stratum corneum resistance and promote transdermal penetration of active ingredients, while ferulic acid inhibits prostatitis. Adenosine synthesis reduces pain; α-tocopherol, as a strong antioxidant, provides hydrogen atoms to capture free radicals, preventing the oxidative degradation of active ingredients such as rose essential oil and ferulic acid; each component is stirred at low speed (300 rpm, 10 min) in step S2 to form a preliminary oil phase mixture, then Angelica extract is added and stirring is continued (5 min) to achieve uniform dispersion, then nano-inclusion complex is added and ultrasonically dispersed (40 kHz) until no agglomerated particles are present, and finally α-tocopherol is added and stirred (10 min) to complete the system stabilization; step S3 high-pressure homogenization (5 MPa, 3 cycles) refines particles through shear force, making the distribution of each component more uniform and improving product stability; after cooling to 25℃, it is filtered through a 0.22 μm microporous membrane for sterilization to ensure the product is sterile and safe.
[0043] According to a preferred embodiment of the present invention, in step S1, the supercritical CO2 extraction pressure is 30 MPa, the temperature is 45°C, and the time is 2 h; the low-temperature drying temperature is ≤40°C; and the sample is passed through an 80-mesh sieve.
[0044] According to a preferred embodiment of the present invention, in step S2, the low-speed stirring speed is 300 rpm for 10 min; the stirring time is 5 min; the ultrasonic dispersion frequency is 40 kHz; and the stirring time after adding α-tocopherol is 10 min.
[0045] According to a preferred embodiment of the present invention, in step S3, the pressure in the high-pressure homogenizer is 5 MPa, and the number of cycles is 3.
[0046] The present invention also provides an application of the compound massage oil described above or the compound massage oil prepared by the preparation method described above in warming the uterus.
[0047] When the massage oil prepared by this invention is used, the mechanical force during the massage promotes the even application of the compound essential oil to the lower abdomen. The skin-friendly nature of sweet almond oil allows it to quickly penetrate to the skin surface. After the active ingredients in the nano-encapsulated sustained-release rose essential oil and angelica extract are absorbed through the skin, they work synergistically in the pelvic area: the anti-inflammatory components of rose essential oil relieve local inflammatory reactions, the blood-activating components of angelica extract promote uterine blood circulation, the warming components of ginger root oil and cinnamon oil increase the local metabolic rate, and α-tocopherol continuously protects the active ingredients from oxidation, ultimately achieving the effects of soothing muscles, promoting circulation, and regulating menstruation by warming the uterus.
[0048] The beneficial effects of this invention are as follows:
[0049] This invention significantly improves the overall performance of compound massage oil in uterine warming care through innovative ingredient design and process optimization. Addressing the issues of easy oxidation and deterioration of rose essential oil and low bioavailability of angelica extract in traditional products, this invention employs nano-encapsulation technology to encapsulate rose essential oil within a β-cyclodextrin cavity, effectively isolating it from oxygen and light, reducing evaporation loss, and simultaneously delaying oxidation reactions, thus enhancing the stability of active ingredients. The angelica extract is extracted using supercritical CO2 extraction technology to simultaneously retain volatile oils and ferulic acid, avoiding the residual risks of traditional solvent extraction. Furthermore, the high permeability under supercritical conditions allows for the full dissolution of fat-soluble components such as ferulic acid, significantly improving bioavailability compared to conventional extraction methods, laying the foundation for its subsequent conditioning effects.
[0050] The synergistic design of the formula further enhances the warming effect on the uterus. Essential oils such as Australian sandalwood and Somali frankincense possess natural soothing properties, relaxing pelvic floor muscles; warming ingredients like Indian ginger root oil and Vietnamese cinnamon oil promote local blood circulation and improve metabolic efficiency; the volatile oils and ferulic acid in angelica extract work synergistically to invigorate blood and regulate menstruation, combining with the gentle moisturizing properties of the base sweet almond oil to form a progressive mechanism of action: soothing, penetrating, and conditioning. All ingredients are uniformly blended through ultrasonic dispersion and high-pressure homogenization, leaving no impurities and ensuring rapid penetration into the deep layers of the skin after application, avoiding the local irritation or efficacy fluctuations caused by uneven dispersion of ingredients in traditional compound essential oils.
[0051] In practical applications, this compound massage oil demonstrates excellent warming effects on the uterus. Its stable active ingredients and optimized penetration effectively relieve menstrual cramps, distension, and other discomforts, promote pelvic blood circulation, and improve local nutrient supply. The synergistic effect of natural plant ingredients also regulates endocrine function and enhances the uterus's nutrient absorption and metabolic capacity. Furthermore, the formula contains no irritating chemical additives, and the addition of α-tocopherol further enhances its antioxidant capacity, reduces the risk of allergies, and long-term use can maintain the health of the pelvic area, providing users with a safe, gentle, and highly effective warming care experience. Detailed Implementation
[0052] The following detailed embodiments are only used to further illustrate this application and should not be construed as limiting the scope of protection of this application. Those skilled in the art can make some non-essential improvements and adjustments to this application based on the above application content.
[0053] I. Implementation Examples
[0054] Example 1
[0055] Weigh the following ingredients by weight: 3g Australian sandalwood essential oil, 5g Somali frankincense essential oil, 7g modified rose essential oil nano-inclusion complex, 3g Indian ginger root oil, 2g Vietnamese cinnamon oil, 5g Angelica extract, 1g α-tocopherol, and 64g food-grade sweet almond oil. The preparation method of the modified rose essential oil nano-inclusion complex is as follows: β-cyclodextrin is added to deionized water, heated to 60℃ and stirred to dissolve, and then cooled to room temperature for later use; rose essential oil and anhydrous ethanol are mixed at a mass ratio of 1:5 and ultrasonically dispersed (frequency 40kHz, time 10min); the rose essential oil ethanol solution is added dropwise to the β-cyclodextrin aqueous solution at a dropping rate of 1mL / min (β-cyclodextrin to rose essential oil mass ratio is 9:1), and the mixture is magnetically stirred (speed 800rpm) at 40℃ until the inclusion rate monitored by fluorescence spectroscopy reaches more than 90%; the reaction solution is transferred to a dialysis bag with a molecular weight cutoff of 10kDa, dialyzed in deionized water for 24h, and the dialysate is freeze-dried at -50℃ (freezing time 2h, vacuum degree 10Pa, sublimation drying time 24h) to obtain modified rose essential oil nano-inclusion complex with a particle size of 50-100nm. The preparation steps of Angelica sinensis extract are as follows: Dried Angelica sinensis root is crushed into 40-60 mesh particles and placed in the extraction vessel of a supercritical CO2 extraction device. After sealing, high-pressure CO2 is introduced (pressure 30MPa, temperature 45℃, flow rate 20L / h). At the same time, an ethanol aqueous solution (volume to raw material mass ratio 1:5, injection rate 0.5mL / min) is injected as an entrainer through an entrainer pump. The parameters are maintained for continuous extraction for 2 hours. After extraction, the mixed fluid is introduced into a separation vessel. The first separation pressure is 8MPa and temperature is 35℃, and the second separation pressure is 5MPa and temperature is 25℃. CO2 is volatilized by depressurization and heating. The mixed extract containing volatile oil and ferulic acid is collected. The extract is filtered through a 0.45μm organic filter membrane to remove impurities. Then, the residual ethanol is recovered by vacuum distillation through a rotary evaporator (vacuum degree -0.09MPa, temperature 40℃) to obtain Angelica sinensis extract. The preparation method of the compound massage essential oil is as follows: S1. Pretreatment of each raw material: Australian sandalwood essential oil, Somali frankincense essential oil, ginger root oil, and cinnamon oil are filtered to remove impurities after the main component content is confirmed by GC-MS detection; Angelica extract is extracted by supercritical CO2 to obtain a complex of volatile oil and ferulic acid, dried at low temperature (≤40℃) and then pulverized through an 80-mesh sieve; S2. Food-grade sweet almond oil is added to the reaction vessel, heated to 40℃ in a water bath and stirred evenly; Australian sandalwood essential oil and Somali frankincense essential oil are added in sequence. Oil, ginger root oil, and cinnamon oil were stirred at low speed (300 rpm) for 10 minutes to form an oil phase mixture; Angelica extract was added and stirring was continued for 5 minutes; modified rose essential oil nano-inclusion complex was added and ultrasonically dispersed (frequency 40 kHz) for 10 minutes until homogeneous; finally, α-tocopherol was added and stirred for 10 minutes; S3, the mixture was passed through a high-pressure homogenizer (pressure 5 MPa, 3 cycles); after cooling to 25℃, it was filtered through a 0.22 μm microporous membrane for sterilization to obtain the compound massage essential oil.
[0056] Example 2
[0057] Weigh the following raw materials by weight: 2g Australian sandalwood essential oil, 3g Somali frankincense essential oil, 5g modified rose essential oil nano-inclusion complex, 2g Indian ginger root oil, 1g Vietnamese cinnamon oil, 3g Angelica extract, 0.5g α-tocopherol, and 83.5g food-grade sweet almond oil. The preparation method of the modified rose essential oil nano-inclusion complex is the same as in Example 1, except that the inclusion amount of β-cyclodextrin and rose essential oil is adjusted to 5% (total raw materials). The preparation steps of the Angelica extract are the same as in Example 1. In the preparation method of the compound massage essential oil, the low-speed stirring speed in step S2 is 300 rpm for 10 min; stirring continues for 5 min; ultrasonic dispersion frequency is 40 kHz for 10 min; stirring is performed for 10 min after adding α-tocopherol; high-pressure homogenization in step S3 is performed at a pressure of 5 MPa for 3 cycles, with the remaining parameters the same as in Example 1.
[0058] Example 3
[0059] Weigh the following raw materials by weight: 5g Australian sandalwood essential oil, 8g Somali frankincense essential oil, 10g modified rose essential oil nano-inclusion complex, 4g Indian ginger root oil, 3g Vietnamese cinnamon oil, 7g Angelica extract, 1.5g α-tocopherol, and 61.5g food-grade sweet almond oil. The preparation method of the modified rose essential oil nano-inclusion complex is the same as in Example 1, only the inclusion amount is adjusted to 10%. In the preparation step of the Angelica extract, the injection rate of the supercritical CO2 extraction ethanol-water solution is adjusted to 0.5mL / min, and the ratio of the amount used to the raw material mass is 1:5; the remaining parameters are the same as in Example 1. In the preparation method of the compound massage essential oil, the low-speed stirring time in step S2 is extended to 15min (the rotation speed remains at 300rpm), and the ultrasonic dispersion time is extended to 15min; the remaining parameters are the same as in Example 1.
[0060] Comparative Example 1
[0061] Weigh the following raw materials by weight: 3g Australian sandalwood essential oil, 5g Somali frankincense essential oil, 7g common rose essential oil (without nano-encapsulation), 3g Indian ginger root oil, 2g Vietnamese cinnamon oil, 5g Angelica extract, 1g α-tocopherol, and 74g food-grade sweet almond oil. The Angelica extract was extracted with ethanol (ethanol to raw material mass ratio 3:1, reflux extraction for 2 hours), and the remaining steps were the same as in Example 1.
[0062] Comparative Example 2
[0063] Weigh the following raw materials by weight: 3g Australian sandalwood essential oil, 5g Somali frankincense essential oil, 7g modified rose essential oil nano-inclusion complex, 3g Indian ginger root oil, 2g Vietnamese cinnamon oil, 5g Angelica extract, 1g α-tocopherol, and 74g food-grade sweet almond oil. The Angelica extract was extracted using conventional CO2 extraction (non-supercritical, 1MPa pressure), and the remaining steps were the same as in Example 1.
[0064] Comparative Example 3
[0065] Weigh the following ingredients by weight: 3g Australian sandalwood essential oil, 5g Somali frankincense essential oil, 7g modified rose essential oil nano-inclusion complex, 3g Indian ginger root oil, 2g Vietnamese cinnamon oil, 5g Angelica extract, 1g α-tocopherol, and 74g food-grade sweet almond oil. In the preparation method of the compound massage essential oil, the high-pressure homogenization step is omitted; the mixture is only mechanically stirred until homogeneous. The remaining steps are the same as in Example 1.
[0066] II. Performance Testing
[0067] The materials prepared in Examples 1-3 and Comparative Examples 1-3 were subjected to performance testing according to the following methods:
[0068] 1. Stability test (inclusion rate and volatility of rose essential oil):
[0069] Inclusion rate determination: Take 1g of the modified rose essential oil nano-inclusion complex from the examples / comparative series, add 10mL of deionized water, sonicate (40kHz, 10min), centrifuge (8000rpm, 10min), take the supernatant and use a fluorescence spectrometer (excitation wavelength 280nm, emission wavelength 330nm) to detect the fluorescence intensity of the unincluded rose essential oil, and calculate the inclusion rate by comparing with the standard (inclusion rate = (initial rose essential oil amount - unincluded amount) / initial rose essential oil amount × 100%).
[0070] Volatility determination: Take 10 mL of compound massage essential oil sample and place it in a sealed container. Keep it at 40℃ for 7 days. Detect the residual amount of characteristic components (citronellol and geraniol) of rose essential oil by gas chromatography-mass spectrometry (GC-MS) and calculate the volatility (Volatile rate = (Initial content - Residual amount after 7 days) / Initial content × 100%).
[0071] 2. Transdermal permeability test (Angelica extract and rose essential oil):
[0072] A Franz diffusion cell (effective diffusion area 3.14 cm²) was used. 2A rat abdominal skin (hairless and treated as a barrier model) was fixed in the tank with the stratum corneum facing upwards. 500 μL of compound massage essential oil sample was added to the donor tank, and phosphate buffer (pH = 7.4) was added to the receiver tank. The tank was maintained at 37℃ with magnetic stirring (500 rpm) to maintain the leakage conditions. At 0.5 h, 1 h, 2 h, 4 h, 6 h, 8 h, and 12 h, 500 μL of the receiving solution was collected (with an equal amount of buffer added). The peak areas of Angelica sinensis volatile oil (α-pinene) and rose essential oil (citronellol) were detected by high-performance liquid chromatography (HPLC, C18 column, mobile phase methanol:water = 70:30, flow rate 1 mL / min, detection wavelength 270 nm). The cumulative permeation was calculated (Q = (C × V) / A, where C is the concentration of the component in the receiving solution, V is the volume of the receiver tank, and A is the diffusion area).
[0073] 3. Evaluation of the warming effect on the uterus (human volunteer test):
[0074] Twenty healthy female volunteers (aged 25-35, with regular menstrual cycles and no gynecological diseases) were recruited and randomly divided into four groups (Example Groups 1-3 and Control Groups 1-3, with 5 participants in each group). On days 1-3 of their menstrual cycle, after cleaning their abdomen, volunteers applied 5g of the sample evenly to their lower abdomen (within 3cm below the navel) and gently massaged for 10 minutes, twice daily. Abdominal skin temperature changes (ΔT = T - T0) were recorded using an infrared thermal imager at times before application (T0), 30 minutes after application (T30), 1 hour after application (T1h), and 2 hours after application (T2h). Simultaneously, menstrual discomfort was recorded using the Visual Analogue Scale (VAS) (0 points for no discomfort, 10 points for severe pain), and the average relief rate was calculated (Relief rate = (Initial VAS score - VAS score after 30 minutes) / Initial VAS score × 100%).
[0075] 4. Bioavailability test (ferulic acid skin accumulation):
[0076] Abdominal skin (epidermal layer removed) was collected from volunteers 2 hours after the sample was applied. After homogenization, methanol (1:10 w / v) was added and ultrasonically extracted for 30 min (40 kHz). The mixture was centrifuged (12000 rpm, 10 min), and the supernatant was collected. After filtration through a 0.45 μm filter membrane, the mixture was detected by HPLC (C18 column, mobile phase acetonitrile:0.1% formic acid water = 30:70, flow rate 1 mL / min, detection wavelength 320 nm). The concentration of ferulic acid in the skin homogenate (μg / g skin) was calculated.
[0077] 5. Sensory evaluation (appearance and odor):
[0078] Ten professional fragrance evaluators conducted blind tests on the samples. Evaluation criteria included: appearance (clarity, presence of layering) and aroma (purity and irritation of natural plant fragrance). Scoring criteria: 1-5 points (1 = poor, 5 = excellent), with the average value taken.
[0079] 6. Performance test results:
[0080] Table 1: Performance test results of each embodiment and comparative example
[0081]
[0082]
[0083] As can be seen from Table 1, Examples 1-3 of this invention effectively solve the problems of poor stability, low bioavailability, and insufficient synergistic effects of active ingredients in existing compound massage oils through technological innovation. Regarding stability, Examples 1-3 employ nano-encapsulation technology to encapsulate rose essential oil within the cavity of β-cyclodextrin, significantly reducing its volatility (8.2%-8.8% volatility after 7 days vs. 22.1% in Comparative Example 1), while achieving an encapsulation rate as high as 90.8%-92.3% (compared to only 78.6% in Comparative Example 1). This effectively reduces the loss of active ingredients due to oxidation or light exposure, improving long-term storage stability. Regarding bioavailability, Examples 1-3 simultaneously obtained Angelica sinensis volatile oil and ferulic acid using supercritical CO2 extraction technology, avoiding the residual risks associated with traditional solvent extraction. Furthermore, the high permeability under supercritical conditions ensured the full dissolution of lipid-soluble components such as ferulic acid. Combined with the optimized use of an ethanol-water entrainer in the Angelica sinensis extract (dosage to raw material ratio 1:5, injection rate 0.5 mL / min), the dissolution and transdermal absorption of active ingredients were further promoted. The cumulative permeation of Angelica sinensis volatile oil over 12 hours was 11.8-13.2 μg / cm³. 2 ) and the penetration of rose essential oil (9.1-10.3 μg / cm) 2 All were significantly higher than those in control group 1 (5.2 μg / cm). 2 3.5 μg / cm 2The amount of ferulic acid accumulated in the skin (3.8-4.5 μg / g) was also significantly higher than that in control group 1 (1.9 μg / g), indicating that the transdermal absorption efficiency of the active ingredient was greatly improved. Regarding synergistic effects of the ingredients, Examples 1-3 achieved a progressive mechanism of action by precisely controlling the proportions of each raw material (such as the blending of soothing essential oils like Australian sandalwood and Somali frankincense with warming essential oils like Indian ginger root oil and Vietnamese cinnamon oil), combined with a high-pressure homogenization process (5 MPa pressure, 3 cycles) to ensure uniform dispersion of each ingredient without any impurities. In contrast, Comparative List 1 failed to achieve efficient synergy between ingredients due to the lack of nano-encapsulation, resulting in easy volatility of rose essential oil; Comparative List 2 suffered from insufficient dissolution of angelica active ingredients due to low efficiency of ordinary CO2 extraction; and Comparative List 3 resulted in uneven dispersion of ingredients due to the omission of high-pressure homogenization. Ultimately, the increase in abdominal temperature (ΔT only 0.9℃) and the relief rate of menstrual discomfort (45.6%) were significantly lower than those in Examples 1-3 (ΔT 1.6-1.9℃, relief rate 72.3%-81.2%). In summary, Examples 1-3 systematically solved the problems of poor stability, low bioavailability, and insufficient synergy of active ingredients through nano-encapsulation, supercritical extraction, and process optimization, significantly improving the warming effect of the compound massage oil on the uterus.
[0084] The embodiments described above are merely examples of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention.
Claims
1. A compound massage essential oil, characterized by, By mass percentage, raw materials include: Australian sandalwood essential oil: 2-5%; Somali frankincense essential oil: 3-8%; Modified rose essential oil nanoinclusion: 5-10%; Indian ginger oil: 2-4%; Vietnamese cinnamon oil: 1-3%; Angelica extract: 3-7%; Alpha-tocopherol: 0.5-1.5%; Food-grade sweet almond oil: the rest; The preparation method of the rose essential oil nanoinclusion includes: adding β-cyclodextrin into deionized water, heating to 60 DEG C and stirring to dissolve, cooling to room temperature for standby; taking rose essential oil and mixing with anhydrous ethanol, ultrasonic dispersion; drop the rose essential oil ethanol solution into the β-cyclodextrin aqueous solution, while magnetic stirring, 40 DEG C reaction until the fluorescence spectrum monitoring inclusion rate reaches more than 90% to stop; transfer the reaction solution to a dialysis bag, dialyze in deionized water, remove the un-included essential oil and ethanol; freeze-drying of the dialysate.
2. The compound massage essential oil according to claim 1, characterized in that, The frequency of ultrasonic dispersion is 40 kHz, and the time is 10 min; the drop rate of the rose essential oil ethanol solution is 1 mL / min; the rotating speed of magnetic stirring is 800 rpm; the 40 DEG C reaction time is 2 h; the molecular weight cut-off of the dialysis bag is 10 kDa; the dialysis time in deionized water is 24 h, the freeze-drying temperature of the dialysate is-50 DEG C, the freezing time is 2 h, the vacuum degree is 10 Pa, and the sublimation drying time is 24 h; the particle size of the rose essential oil nanoinclusion is 50-100 nm.
3. The compound massage essential oil according to claim 1, characterized in that, The angelica extract includes volatile oil and ferulic acid.
4. The compound massage essential oil according to claim 1, characterized in that, The preparation steps of the angelica extract include: taking dried angelica root, crushing by a pulverizer, placing in an extraction kettle of a supercritical CO2 extraction device, sealing, and then introducing high-pressure CO2; setting the extraction pressure to 30 MPa and the temperature to 45 DEG C; at the same time, injecting an ethanol aqueous solution as a carrier by a carrier pump; maintaining the above parameters for continuous extraction; after the extraction is completed, introducing the mixed fluid into a separation kettle, and making CO2 volatilize by reducing pressure and increasing temperature; collecting the mixed extraction liquid containing volatile oil and ferulic acid; filtering the extraction liquid through an organic filter membrane to remove impurities, and then reducing pressure and distilling the residual ethanol by a rotary evaporator.
5. The compound massage essential oil according to claim 1, characterized in that, The dried angelica root is crushed to a particle size of 40-60 mesh; the flow rate of high-pressure CO2 is 20 L / h; the injection rate of the ethanol aqueous solution is 0.5 mL / min; the mass ratio of the amount of the ethanol aqueous solution to the raw material is 1:5; the continuous extraction time is 2 h; the first-stage separation pressure in the separation kettle is 8 MPa and the temperature is 35 DEG C; the second-stage separation pressure is 5 MPa and the temperature is 25 DEG C; the filter pore of the organic filter membrane is 0.45 μm; the vacuum degree of the rotary evaporator is-0.09 MPa and the temperature is 40 DEG C.
6. A method of preparing the compound massage oil according to any one of claims 1-5, characterized by the steps of It includes: S1, pretreatment of each raw material: after confirming the main component content by GC-MS detection, filtering the Australian sandalwood essential oil, Somali frankincense essential oil, ginger oil, and cinnamon oil to remove impurities; obtaining the compound of volatile oil and ferulic acid from the angelica extract by supercritical CO2 extraction, drying at low temperature, and then crushing and sieving; S2, add food grade sweet almond oil into the reaction kettle, heated to 40℃ in water bath and stirred evenly; add Australia sandalwood essential oil, Somali frankincense essential oil, ginger oil and cinnamon oil in turn, low speed stirring to form oil phase mixture; add angelica extract and continue stirring; add modified rose essential oil nano inclusion compound, ultrasonic dispersion until uniform; finally add α-tocopherol and stir; S3, pass the mixture through high pressure homogenizer; cool to 25℃ and filter through microporous filter membrane to remove bacteria.
7. The production method according to claim 6, wherein In step S1, the pressure of supercritical CO2 extraction is 30 MPa, the temperature is 45℃, and the time is 2h; the temperature of low temperature drying is ≤40℃; pass through 80 mesh sieve.
8. The preparation method according to claim 6, characterized in that, In step S2, the stirring speed of low speed stirring is 300rpm, and the time is 10min; the time of continuous stirring is 5min; the ultrasonic dispersion frequency is 40kHz; the stirring time after adding α-tocopherol is 10min.
9. The preparation method according to claim 6, characterized in that, In step S3, the pressure in high pressure homogenizer is 5MPa, and the cycle number is 3 times.
10. The use of the compound massage oil according to any one of claims 1 to 5 or the compound massage oil prepared by the method according to any one of claims 6 to 9, characterized in that, The application of the compound massage essential oil in warming uterus.