A natural firming, anti-wrinkle and skin-brightening plant essential oil, its preparation method and application
Through the specific proportion of plant essential oil combination and marine biosterol preparation methods, the problem of existing plant essential oil skin care products in poor anti-wrinkle and brightener effects is solved, and significant anti-wrinkle and brightener effects are achieved, and the safety and permeability of the product are ensured.
Patent Information
- Application Number
- CN202510444617.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-10
- Publication Date
- 2025-07-29
- Estimated Expiration
- 2045-04-10
AI Technical Summary
The existing plant essential oil skin care products have average effects in anti-wrinkle and brightening, and it is necessary to optimize essential oil compositions to improve the effect.
The combination of frankincense oil, sandalwood oil, lavender oil, myrrh oil, Italian chrysanthemum oil, rock rose oil, Turkic rose oil, rock orchid grass root oil and marine biosterol in a specific proportion is used to extract marine biosterols by heating and stirring and chromatography to prepare natural firming, anti-wrinkle and brightening plant essential oil.
It significantly improves the anti-wrinkle and brightening effect, and meets cosmetic safety standards and is highly safe. Marine biosterols enhance the penetration and absorption capacity of essential oils.
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Figure CN119950367B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of skin care product preparation, and specifically relates to a natural firming, anti-wrinkle and brightening plant essential oil, its preparation method and application. Background Art
[0002] Plant essential oils have many advantages in skin care, including enhancing skin penetration, lubricating the skin and maintaining elasticity, promoting metabolism and detoxification, aromatherapy effects and psychological soothing, enhancing skin protection, improving the adhesion of makeup, and having a fresh and natural feeling when used. These advantages make plant essential oils an ideal choice for many people's daily skin care.
[0003] For example, the patent document with the authorized publication number CN115487096B discloses a plant essential oil composition with the effects of removing dark circles, moisturizing and repairing, which has the effects of removing dark circles, moisturizing, repairing and restoring elasticity. Another example is that the patent document with the authorized publication number CN104490704B discloses a plant essential oil skin care product, which has the effects of moisturizing the skin and shrinking pores.
[0004] However, the existing skin care products based on these plant essential oil compositions generally have mediocre effects in anti-wrinkle and brightening when used. Therefore, it is urgent to optimize the formulations of these essential oil compositions. Summary of the Invention
[0005] The purpose of the present invention is to provide a natural firming, anti-wrinkle and brightening plant essential oil, its preparation method and application, so as to enhance its effects in anti-wrinkle and brightening.
[0006] The present invention realizes the above purpose through the following technical solutions:
[0007] A natural firming, anti-wrinkle and brightening plant essential oil, calculated by weight percentage, the raw materials of the plant essential oil include:
[0008] Frankincense oil 30.0 - 40.0%;
[0009] Sandalwood oil 15.0 - 20.0%;
[0010] Lavender oil 10.0 - 15.0%;
[0011] Myrrh oil 8.0 - 12.0%;
[0012] Helichrysum italicum oil 12.0 - 18.0%;
[0013] Cistus ladaniferus oil 0.5 - 1.5%;
[0014] Rosa damascena flower oil 5.0 - 10.0%;
[0015] 0.5 - 1.5% of vetiver root oil;
[0016] 0.1 - 0.5% of marine biological sterol.
[0017] Further improvement lies in that, by weight percentage, the raw materials of the plant essential oil include:
[0018] 35.0% of frankincense oil;
[0019] 17.5% of sandalwood oil;
[0020] 12.5% of lavender oil;
[0021] 10.0% of myrrh oil;
[0022] 15.0% of helichrysum italicum oil;
[0023] 1.0% of cistus ladaniferus oil;
[0024] 8.0% of rosa damascena flower oil;
[0025] 0.98% of vetiver root oil;
[0026] 0.02% of marine biological sterol.
[0027] Further improvement lies in that the marine biological sterol is composed of a mixture of styelasterol and sarcophytol A.
[0028] Further improvement lies in that the weight ratio of styelasterol to sarcophytol A is 1:3.
[0029] The present invention also provides a preparation method of the natural firming, anti - wrinkle and brightening plant essential oil, and the steps include:
[0030] S1. Weigh frankincense oil, sandalwood oil, lavender oil, myrrh oil, helichrysum italicum oil, cistus ladaniferus oil, rosa damascena flower oil and vetiver root oil according to the weight ratio and place them in a container to be mixed until homogeneous to obtain a mixed essential oil;
[0031] S2. Prepare the marine biological sterol;
[0032] S3. Add the marine biological sterol to the mixed essential oil according to the weight ratio and mix evenly again to obtain the product.
[0033] Further improvement lies in that in step S1, the specific operation of mixing until homogeneous is: stirring and mixing at a rate of 150 - 300 r / min for 2 - 4 h under the heating condition of 35 - 40 °C.
[0034] Further improvement lies in that the specific operation of step S2 is:
[0035] S2-1. Take fresh Styela clava, wash, dry in the sun, and crush it into particles with a particle size of ≤0.2 mm. Add the particles to an ethanol solution with a concentration of 90% for extraction. After extraction, filter to obtain the filtrate, and concentrate it under reduced pressure to obtain a primary extract. Then, extract the primary extract with ethyl acetate, and concentrate it under reduced pressure again to obtain a secondary extract. Next, add the secondary extract to a methanol solution with a concentration of 90%, extract it with n-hexane, and concentrate it under reduced pressure to obtain an n-hexane extract. Perform normal-pressure silica gel column chromatography on the n-hexane extract, and perform gradient elution with a chloroform / methanol eluent. The gradient volume ratio changes from 100:0 to 50:50. After monitoring by TLC, combine the same parts, concentrate, and then perform Sephadex LH-20 gel column chromatography. The eluent is methanol:chloroform = 1:1 to obtain two components. Take the colorless needle crystal component, which is Styela clava sterol;
[0036] S2-2. Take fresh Sarcophyton glaucum, wash, dry in the sun, and crush it into particles with a particle size of ≤0.2 mm. Add the particles to an ethanol solution with a concentration of 90% for extraction. After extraction, filter to obtain the filtrate, and concentrate it under reduced pressure to obtain an extract. Partition the extract with ethyl acetate / water, take the ethyl acetate extract, and concentrate it under reduced pressure to obtain an ethyl acetate extract. Then, perform column chromatography on the extract with silica gel H, and perform gradient elution with a petroleum ether / ethyl acetate eluent with gradually increasing polarity. Two components are obtained successively from the eluent with a volume ratio of petroleum ether:ethyl acetate = 20:80. Take the colorless columnar crystal component, which is Sarcophyton glaucum sterol;
[0037] S2-3. Mix the above-mentioned Styela clava sterol and Sarcophyton glaucum sterol evenly according to the weight ratio to obtain marine biological sterol.
[0038] Further improvement lies in that the specific operation of the even mixing is: Stir and mix at a rate of 250-350 r / min for 0.2-1 h under the heating condition of 40-45 °C.
[0039] The present invention also provides an application of the natural firming, anti-wrinkle and brightening plant essential oil in skin care products.
[0040] Further improvement lies in that the skin care product is one of a water-based product, a facial mask, a lotion, a cream or a liquid foundation. Of course, the plant essential oil can also be diluted and used directly.
[0041] The beneficial effects of the present invention are as follows:
[0042] (1) The present invention adopts a unique essential oil formula, making the product outstanding in the comprehensive effect of anti-wrinkle and brightening, without any chemical components, and all meeting the relevant regulations of the "Technical Specifications for Cosmetic Safety", with high safety;
[0043] (2)The present invention adds marine biological sterols made from stigmasterol and sarcosterol in the plant essential oil. It has the effects of antioxidant and moisturizing by itself, and can also enhance the penetration and absorption of the essential oil, thereby further enhancing the anti-wrinkle and skin brightening effects. Description of the Drawings
[0044] Figure 1 It is a graph of the number of wrinkles after using the essential oil samples of each example and comparative example;
[0045] Figure 2 It is a graph of the depth of wrinkles after using the essential oil samples of each example and comparative example;
[0046] Figure 3 It is a graph of the area of wrinkles after using the essential oil samples of each example and comparative example;
[0047] Figure 4 It is a graph of the length of wrinkles after using the essential oil samples of each example and comparative example. Detailed Embodiments
[0048] The following further describes the present application in conjunction with the drawings. It is necessary to point out here that the following detailed embodiments are only used to further illustrate the present application and cannot be understood as limiting the protection scope of the present application. Those skilled in the art can make some non-essential improvements and adjustments to the present application according to the above application content.
[0049] I. Main Instruments and Materials
[0050] Frankincense (BOSWELLIA CARTERII) oil: The main components are α-pinene, limonene, and α-thujene. Frankincense essential oil has the effect of whitening and lightening spots, and can be used in combination with other essential oils, such as mixed with cinnamon and rose essential oils for lightening spots and removing scars.
[0051] Sandalwood (SANTALUM ALBUM) oil: The main components are α- and β-santalene, santene, santanone, α-santalol, and santalol. Sandalwood essential oil can adjust the oil secretion of the skin in skin care and is suitable for oily and dry skin. It is a mild astringent and can help whiten and lighten spots.
[0052] Lavender (LAVANDULA ANGUSTIFOLIA) oil: The main components are linalool, linalyl acetate, borneol, lavandulyl acetate, agarwood alcohol, limonene, caryophyllene, coumarin, and terpinene. Lavender essential oil has a soothing and calming effect, helps fade age spots, and it can whiten and lighten spots by inhibiting the activity of tyrosinase.
[0053] Myrrh (COMMIPHORA MYRRHA) oil: The main components are furanoeudesma-1,3-diene, curzerene, β-cadinene, β-elemene, lindenen, geranyllinalool. Myrrh essential oil can promote blood circulation to remove blood stasis, treat pigmentation in any part, and help whiten the skin and fade spots.
[0054] Helichrysum italicum flower oil: The main components are neryl acetate, α-pinene, γ-curcumene, italidione I, II. Helichrysum italicum flower oil has the functions of antioxidant, promoting collagen production, repairing damaged skin, and soothing sensitive skin.
[0055] Cistus ladaniferus oil: The main components are α-pinene, borneol, bornyl acetate, sabinene, ladaneol, viridiflorol, durenol, limonene. Cistus ladaniferus oil can be used to deeply purify the skin, clean harmful impurities in the skin, such as toxins, pollution and free radicals, so as to make the skin glow, smooth and energetic.
[0056] Rosa damascena flower oil: The main components are citronellol, nerol, linalool, phenethyl alcohol. Rosa damascena flower oil can effectively inhibit the deposition of melanin, decompose melanin to make the skin fair and smooth, and effectively fade freckles and age spots.
[0057] Vetiveria zizanioides root oil: The main components are khusimol, nookatone, β-vetivenyl neryl ether, β-vetivene, α and β-vetivone, vetiverol. Vetiveria zizanioides root oil can help the skin self-repair, moisturize and resist wrinkles, inhibit the activity of tyrosinase, fade spots, brighten the skin, and improve skin relaxation and fine lines.
[0058] Sterol biological sources: Fresh Styela clava: taken from the scallop aquaculture area in the coastal waters of Bohai Sea, Shandong; Sarcophyton crassocaule: taken from the waters of Sanya, Hainan, China.
[0059] Detection instruments: Skin wrinkle analysis system Primos (LMI Technologies Gmbh Canfield, Canada); Visia-CR(Canfield); Image-Pro skin comprehensive analysis software (Media Cybernetics).
[0060] II. Conduct experiments
[0061] Example 1
[0062] A natural firming, anti-wrinkle and skin-brightening plant essential oil. By weight percentage, the raw materials of the plant essential oil include: 30.0 g of frankincense oil; 20.0 g of sandalwood oil; 15.0 g of lavender oil; 12.0 g of myrrh oil; 12.0 g of helichrysum italicum oil; 0.5 g of cistus ladaniferus oil; 9.9 g of rosa damascena flower oil; 0.5 g of vetiver root oil; 0.1 g of marine sterol. Among them, the marine sterol is composed of ascidiasterol and sarcophytol A, and the weight ratio of ascidiasterol to sarcophytol A is 1:3.
[0063] The preparation method of the natural firming, anti-wrinkle and skin-brightening plant essential oil comprises the following steps:
[0064] S1. Weigh frankincense oil, sandalwood oil, lavender oil, myrrh oil, helichrysum italicum oil, cistus ladaniferus oil, rosa damascena flower oil and vetiver root oil according to the weight ratio and place them in a container. Stir and mix them at a rate of 150 r / min for 4 h under the heating condition of 35 °C until the essential oils are mixed into a homogeneous state to obtain a mixed essential oil;
[0065] S2. Prepare marine sterol:
[0066] S2-1. Adopt conventional extraction and separation techniques. Specifically, take fresh ascidia, wash and dry it in the sun, crush it into particles with a particle size ≤ 0.2 mm, add the particles to an ethanol solution with a concentration of 90% for extraction, filter the extract after extraction and concentrate it under reduced pressure to obtain a first extract. Then, extract the first extract with ethyl acetate, and concentrate it under reduced pressure again to obtain a second extract. Then, add the second extract to a methanol solution with a concentration of 90%, extract it with n-hexane, and concentrate it under reduced pressure to obtain an n-hexane extract. Perform normal-pressure silica gel column chromatography on the n-hexane extract, and perform gradient elution with a chloroform / methanol eluent. The gradient volume ratio changes from 100:0 to 50:50. After monitoring by TLC, combine the same parts and concentrate them, and then perform Sephadex LH-20 gel column chromatography. The eluent is methanol:chloroform = 1:1 to obtain two components. Take the colorless needle crystal component among them, which is ascidiasterol;
[0067] S2-2. Adopt conventional extraction and separation techniques. Specifically, take fresh sarcophyton glaucum, wash and dry it in the sun, crush it into particles with a particle size ≤ 0.2 mm, add the particles to an ethanol solution with a concentration of 90% for extraction, filter the extract after extraction and concentrate it under reduced pressure to obtain an extract. Distribute the extract with ethyl acetate / water, take the ethyl acetate extract and concentrate it under reduced pressure to obtain an ethyl acetate extract. Then, perform column chromatography on the extract with silica gel H, and perform gradient elution with a petroleum ether / ethyl acetate eluent with gradually increasing polarity. Two components are successively obtained from the eluent with a volume ratio of petroleum ether:ethyl acetate = 20:80. Take the colorless columnar crystal component among them, which is sarcophytol A;
[0068] S2-3. Mix the stenasterol and sarcophytol evenly according to the weight ratio to obtain marine biological sterols.
[0069] S3. Add the marine biological sterols to the mixed essential oils according to the weight ratio, and stir and mix at a rate of 250 r / min for 1 h under the heating condition of 40 °C to obtain the product.
[0070] Example 2
[0071] A natural firming, anti-wrinkle and brightening plant essential oil. By weight percentage, the raw materials of the plant essential oil include: 35.0 g of frankincense oil, 17.5 g of sandalwood oil, 12.5 g of lavender oil, 10.0 g of myrrh oil, 15.0 g of helichrysum italicum oil, 1.0 g of cistus ladaniferus oil, 8.0 g of rosa damascena flower oil, 0.8 g of vetiver root oil, and 0.2 g of marine biological sterols. Among them, the marine biological sterols are composed of stenasterol and sarcophytol, and the weight ratio of stenasterol to sarcophytol is 1:3.
[0072] The preparation method of the natural firming, anti-wrinkle and brightening plant essential oil comprises the steps of:
[0073] S1. Weigh frankincense oil, sandalwood oil, lavender oil, myrrh oil, helichrysum italicum oil, cistus ladaniferus oil, rosa damascena flower oil and vetiver root oil according to the weight ratio and place them in a container, and stir and mix at a rate of 200 r / min for 3 h under the heating condition of 38 °C until the essential oils are mixed into a homogeneous state to obtain mixed essential oils.
[0074] S2. Prepare marine biological sterols:
[0075] S2-1. Adopt conventional extraction and separation techniques, specifically: take fresh Styela clava, wash and dry it in the sun, crush it into particles with a particle size ≤ 0.2 mm, add the particles to an ethanol solution with a concentration of 90% for extraction, filter the extract after extraction and concentrate it under reduced pressure to obtain a first extract, then extract the first extract with ethyl acetate, and then concentrate it under reduced pressure to obtain a second extract. Then add the second extract to a methanol solution with a concentration of 90%, extract it with n-hexane, and then concentrate it under reduced pressure to obtain an n-hexane extract. Perform normal pressure silica gel column chromatography on the n-hexane extract, and perform gradient elution with a chloroform / methanol eluent, and the gradient volume ratio changes from 100:0 to 50:50. Monitor by TLC, combine the same parts and concentrate them, and then perform Sephadex LH-20 gel column chromatography. The eluent is methanol:chloroform = 1:1 to obtain two components. Take the colorless needle crystal component among them, which is stenasterol.
[0076] S2-2. Adopt conventional extraction and separation techniques, specifically: Take fresh Sarcophyton glaucum, wash and dry it in the sun, crush it into particles with a particle size ≤ 0.2 mm, add the particles to an ethanol solution with a concentration of 90% for extraction, filter the extract after extraction and concentrate it under reduced pressure to obtain an extract, partition the extract with ethyl acetate / water, take the ethyl acetate extract and concentrate it under reduced pressure to obtain an ethyl acetate extract, then perform column chromatography on the extract with silica gel H, and perform gradient elution with a petroleum ether / ethyl acetate eluent with gradually increasing polarity, and obtain two components in sequence from the eluent with a volume ratio of petroleum ether:ethyl acetate = 20:80, take the colorless columnar crystal component, which is Sarcophyton sterol;
[0077] S2-3. Take the styela sterol and Sarcophyton sterol and mix them evenly according to the weight ratio to obtain marine biological sterol;
[0078] S3. According to the weight ratio, add the marine biological sterol to the mixed essential oil, and stir and mix at a rate of 300 r / min under heating conditions at 42 °C for 0.6 h to obtain it.
[0079] Example 3
[0080] A natural firming, anti-wrinkle and brightening plant essential oil. By weight percentage, the raw materials of the plant essential oil include: 40.0 g of frankincense oil; 15.5 g of sandalwood oil; 10.0 g of lavender oil; 8.0 g of myrrh oil; 18.0 g of Helichrysum italicum oil; 1.5 g of Cistus ladaniferus oil; 5.0 g of Rosa damascena oil; 1.5 g of Vetiver root oil; 0.5 g of marine biological sterol. Among them, the marine biological sterol is composed of styela sterol and Sarcophyton sterol, and the weight ratio of styela sterol to Sarcophyton sterol is 1:3.
[0081] The preparation method of the natural firming, anti-wrinkle and brightening plant essential oil comprises the steps of:
[0082] S1. Weigh frankincense oil, sandalwood oil, lavender oil, myrrh oil, Helichrysum italicum oil, Cistus ladaniferus oil, Rosa damascena oil and Vetiver root oil according to the weight ratio and place them in a container, and stir and mix at a rate of 300 r / min under heating conditions at 40 °C for 2 h to make the essential oils mixed into a homogeneous state to obtain a mixed essential oil;
[0083] S2. Prepare marine biological sterol:
[0084] S2-1. Use conventional extraction and separation techniques, specifically: Take fresh Styela clava, wash and dry it in the sun, crush it into particles with a particle size ≤ 0.2 mm, add the particles to an ethanol solution with a concentration of 90% for extraction, filter the extract after extraction, and concentrate it under reduced pressure to obtain a first extract. Then, extract the first extract with ethyl acetate, and concentrate it under reduced pressure to obtain a second extract. Then, add the second extract to a methanol solution with a concentration of 90%, extract it with n-hexane, and concentrate it under reduced pressure to obtain an n-hexane extract. Perform normal pressure silica gel column chromatography on the n-hexane extract, use chloroform / methanol eluent for gradient elution, and the gradient volume ratio changes from 100:0 to 50:50. After monitoring by TLC, combine the same parts and concentrate them, and then perform Sephadex LH-20 gel column chromatography. The eluent is methanol:chloroform = 1:1, and two components are obtained. Take the colorless needle crystal component among them, which is Styela clava sterol;
[0085] S2-2. Use conventional extraction and separation techniques, specifically: Take fresh Sarcophyton glaucum, wash and dry it in the sun, crush it into particles with a particle size ≤ 0.2 mm, add the particles to an ethanol solution with a concentration of 90% for extraction, filter the extract after extraction, and concentrate it under reduced pressure to obtain an extract. Partition the extract with ethyl acetate / water, take the ethyl acetate extract and concentrate it under reduced pressure to obtain an ethyl acetate extract. Then, perform column chromatography on the extract with silica gel H, use petroleum ether / ethyl acetate eluent with gradually increasing polarity for gradient elution, and obtain two components successively from the eluent with a volume ratio of petroleum ether:ethyl acetate = 20:80. Take the colorless columnar crystal component among them, which is Sarcophyton glaucum sterol;
[0086] S2-3. Take the above-mentioned Styela clava sterol and Sarcophyton glaucum sterol, mix them evenly according to the weight ratio, and then the marine biological sterol can be obtained;
[0087] S3. According to the weight ratio, add the marine biological sterol to the mixed essential oil, and stir and mix at a rate of 350 r / min for 0.2 h under the heating condition of 45 °C, then it can be obtained.
[0088] Comparative Example 1
[0089] A natural firming, anti-wrinkle and brightening plant essential oil. By weight percentage, the raw materials of the plant essential oil include: 35.0 g of frankincense oil, 17.5 g of sandalwood oil, 12.5 g of lavender oil, 10.0 g of myrrh oil, 15.0 g of Helichrysum italicum oil, 1.0 g of Cistus ladaniferus oil, 8.0 g of Rosa damascena flower oil, 1.0 g of Vetiver root oil.
[0090] The preparation method of the natural firming, anti-wrinkle and brightening plant essential oil includes the following steps:
[0091] S1. Weigh out frankincense oil, sandalwood oil, lavender oil, myrrh oil, helichrysum italicum oil, cistus ladaniferus oil, rosa damascena flower oil and vetiver root oil according to the weight ratio and place them in a container. Stir and mix at a rate of 200 r / min for 3 h under the heating condition of 38 °C until the essential oils are mixed into a homogeneous state, thus obtaining.
[0092] Comparative Example 2
[0093] A natural firming, anti-wrinkle and brightening plant essential oil. By weight percentage, the raw materials of the plant essential oil include: 35.0 g of frankincense oil, 17.5 g of sandalwood oil, 12.5 g of lavender oil, 10.0 g of myrrh oil, 15.0 g of helichrysum italicum oil, 1.0 g of cistus ladaniferus oil, 8.0 g of rosa damascena flower oil, 0.8 g of vetiver root oil, and 0.2 g of marine biological sterol. Among them, the marine biological sterol is stigmasterol.
[0094] The preparation method of the natural firming, anti-wrinkle and brightening plant essential oil comprises the steps of:
[0095] S1. Weigh out frankincense oil, sandalwood oil, lavender oil, myrrh oil, helichrysum italicum oil, cistus ladaniferus oil, rosa damascena flower oil and vetiver root oil according to the weight ratio and place them in a container. Stir and mix at a rate of 200 r / min for 3 h under the heating condition of 38 °C until the essential oils are mixed into a homogeneous state to obtain a mixed essential oil;
[0096] S2. Prepare the marine biological sterol:
[0097] Adopt conventional extraction and separation techniques, specifically: Take fresh Styela clava, wash and dry it in the sun, crush it into particles with a particle size ≤ 0.2 mm, add the particles to an ethanol solution with a concentration of 90% for extraction, filter the extract after extraction and concentrate it under reduced pressure to obtain a first extract. Then, extract the first extract with ethyl acetate, and concentrate it under reduced pressure to obtain a second extract. Then, add the second extract to a methanol solution with a concentration of 90%, extract it with n-hexane, and concentrate it under reduced pressure to obtain an n-hexane extract. Perform normal pressure silica gel column chromatography on the n-hexane extract, use chloroform / methanol eluent for gradient elution, and the gradient volume ratio changes from 100:0 to 50:50. Monitor by TLC, combine the same parts and concentrate them, and then perform Sephadex LH-20 gel column chromatography. The eluent is methanol:chloroform = 1:1 to obtain two components. Take the colorless needle crystal component, which is stigmasterol;
[0098] S3. According to the weight ratio, add the marine biological sterol to the mixed essential oil, and stir and mix at a rate of 300 r / min for 0.6 h under the heating condition of 42 °C, thus obtaining.
[0099] Comparative Example 3
[0100] A natural firming, anti-wrinkle and skin-brightening plant essential oil. By weight percentage, the raw materials of the plant essential oil include: 35.0 g of frankincense oil, 17.5 g of sandalwood oil, 12.5 g of lavender oil, 10.0 g of myrrh oil, 15.0 g of helichrysum italicum oil, 1.0 g of cistus ladaniferus oil, 8.0 g of rosa damascena flower oil, 0.8 g of vetiver root oil, and 0.2 g of marine sterol. Among them, the marine sterol is sarcophytol A.
[0101] The preparation method of the natural firming, anti-wrinkle and skin-brightening plant essential oil comprises the following steps:
[0102] S1. Weigh frankincense oil, sandalwood oil, lavender oil, myrrh oil, helichrysum italicum oil, cistus ladaniferus oil, rosa damascena flower oil and vetiver root oil according to the weight ratio and place them in a container. Stir and mix at a rate of 200 r / min for 3 h under the heating condition of 38 °C until the essential oils are mixed into a homogeneous state to obtain a mixed essential oil;
[0103] S2. Extract marine sterol:
[0104] Adopt conventional extraction and separation techniques. Specifically, take fresh sarcophyton glaucum, wash and dry it in the sun, crush it into particles with a particle size ≤ 0.2 mm, add the particles to an ethanol solution with a concentration of 90% for extraction, filter the extract after extraction and concentrate it under reduced pressure to an extract, partition the extract with ethyl acetate / water, take the ethyl acetate extract and concentrate it under reduced pressure to obtain an ethyl acetate extract, then perform column chromatography on the extract with silica gel H, elute it with a petroleum ether / ethyl acetate eluent with gradually increasing polarity in a gradient manner, and obtain two components successively from the eluent with a volume ratio of petroleum ether:ethyl acetate = 20:80. Take the colorless columnar crystal component, which is sarcophytol A;
[0105] S3. Add marine sterol to the mixed essential oil according to the weight ratio, and stir and mix at a rate of 300 r / min for 0.6 h under the heating condition of 42 °C to obtain the product.
[0106] In addition, on the basis of Example 3, gradually increase the dosage of marine sterol and keep the process parameters unchanged to obtain the following Comparative Examples 4-6 (Table 1):
[0107] Table 1: Dosages of each component in Comparative Examples 4-6
[0108]
[0109] III. Safety and skin care effect tests
[0110] Take the plant essential oils prepared in the above Examples 1-3 and Comparative Examples 1-6, use sweet almond oil as the base oil to dilute them (dilution ratio is 1:100) to obtain the essential oil samples to be tested, and conduct the following tests on the essential oil samples:
[0111] (1) Safety test:
[0112] Referring to the test methods in Chapter 7 of the "Technical Specifications for Cosmetics Safety (2015 Edition)", the human skin patch test was adopted. 100 volunteers (with actual ages ranging from 20 to 55 years old) were selected as the test subjects (excluding insulin-dependent diabetes patients, asthma or other chronic respiratory disease patients under treatment, highly sensitive individuals, lactating or pregnant women, etc. Eligible volunteers signed an informed consent form), and the potential possibility of the plant essential oils in the above-mentioned examples and comparative examples causing adverse reactions on human skin was detected. The specific detection process was as follows: The essential oil sample was placed in the small chamber of the patch tester, with a dosage of 0.02 ml. The control hole was blank-controlled with distilled water. The patch tester with the sample was applied to the flexor side of the forearm of the subject, and gently pressed with the palm to make it evenly adhere to the skin for 24 h. The skin reactions were observed according to the grading standard in Table 2 below 30 min, 24 h, and 48 h after removing the patch tester of the test substance, and the results were recorded.
[0113] Table 2: Grading standard for closed patch skin reactions
[0114]
[0115] (2) Anti-wrinkle effect test:
[0116] Referring to the "Test Method for Anti-wrinkle Efficacy of Cosmetics (T / ZHCA006-2019)", 270 Chinese female volunteers with crow's feet grade ≥ 2 points (with actual ages ranging from 35 to 62 years old, eligible volunteers were selected and signed an informed consent form) were selected. There were no obvious interfering factors affecting the test results in the test area: birthmarks, pimples, scratches, moles, etc. Women in lactation, pregnancy, or family planning period; people with allergic constitution, allergic dermatitis, and those receiving dermatological treatment, etc. who affected the test were excluded. The test environment temperature was (21.0 ± 1.0) °C, and the test environment humidity was 50% ± 10%. The volunteers were randomly divided into 9 groups, with 30 in each group. Each group continuously used the essential oil samples of the above-mentioned examples and comparative examples for 4 weeks. Photos were taken using a Primos-CR-3D skin analyzer at 0 week, 2 weeks, and 4 weeks respectively (Note: Before taking the photos, the facial skin of the volunteers was cleaned with clean water. After cleaning, they entered the constant temperature and humidity room and sat still for 30 min, and then the volunteers participating in the test were photographed). The parameters of the crow's feet degree were analyzed, including the number, depth, area, and length, and the results were recorded (the average value of each group was taken). [[ID=??]] [[ID=??]]
[0117] (3) Skin brightening effect test:
[0118] 270 volunteers were selected. Inclusion criteria: healthy Chinese women, aged 18 - 45; not sensitive to common skin care products; high compliance. Exclusion criteria: those who had used antihistamines in the past week or immunosuppressants in the past month; those who had used any anti - inflammatory drugs on the test area in the past two months; insulin - dependent diabetes patients; patients with respiratory diseases under treatment; people with allergic constitution, allergic dermatitis, etc., and those with a history of skin diseases; people under dermatological treatment or those who had taken hydroxy - acid, whitening, and anti - aging drugs within one month; those with skin manifestations such as large - area birthmarks, scratches, leukoplakia, pigmented nevi, keloid scars, etc. on the test area that affected the experiment. Eligible volunteers signed the informed consent form.
[0119] The volunteers were randomly divided into 9 groups, with 30 in each group. In a test environment with constant temperature and humidity, the temperature was (21.0 ± 1.0) °C and the humidity was 50% ± 10%. Before the test, the subjects first cleaned their faces uniformly as required, rested in the constant - temperature and humidity room for 20 min, and used the standard light of Visia - CR to collect facial images as the initial facial images before applying the samples; then, each group of volunteers was respectively applied with the essential oil samples of each example and comparative example. According to the dosage of 2 mg / cm 2 , after the plant essential oil was applied to fully adhere to the skin, Visia - CR was used to collect the second facial image; 8 h after application, Visia - CR was used again to collect the facial image to obtain the third facial image.
[0120] For the above - mentioned standard - light images, skin color analysis was carried out. The AOI area was selected on the cheek or forehead. Using the Lab color channel of the calculation macro part, the Lab mean value was obtained, the L value representing skin color brightness was extracted, the ITA° value (individual type angle) representing skin color whiteness was calculated, and the results were recorded.
[0121] IV. Result Analysis
[0122] (1) Safety test:
[0123] All 100 volunteers completed the 24 - h skin - closed patch test of each example and comparative example. 30 min, 24 h, and 48 h after removing the patch tester, the essential oil samples of each example and comparative example did not cause adverse reactions to the skin, that is, all were grade 0 negative reactions.
[0124] (2) Anti - wrinkle effect test:
[0125] After the subjects continuously used the plant essential oil, the anti - wrinkle efficacy of the essential oil was evaluated using the skin wrinkle analysis system Primos. The evaluation results were statistically obtained Figures 1-4It can be seen that for the essential oil samples prepared in Examples 1-3 of the present invention, after 4 weeks of use, the number of wrinkles, wrinkle depth, wrinkle area, and wrinkle length have all been significantly improved. In particular, in Example 2, the effects in all aspects are better than those in Example 1 and Example 3.
[0126] In Comparative Example 1, marine biological sterol was not added to the formula, resulting in a significantly worse anti-wrinkle effect compared to Example 2; in Comparative Example 2 and Comparative Example 3, only one component of styelasterol or sarcophytol A was added respectively, and the anti-wrinkle effect was also significantly worse than that in Example 2, and only slightly improved compared to Comparative Example 1. This shows that styelasterol and sarcophytol A must be added simultaneously in a certain proportion to achieve the best effect, otherwise the effect is not obvious; in Comparative Examples 4-6, the amount of marine biological sterol was gradually increased on the basis of Example 3. It can be seen that when the amount of marine biological sterol is 0.7 g, its effect is basically equivalent to that of Example 3, with advantages and disadvantages. This shows that the additional 0.2 g does not play a role. When the amount of marine biological sterol is 0.9 g and 1.1 g, the anti-wrinkle effect becomes worse and worse, and is comprehensively inferior to Example 3. When the amount reaches 1.1 g, the anti-wrinkle effect in some aspects is even inferior to that without adding marine biological sterol. This shows that the amount of marine biological sterol is not the more the better, and it can only play a better effect within the range of less than 0.5%.
[0127] (3)Skin brightening effect test:
[0128] Table 3: Test results of skin brightening effect
[0129]
[0130] As can be seen from Table 3, after using the essential oil samples prepared in Examples 1-3 of the present invention, the whiteness and brightness of the skin can be immediately significantly improved, and can be maintained at a level basically equivalent to that immediately after use after 8 h, indicating that the plant essential oil of the present invention can significantly brighten the skin color.
[0131] In Comparative Example 1, marine biological sterol was not added to the formulation, resulting in a significantly worse skin brightening effect compared to Example 2. In Comparative Example 2 and Comparative Example 3, only one component of Styela clava sterol or Sarcophyton glaucum sterol was added respectively, and the skin brightening effect was also significantly worse compared to Example 2, and only slightly improved compared to Comparative Example 1. This shows that Styela clava sterol and Sarcophyton glaucum sterol must be added simultaneously in a certain proportion to achieve the best effect, otherwise the effect is not obvious. In Comparative Examples 4-6, the amount of marine biological sterol was gradually increased on the basis of Example 3. It can be seen that there is a difference from the anti-wrinkle effect here. When the amount of marine biological sterol exceeds 0.5 g, with the increase of the amount, the skin brightening effect becomes worse and worse, and all are comprehensively inferior to Example 3, further demonstrating that the amount of marine biological sterol is not the more the better, and it can only achieve a better effect within the range of less than 0.5%.
[0132] The above embodiments only represent several implementation manners of the present invention, and the description thereof is relatively specific and detailed, but it should not be construed as a limitation to the scope of the patent of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can be made, and these all belong to the protection scope of the present invention.
Claims
1. A natural firming, anti-wrinkle and skin-brightening plant essential oil, characterized in that, The raw materials of the plant essential oil, by weight percentage, include: Boswellia oil 30.0 - 40.0%; Santalum oil 15.0 - 20.0%; Lavender oil 10.0 - 15.0%; Commiphora oil 8.0 - 12.0%; Helichrysum italicum oil 12.0 - 18.0%; Cistus ladaniferus oil 0.5 - 1.5%; Rosa damascena flower oil 5.0 - 10.0%; Vetiver root oil 0.5 - 1.5%; and Marine biological sterol 0.1 - 0.5%; The marine biological sterol is composed of a mixture of styelosterol and sarcophytol A, and the weight ratio of styelosterol to sarcophytol A is 1:3; The preparation steps of the styelosterol are as follows: Take fresh Styela clava, wash and dry in the sun, crush it into particles with a particle size ≤ 0.2 mm, add the particles to an ethanol solution with a concentration of 90% for extraction, filter the extract after extraction, and concentrate it under reduced pressure to obtain a primary extract. Then, extract the primary extract with ethyl acetate, and concentrate it under reduced pressure to obtain a secondary extract. Then, add the secondary extract to a methanol solution with a concentration of 90%, extract it with n - hexane, and concentrate it under reduced pressure to obtain an n - hexane extract. Perform normal - pressure silica gel column chromatography on the n - hexane extract, use chloroform / methanol eluent for gradient elution, and the gradient volume ratio changes from 100:0 to 50:
50. Monitor by TLC, combine the same parts and concentrate, and then perform Sephadex LH - 20 gel column chromatography. The eluent is methanol:chloroform = 1:1 to obtain two components. Take the colorless needle - shaped crystal component, which is styelosterol; The preparation steps of the sarcophytol A are as follows: Take fresh Sarcophyton glaucum, wash and dry in the sun, crush it into particles with a particle size ≤ 0.2 mm, add the particles to an ethanol solution with a concentration of 90% for extraction, filter the extract after extraction, and concentrate it under reduced pressure to obtain an extract. Partition the extract with ethyl acetate / water, take the ethyl acetate extract and concentrate it under reduced pressure to obtain an ethyl acetate extract. Then, perform column chromatography on the extract with silica gel H, use petroleum ether / ethyl acetate eluent with gradually increasing polarity for gradient elution, and obtain two components in sequence from the eluent with a volume ratio of petroleum ether:ethyl acetate = 20:
80. Take the colorless columnar crystal component, which is sarcophytol A.
2. The natural firming, anti-wrinkle and brightening plant essential oil according to claim 1, characterized in that, The raw materials of the plant essential oil, by weight percentage, include: Boswellia oil 35.0%; Santalum oil 17.5%; Lavender oil 12.5%; Commiphora oil 10.0%; Helichrysum italicum oil 15.0%; Cistus ladaniferus oil 1.0%; Rosa damascena flower oil 8.0%; Vetiver root oil 0.8%; and Marine biological sterol 0.2%.
3. A method for preparing the natural firming, anti-wrinkle and skin-brightening plant essential oil as described in claim 1 or 2, characterized in that, The steps of the preparation method include: S1. Weigh Boswellia oil, Santalum oil, Lavender oil, Commiphora oil, Helichrysum italicum oil, Cistus ladaniferus oil, Rosa damascena flower oil, and Vetiver root oil according to the weight ratio, place them in a container and mix until homogeneous to obtain a mixed essential oil; S2. Take the styelosterol and sarcophytol A and mix them evenly according to the weight ratio to obtain the marine biological sterol; S3. Add the marine biological sterol to the mixed essential oil according to the weight ratio and mix evenly again to obtain the product.
4. The preparation method of the natural firming, anti-wrinkle and brightening plant essential oil according to claim 3, characterized in that, In step S1, the specific operation of mixing to homogeneity is as follows: stirring and mixing at a rate of 150 - 300 r / min for 2 - 4 h under the heating condition of 35 - 40 °C.
5. The preparation method of the natural firming, anti-wrinkle and brightening plant essential oil according to claim 3, wherein, In step S3, the specific operation of mixing evenly is as follows: stirring and mixing at a rate of 250 - 350 r / min for 0.2 - 1 h under the heating condition of 40 - 45 °C.
6. Application of the natural firming, anti-wrinkle and brightening plant essential oil according to claim 1 or 2 in skin care products.
7. The application according to claim 6, characterized in that The skin care product is one of an aqueous solution, a facial mask, a lotion, a cream or a liquid foundation.
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