WO2018019145A1 - 一种山茶花提取液及其制备方法和应用 - Google Patents
一种山茶花提取液及其制备方法和应用 Download PDFInfo
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- WO2018019145A1 WO2018019145A1 PCT/CN2017/093117 CN2017093117W WO2018019145A1 WO 2018019145 A1 WO2018019145 A1 WO 2018019145A1 CN 2017093117 W CN2017093117 W CN 2017093117W WO 2018019145 A1 WO2018019145 A1 WO 2018019145A1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
Definitions
- the invention belongs to the technical field of cosmetics, in particular to a camellia extract and a preparation method and application thereof.
- Camellia also known as Camellia, is a Camellia genus of Camellia. It originated in China and has a long history of cultivation. So far, Japan, South Korea, Australia, the United States and other countries have developed rapidly in the breeding, planting and production of camellia, and have entered industrial production. stage. Camellia has the functions of promoting blood circulation, stopping diarrhea, and detoxifying and sore. The rich flavonoids, saponins and polyphenols contained in Camellia have excellent anti-oxidation and anti-free radical effects, and the cosmetics prepared by them have anti-free radical, anti-aging, blemish, moisturizing and sunscreen effects.
- the camellia extract is mostly extracted by high-temperature reflux extraction or distillation with organic solvent or directly extracted with water as a solvent.
- the obtained extract has low anti-oxidation effect components, so it needs to be concentrated to concentrate or dried to be dry powder for storage. Dilute or dissolve when using.
- the small amount of active ingredients in the camellia extract or dry powder obtained by such a method not only causes the camellia to lose its original color and fragrance, but also greatly reduces its antioxidant and anti-free radical effects.
- camellia extract in which the anti-oxidant effect of Camellia is comprehensive and high in content, and it is of great significance for safety and stability.
- a first object of the present invention is to provide a method for preparing a camellia extract to overcome the defects in the prior art, and to obtain an anti-oxidation effect component which is comprehensive and high in content, has excellent antioxidant effect, and is safe and stable. Good camellia extract.
- the present invention adopts the following technical solutions:
- a method for preparing a camellia extract comprises the following steps:
- control ultrasonic frequency is 20 ⁇ 25KHz
- ultrasonic power is 1.0 ⁇ 2.0KW
- the ultrasonic temperature is 15 to 50 ° C, then filtered, sterilized and tested to obtain a camellia extract.
- the length of the small step in the step 1) is 0.5 to 3 cm.
- the inorganic acid and/or organic acid in the step 2) is added in an amount of 0.25 to 2.5% by mass of the solvent.
- the solvent in the step 2) is one or more of water, ethanol, 1,3-propanediol, 1,2-propanediol, glycerin, 1,3-butanediol, and sorbitol.
- the inorganic acid in the step 2) is one or both of hydrochloric acid and acetic acid.
- the organic acid in the step 2) is one or more of phytic acid, citric acid, ascorbic acid and lactic acid.
- a second object of the present invention is to provide a camellia extract prepared by the above method.
- camellia extract contains the following antioxidant components: kaempferol: 0.43 to 4.52 ppm, quercetin: 1.09 to 8.17 ppm, and quercetin: 45.62 to 197.81 ppm.
- a third object of the present invention is to provide a cosmetic application using the above-mentioned camellia extract as an active ingredient.
- camellia extract is used in the preparation of a cosmetic having antioxidant effects.
- a whitening lotion prepared from the camellia extract as an active ingredient consisting of the following parts by weight:
- Camellia extract 2.0 to 10.0 parts of Camellia extract, 1.0 to 3.0 parts of plant sensitizer, 2.0 to 5.0 parts of glycerin, 2.0 to 6.0 parts of 1,3-butanediol, 0.2 to 5.0 parts of trehalose, 0.2 to 2.0 parts of betaine, and white fungus 0.005 to 0.4 parts of polysaccharide, 0.005 to 0.2 parts of sodium hyaluronate, 0.3 to 0.6 parts of phenoxyethanol, 0.1 to 0.3 parts of ethylhexylglycerol, 0.1 to 0.3 parts of essential oil, and the balance of water.
- An anti-aging whitening gel prepared from the camellia extract as an active ingredient consisting of the following parts by weight:
- Camellia extract 1.0 to 10.0 parts, plant sensitizer 1.0 to 3.0 parts, glycerin 2.0 to 6.0 parts, 1,3-propanediol 2.0 to 6.0 parts, trehalose 0.2 to 5.0 parts, betaine 0.2 to 2.0 parts, hyaluronic acid 0.005 to 0.2 parts of sodium, 0.5 to 1.0 part of xanthan gum, 0.05 to 0.20 parts of disodium EDTA, 0.3 to 0.6 parts of phenoxyethanol, 0.1 to 0.3 parts of ethylhexylglycerol, 0.1 to 0.3 parts of essential oil, and the balance of water.
- An anti-aging whitening emulsion prepared from the camellia extract as an active ingredient consisting of the following parts by weight:
- Camellia extract 5.0 to 8.0 parts of Camellia extract, 5.0 to 11.0 parts of grape seed oil, 7.0 to 12.0 parts of olive oil, 2.0 to 6.0 parts of glycerin, 2.0 to 6.0 parts of 1,3-propanediol, 1.5 to 4.0 parts of glyceryl caprylate, and wild Soybean seed extract 0.5-1.0 parts, carbomer 0.2-0.8 parts, sodium hyaluronate 0.005-0.1 parts, phenoxyethanol 0.3-0.6 parts, ethylhexyl glycerol 0.1-0.3 parts, essential oil 0.1-0.3 parts, hydrogen Sodium oxide (33% solution) 0.2 to 0.8 parts, the balance of water.
- An anti-oxidative whitening sleep mask prepared from the camellia extract as an active component consisting of the following components by weight:
- Camellia extract 2.0 to 15.0 parts, glycerin 1.0 to 4.0 parts, 1,3-propanediol 2.0 to 6.0 parts, 1,3-butanediol 2.0 to 6.0 parts, trehalose 0.5 to 2.0 parts, Tremella polysaccharides 0.005 to 0.3 parts, 0.4-0.9 parts of acryloyldimethyltaurylamine/VP copolymer, 0.005-0.2 parts of sodium hyaluronate, 0.05-0.2 parts of disodium EDTA, 0.3-0.6 parts of phenoxyethanol, 0.1-0.3 of ethylhexyl glycerol Serve, 0.1 to 0.3 parts of essential oil, the balance of water.
- An anti-oxidant whitening cream prepared by using the camellia extract as an active component consisting of the following components by weight:
- the present invention has the following beneficial effects:
- the anti-oxidation effect component of the camellia extract in the camellia extract of the present invention has a comprehensive and low-stability active ingredient, a pigment, and a volatile volatile oil component, and the color and flavor of the camellia and the active ingredient are maintained to the greatest extent, and the antioxidant property is strong. , good security and stability.
- the cosmetics prepared by using the camellia extract of the invention are safe and have no side effects, can effectively promote cell metabolism after being applied to the skin, maintain skin elasticity, can improve and nourish the skin, and have excellent whitening, blemishes and anti-aging. Efficacy, can effectively delay skin aging, make skin regain luster and elasticity.
- Figure 1 is a flow chart showing the extraction process of the camellia extract of the present invention.
- Example 2 is an HPLC chart of a camellia extract prepared in Example 3 of the present invention.
- Fig. 5 is a graph showing the skin condition before and after the use of the cosmetic containing the camellia extract of the present invention.
- Fig. 6 is a comparison diagram of infrared photographs of skin conditions before and after use of a cosmetic containing the camellia extract of the present invention.
- Fig. 7 is a view showing a skin wrinkle before use of a cosmetic containing the camellia extract of the present invention.
- Fig. 8 is a view showing a skin wrinkle after use of a cosmetic containing the camellia extract of the present invention.
- the raw materials and equipment of the present invention are all commercially available.
- Test method DPPH (1,1-diphenyl-2-trinitrophenylhydrazine) analysis method is based on DPPH radicals having a single electron, used as a monitoring reaction substance in a chemical reaction containing free radicals, Evaluation of in vitro antioxidant activity of antioxidant components.
- Test method ABTS (2,2'-azino-bis-(3-ethylbenzodihydrothiazoline-6-sulfonic acid)) analysis method, according to ABTS free radicals, oxidized to green under the action of appropriate oxidant ABTS ⁇ +, the production of ABTS ⁇ + is inhibited in the presence of antioxidants.
- the absorbance of ABTS can be determined at 734nm or 405nm to determine and calculate the total antioxidant capacity of the sample. It is widely used in natural water-soluble phenolic substances. Determination of antioxidant activity.
- High performance liquid chromatography conditions using Shimadzu C18 reverse phase column, methanol-0.4% phosphoric acid as mobile phase, mobile phase flow rate: 1.0mL ⁇ min ⁇ 1 , detection wavelength: 370nm, column temperature: 40°C, injection volume: 10 ⁇ L, using commercially available quercetin, kaempferol, and quercetin standards (analytically pure, 99.9%) as standard samples for quantitative detection.
- Camellia extract dilution ie 10g camellia extract diluted with 90g water
- carry out patch test soak the dilution 4 layers of 1cm 2 gauze, set the forearm flexion side, which is slightly larger than the gauze Covered with clear cellophane, surrounded by adhesive plaster, removed after 48 hours to see the reaction induced by local skin, and the safety results of the camellia extract were determined according to the local skin performance at 48 hours and 72 hours respectively.
- the extracts were stored at 50 ° C, 4 ° C, room temperature (25 ° C), and exposed to direct sunlight for 1-3 months. The appearance was observed and the antioxidant activity was measured by an antioxidant test.
- step 2) soaked mixture is sonicated for 30 ⁇ 60min, ultrasonic frequency is 20 ⁇ 25KHz, ultrasonic power is 1.0 ⁇ 2.0KW, ultrasonic temperature is 15 ⁇ 50 ° C, filtered to obtain camellia extract.
- Camellia extract formulations of Examples 1 to 11 are shown in Table 1.
- camellia extracts Two commercially available camellia extracts were used as comparisons and tested for efficacy.
- Commercially available camellia extracts were obtained by heating and leaching with ethanol, respectively.
- Comparative Example 1 contains only one antioxidant component, quercetin, and the Camellia extract of Comparative Example 2, although containing three antioxidant components, kaempferol, quercetin and Quercetin, but the content of the antioxidant component in the camellia extract of the present invention is significantly higher than that of the Camellia extract of Comparative Example 1 and Comparative Example 2, indicating that the antioxidant component of the camellia extract of the present invention is comprehensive and high in content.
- camellia extracts prepared in Examples 1 to 11 and Comparative Examples 1 and 2 were prepared into a test solution having a concentration of 2.5%, and the DPPH radical scavenging rate was measured. The results are shown in Tables 5 and 6.
- camellia extracts prepared in Examples 1 to 11 and Comparative Examples 1 and 2 were prepared into a test solution having a concentration of 2.5%, and the ABTS radical scavenging rate was measured. The results are shown in Table 8 and Table 9.
- Table 8 ABTS free radical scavenging rate of Camellia extracts of Examples 1-11
- Camellia extract has excellent antioxidant properties.
- the camellia extracts of Examples 1 to 11 were separately stored at 50 ° C, incubator storage conditions, 4 ° C, refrigerator refrigeration conditions, room temperature (25 ° C, cool and ventilated) conditions or (25 ° C, direct sunlight) Under the conditions of 2 months, the appearance color was observed and its ability to scavenge DPPH free radicals and ABTS free radicals was examined.
- the camellia extract of the invention has good stability, and is kept at a constant temperature of 50 ° C for 2 months, the color is slightly lighter, the active ingredient is basically unchanged, and the DPPH free radical and ABTS free radical ability are still kept high. Whether it is low temperature, normal temperature or direct sunlight, the color of the camellia extract is unchanged, and the active ingredient is basically unchanged, indicating that the camellia extract of the present invention has good stability.
- the preparation method of the above lotion containing the camellia extract comprises the following steps:
- the anti-aging whitening gel formula containing camellia extract is shown in Table 12:
- the preparation method of the above gel containing the camellia extract comprises the following steps:
- the anti-aging whitening lotion formula containing the camellia extract is shown in Table 13:
- the preparation method of the above emulsion containing Camellia extract comprises the following steps:
- step 2 2) adding the formulated amount of grape seed oil, olive oil, caprylic glyceride, wild soybean seed extract to the phase A prepared in step 1);
- the sleep mask formula containing the camellia extract is shown in Table 14:
- the preparation method of the above sleeping mask containing the camellia extract comprises the following steps:
- the antioxidant whitening cream formula containing Camellia extract is shown in Table 15:
- the above preparation method of the cream containing the camellia extract comprises the following steps:
- the skin care process involves a plurality of steps.
- the skin care steps are generally: washing the face, taking a lotion, taking an emulsion, condensing, applying a cream, and using a sleep mask before going to bed. Therefore, it is necessary to use all the cosmetics of Examples 17 to 31 of the present invention.
- the skin condition before and after skin care using the skin care product containing the camellia extract of the present invention is examined, and photographs and infrared photographs are taken before the tester uses 45 days and 90 days of use, as shown in Figs. 5 and 6. Can be seen from Figure 5 and Figure 6. Out, before use, the tester had more dark spots on the skin, dull complexion and uneven skin tone.
- the pigment at the bottom of the skin became uniform, the skin pigmentation was significantly reduced, and the skin texture became well-balanced, indicating that the camellia extract was extracted by the present invention.
- the cosmetics in which the liquid is an active component have excellent whitening and blemish effects.
- the above-mentioned cosmetics of the present invention are used alone or in combination with other cosmetics, and have the effects of whitening, blemishes, and anti-aging.
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Abstract
一种山茶花提取液的制备方法，包括如下步骤：1)、新鲜山茶花和/或新鲜山茶花花蕾剔除杂质并切碎成小段，作为原料备用；2)、将一定量的原料置入超声釜中，加入质量比为1:3～30的溶剂，搅拌均匀后加入一定量的无机酸和/或有机酸，调节pH值至1.3～3.0，浸泡10～30min；3)、然后超声处理30～60min，控制超声频率为20～25KHz，超声功率为1.0～2.0KW，超声温度为15～50℃，然后过滤，灭菌并检测，得到山茶花提取液。山茶花提取液在最大程度上保持了山茶花的色泽香味和有效活性成分，其抗氧化功效成分全面且含量高，安全性和稳定性好，采用山茶花提取液为活性组分制备的化妆品具有优异的美白、淡斑及抗衰老功效。
Description
本发明属于化妆品技术领域，具体地说，是关于一种山茶花提取液及其制备方法和应用。
发明背景
山茶花，又名茶花，为山茶科山茶属植物，起源于中国，栽培历史悠久，至今日本、韩国、澳大利亚、美国等国在山茶花的育种、种植、生产方面发展很快，已进入产业化生产的阶段。山茶花具有活血止血、收敛止泻、解毒敛疮之功能。茶花含有的丰富的黄酮类、皂苷类、多酚类化合物具有优异的抗氧化抗自由基的功效，以其制备的化妆品具有抗自由基、抗衰、淡斑、保湿、防晒的效果。
目前，山茶花提取液多采用有机溶剂高温回流提取或蒸馏提取或直接用水作溶剂高温提取，所得的提取液中抗氧化功效成分含量低，因此需要再通过浓缩为浓缩液或干燥成为干粉以便于存储，使用时再进行稀释或溶解。这样的方法得到的山茶花提取液或干粉中的活性成分少，不仅使得山茶花失去原有的色泽和香味，还极大地降低了其抗氧化抗自由基的功效。
因此，研发一种山茶花提取液，其中的山茶花抗氧化功效成分全面且含量高，且安全性和稳定性好就具有十分重要的意义。
发明内容
本发明的第一个目的在于提供一种山茶花提取液的制备方法，以克服现有技术中的缺陷，制备得到抗氧化功效成分全面且含量高，具有优异的抗氧化功效且安全性和稳定性好的山茶花提取液。
为实现上述目的，本发明采用如下技术方案：
一种山茶花提取液的制备方法，包括如下制备步骤：
1)、新鲜山茶花和/或新鲜山茶花花蕾剔除杂质并切碎成小段，作为原料备用；
2)、将一定量的原料置入超声釜中，加入与原料质量比为1:3～30的溶剂，搅拌均匀后加入一定量的无机酸和/或有机酸，调节pH值至1.3～3.0，浸泡10～30min；
3)、然后超声处理30～60min，控制超声频率为20～25KHz，超声功率为1.0～2.0KW，
超声温度为15～50℃，然后过滤，灭菌并检测，得到山茶花提取液。
进一步地，所述步骤1)中的小段的长度为0.5～3cm。
所述步骤2)中的所述无机酸和/或有机酸的加入量为溶剂质量的0.25～2.5％。
所述步骤2)中的溶剂为水、乙醇、1,3-丙二醇、1,2-丙二醇、甘油、1,3-丁二醇、山梨醇中的一种或几种。
所述步骤2)中的无机酸为盐酸和乙酸中的一种或两种。
所述步骤2)中的有机酸为植酸、柠檬酸、抗坏血酸和乳酸中的一种或几种。
本发明的第二个目的在于提供上述方法制备的山茶花提取液。
进一步地，所述山茶花提取液含有如下抗氧化组分：山奈酚：0.43～4.52ppm，槲皮素：1.09～8.17ppm，槲皮苷：45.62～197.81ppm。
本发明的第三个目的是提供一种以上述山茶花提取液为活性成分的化妆品应用。
进一步地，所述的山茶花提取液在制备具有抗氧化功效的化妆品中应用。
一种由所述的山茶花提取液为活性组分制备的美白化妆水，由如下重量份的组分组成：
山茶花提取液2.0～10.0份、植物舒敏剂1.0～3.0份、甘油2.0～5.0份、1,3-丁二醇2.0～6.0份、海藻糖0.2～5.0份、甜菜碱0.2～2.0份、银耳多糖0.005～0.4份、透明质酸钠0.005～0.2份、苯氧乙醇0.3～0.6份、乙基己基甘油0.1～0.3份、精油0.1～0.3份，余量的水。
一种由所述的山茶花提取液为活性组分制备的抗衰老美白凝露，由如下重量份的组分组成：
山茶花提取液1.0～10.0份、植物舒敏剂1.0～3.0份、甘油2.0～6.0份、1,3-丙二醇2.0～6.0份、海藻糖0.2～5.0份、甜菜碱0.2～2.0份、透明质酸钠0.005～0.2份，黄原胶0.5～1.0份、EDTA二钠0.05～0.20份、苯氧乙醇0.3～0.6份、乙基己基甘油0.1～0.3份、精油0.1～0.3份，余量的水。
一种由所述的山茶花提取液为活性组分制备的抗衰老美白乳液，由如下重量份的组分组成：
山茶花提取液1.0～8.0份、葡萄籽油5.0～11.0份、橄榄油7.0～12.0份、甘油2.0～6.0份、1,3-丙二醇2.0～6.0份、辛酸癸酸甘油酯1.5～4.0份、野大豆籽提取物0.5～1.0份、卡波姆0.2～0.8份、透明质酸钠0.005～0.1份、苯氧乙醇0.3～0.6份、乙基己基甘油0.1～0.3份、精油0.1～0.3份、氢氧化钠(33％溶液)0.2～0.8份，余量的水。
一种由所述的山茶花提取液为活性组分制备的抗氧化美白睡眠面膜，由如下重量份的组分组成：
山茶花提取液2.0～15.0份、甘油1.0～4.0份、1,3-丙二醇2.0～6.0份、1,3-丁二醇2.0～6.0份、海藻糖0.5～2.0份、银耳多糖0.005～0.3份、丙烯酰二甲基牛磺酸胺/VP共聚物0.4～0.9份、透明质酸钠0.005～0.2份、EDTA二钠0.05～0.2份、苯氧乙醇0.3～0.6份、乙基己基甘油0.1～0.3份、精油0.1～0.3份，余量的水。
一种由所述的山茶花提取液为活性组分制备的抗氧化美白面霜，由如下重量份的组分组成：
山茶花提取液2.0～6.0份、霍霍巴油5.0～12.0份、乳木果油4.0～8.0份、鲸蜡基葡萄糖苷2.5～6.0份、橄榄油1.0～5.0份、小麦胚芽油2.0～5.0份、甘油2.0～5.0份、1,3-丙二醇2.0～6.0份、辛酸癸酸甘油酯1.0～5.0份、海藻糖0.5～4.0份、野大豆籽提取物0.5～1.0份、维生素E醋酸酯0.05～0.5份、透明质酸钠0.005～0.1份、银耳多糖0.005～0.2份、苯氧乙醇0.3～0.6份、乙基己基甘油0.1～0.3份、精油0.1～0.3份，余量的水。
与现有技术相比，本发明具有如下有益效果：
1)本发明的山茶花提取液中的山茶花抗氧化功效成分全面且低稳定活性成分、色素以及香气挥发油成分含量高，再最大程度地保持了山茶花的色泽香味和有效活性成分，具有抗氧化性强，安全性和稳定性好的特点。
2)采用本发明的山茶花提取液制备的化妆品安全、无副作用，应用于皮肤后可有效促进细胞新陈代谢，保持皮肤弹性，能够改善及营养皮肤，具有优异的具有优异的美白、淡斑及抗衰老功效，能够有效地延缓肌肤衰老，令皮肤重现光泽及弹性。
图1为本发明的山茶花提取液提取工艺流程图。
图2为本发明的实施例3制备的山茶花提取液的HPLC图谱。
图3为对比例1的山茶花提取液的HPLC图谱。
图4为对比例2的山茶花提取液的HPLC图谱。
图5为使用含有本发明的山茶花提取液的化妆品前后的皮肤状况对比图。
图6为使用含有本发明的山茶花提取液的化妆品前后的皮肤状况红外线拍摄对比图。
图7为使用含有本发明的山茶花提取液的化妆品前的皮肤皱纹图。
图8为使用含有本发明的山茶花提取液的化妆品后的皮肤皱纹图。
以下结合具体实施例，对本发明做进一步说明。应理解，以下实施例仅用于说明本发明而非用于限制本发明的范围。
本发明的原料和设备均为市售。
功效检测方法：
(一)、清除DPPH自由基试验
测试方法：DPPH(1，1-二苯基-2-三硝基苯肼)分析方法是依据DPPH自由基具有单电子，在含有自由基的化学反应中作为一种监测反应的物质，用以抗氧化成分的体外抗氧化性评价。
(二)、清除ABTS自由基试验
测试方法：ABTS(2,2’-连氮基-双-(3-乙基苯并二氢噻唑啉-6-磺酸))分析方法，依据ABTS自由基在适当的氧化剂作用下氧化成绿色的ABTS■+，在抗氧化物存在时ABTS■+的产生会被抑制，在734nm或405nm测定ABTS的吸光度即可测定并计算出样品的总抗氧化能力，广泛应用于天然水溶性酚类物质抗氧化活性的测定。
(三)、高效液相色谱(HPLC)定量分析试验
高效液相色谱条件：采用岛津C18反相柱，以甲醇-0.4％磷酸为流动相，流动相流速:1.0mL·min～1，检测波长:370nm，柱温:40℃，进样量:10μL，以市售槲皮素、山奈酚、槲皮苷标准品(分析纯，含量99.9％)为标样，进行定量检测。
(四)、安全性试验
采用10％山茶花提取稀释液(即10g山茶花提取液加入90g水稀释)，进行斑贴实验：将稀释液浸湿4层1cm2大小的纱布，置前臂屈侧，其上用较纱布稍大的透明玻璃纸覆盖，四周用橡皮膏固定，经48小时取下，查看诱发局部皮肤出现的反应，于48小时、72小时分别根据局部皮肤表现判读山茶花提取液的安全性结果。
(五)、稳定性测试
将提取液分别储存在50℃、4℃、室温(25℃)、阳光直射1～3个月，观察其外观、并通过抗氧化测试检测其抗氧化活性变化情况。
(六)、化妆品性能测试
采用Courage+Khazaka electronic GmbH(CK)公司的皮肤测试仪，通过红外线拍摄结果显示皮肤底层色素变化进而获得肌肤质地数据和皱纹测试数据。
实施例1～11、山茶花提取液的制备
实施例1～11的山茶花提取液的具体制备方法如下：
1)新鲜山茶花或新鲜山茶花花蕾，剔除杂质并切碎为0.5～3cm的小段，作为原料备用；
2)、将一定量的原料置入超声釜中，加入与原料质量比为1:3～30的溶剂，搅拌均匀后加入溶剂质量的0.25～2.5％的无机酸和/或有机酸，控制pH值在1.3～3.0，混合液浸泡10～30min；
3)、对步骤2)浸泡好的混合液进行超声处理30～60min，超声频率为20～25KHz，超声功率为1.0～2.0KW，超声温度为15～50℃，过滤得到山茶花提取液。
4)对上述山茶花提取液进行灭菌和功效检测。
实施例1～11的山茶花提取配方如表1所示。
表1山茶花提取配方
注：表1中酸浓度均为质量浓度。
对比例1～2：
采用两家市售的山茶花提取液作为对比，并对其进行功效检测。市售山茶花提取液分别通过乙醇加热浸提得到。
实施例12：
采用高效液相色谱仪分别检测实施例1～11及对比例1～2的提取液中的活性成分，实施例3、对比例1和对比例2的HPLC图谱分别如图2、图3和图4所示，由图2至图4可以看出，本发明的山茶花提取液中含有多种活性成分，其活性组分的种类和含量均明显高于对比例1和对比例2的山茶花提取液。
分析实施例1～11及对比例1～2的提取液中的抗氧化活性组分含量，结果如表2和表3所示。
表2实施例1～11制备的山茶花提取液的抗氧化活性组分含量
表3对比例1～2的山茶花提取液的抗氧化活性组分含量
由表2和表3中的数据可以看出，对比例1中只含有一种抗氧化成分槲皮素，对比例2的山茶花提取液虽然也含有三种抗氧化成分山奈酚、槲皮素和槲皮苷，但本发明的山茶花提取液中的抗氧化成分的含量明显高于对比例1和对比例2的山茶花提取液，说明本发明的山茶花提取液中抗氧化组分全面且含量高。
实施例13：清除DPPH自由基试验
分别将0.04g、0.08g、0.16g、0.312g、0.625g、1.25g、2.5g、5.0g和10.0g实施例1制备的山茶花提取液加水至100g进行稀释，得到含有提取液0.04％、0.08％、0.16％、0.312％、0.625％、1.25％、2.5％、5.0％和10.0％的检测液，分别检测不同浓度检测液的DPPH自由基清除率如表4所示。
表4不同浓度检测液的DPPH自由基清除率
由表4中的数据可以看出，随着检测液中提取液含量的增加，检测液的DPPH自由基
清除率不断增加，当浓度大于2.5％时，DPPH自由基清除率趋于平稳，说明山茶花提取液在浓度2.5％时即可以达到较好的抗氧化性。
分别将实施例1～11与对比例1～2制备的山茶花提取液制备成浓度为2.5％的检测液，并检测其DPPH自由基清除率，结果如表5和表6所示。
表5：实施例1～11的山茶花提取液的DPPH自由基清除率
表6：对比例1～2的山茶花提取液的DPPH自由基清除率
由表5和表6中的数据可以看出，相同浓度的检测液条件下，实施例1～11制备的山茶花提取液的DPPH自由基清除率明显高于对比例1和2，几乎是对比例1和2的两倍，说明本发明的山茶花提取液具有优异的抗氧化性能。
实施例14：清除ABTS自由基实验
分别将0.04g、0.08g、0.16g、0.312g、0.625g、1.25g、2.5g、5.0g和10.0g实施例1制备的山茶花提取液加水至100g进行稀释，得到含有提取液0.04％、0.08％、0.16％、0.312％、0.625％、1.25％、2.5％、5.0％和10.0％的检测液，分别检测不同浓度检测液的ABTS自由基清除率如表7所示。
表7不同浓度检测液的ABTS自由基清除率
由表7中的数据可以看出，随着检测液中提取液含量的增加，检测液的ABTS自由基清除率不断增加，当浓度大于2.5％时，ABTS自由基清除率趋于平稳，说明山茶花提取液在浓度2.5％时即可以达到较好的抗氧化性。
分别将实施例1～11与对比例1～2制备的山茶花提取液制备成浓度为2.5％的检测液，并检测其ABTS自由基清除率，结果如表8和表9所示。
表8：实施例1～11的山茶花提取液的ABTS自由基清除率
表9：对比例1～2的山茶花提取液的ABTS自由基清除率
由表8和表9中的数据可以看出，相同浓度的检测液条件下，实施例1～11制备的山茶花提取液的ABTS自由基清除率明显高于对比例1和2，说明本发明的山茶花提取液具有优异的抗氧化性能。
实施例15：安全性试验
根据安全性试验方法，测试实施例1～11制备的山茶花提取液的安全性，斑贴试验皮肤不良反应分级标准如表10所示。
表10：斑贴试验皮肤不良反应分级标准
| 皮肤不良反应 | 分级 |
| 无反应 | 0 |
| 淡红斑 | 1 |
| 红斑、浸润、丘疹 | 2 |
| 红斑、水肿、丘疹、水疱 | 3 |
| 红斑、水肿、大疱 | 4 |
结果显示，经48小时和72小时试验，测试的局部皮肤与未测试皮肤相比并未出现淡红斑敏，红肿等现象。实施例1～11制备的山茶花提取液的分级均为0级。说明本发明的山茶花提取液对皮肤刺激性小，不会引皮肤过敏，安全性好。
实施例16：稳定性测试
根据稳定性测试方法，将实施例1～11的山茶花提取液分别储存于50℃，恒温箱保存条件、4℃，冰箱冷藏条件、室温(25℃，阴凉通风)条件或(25℃，阳光直射)条件下2个月，观察其外观颜色并检测其清除DPPH自由基和ABTS自由基能力。
结果表明：本发明的山茶花提取液具有良好的稳定性，50℃恒温保存2个月，颜色略变浅，活性成分基本没变化，依然保持较高的清楚DPPH自由基和ABTS自由基能力。无论是低温，常温还是阳光直射，山茶花提取液的颜色不变，活性成分基本不变，说明本发明的山茶花提取液具有良好的稳定性。
实施例17～19：含有山茶花提取液的美白化妆水的制备
含有山茶花提取液的美白化妆水配方如表11所示：
表11含有山茶花提取液的美白化妆水配方
上述含有山茶花提取液的化妆水的制备方法，包括如下步骤：
1)将配方量的水、甘油、1,3-丁二醇、透明质酸钠、银耳多糖、海藻糖、甜菜碱加入反应锅中，开启搅拌，加热至75～80℃，搅拌均匀；
2)开冷却循环水，边搅拌边降温，待温度降至40～45℃时加入配方量的山茶花提取液、植物舒敏剂、苯氧乙醇、乙基己基甘油和精油，搅拌均匀；
3)继续搅拌并冷却至38℃，出锅，检测合格后灌装。
实施例20～22：含有山茶花提取液的抗衰老美白凝露的制备
含有山茶花提取液的抗衰老美白凝露配方如表12所示：
表12含有山茶花提取液的抗衰老美白凝露配方
上述含有山茶花提取液的凝露的制备方法，包括如下步骤：
1)将配方量的水、甘油、1,3-丙二醇、透明质酸钠、黄原胶、EDTA二钠、海藻糖、甜菜碱加入反应锅中，开启搅拌，加热至75～80℃，搅拌均匀；
2)开冷却循环水，边搅拌边降温，待温度降至40～45℃时加入配方量的山茶花提取
液、植物舒敏剂、苯氧乙醇、乙基己基甘油和精油，搅拌均匀；
3)继续搅拌冷却至38℃，出锅，检测合格后灌装。
实施例23～25：含有山茶花提取液的抗衰老美白乳液的制备
含有山茶花提取液的抗衰老美白乳液配方如表13所示：
表13含有山茶花提取液的抗衰老美白乳液配方
上述含山茶花提取液的乳液的制备方法，包括如下步骤：
1)将配方量的卡波姆和透明质酸钠先用配方量的甘油、1,3-丙二醇预分散，然后加入水搅拌均匀，作为A相备用；
2)将配方量的葡萄籽油、橄榄油、辛酸癸酸甘油酯、野大豆籽提取物混合后加入步骤1)制备的A相中；
3)将配方量的氢氧化钠加入A相中，搅拌均匀，并根据粘度变化调整搅拌速度；
4)将配方量的山茶花提取液、苯氧乙醇、乙基己基甘油、精油加入A相中，搅拌均匀，出锅，检测合格后灌装。
实施例26～28：含有山茶花提取液的抗氧化美白睡眠面膜的制备
含有山茶花提取液的睡眠面膜配方如表14所示：
表14含有山茶花提取液的睡眠面膜配方
上述含有山茶花提取液的睡眠面膜的制备方法，包括如下步骤：
1)将配方量的丙烯酰二甲基牛磺酸胺/VP共聚物、银耳多糖和透明质酸钠先用配方量的甘油、1,3-丙二醇、1,3-丁二醇预分散，然后加水、EDTA二钠搅拌均匀，作为A相备用；
2)将配方量的海藻糖、山茶花提取液、苯氧乙醇、乙基己基甘油、精油加入A相中，搅拌均匀，出锅，检测合格后灌装。
实施例29～31：含有山茶花提取液的抗氧化美白面霜的制备
含有山茶花提取液的抗氧化美白面霜配方如表15所示：
表15含有山茶花提取液的抗氧化美白面霜配方
上述含有山茶花提取液的面霜制备方法，包括如下步骤：
1)将配方量的银耳多糖和透明质酸钠先用甘油、1,3-丙二醇预分散，然后加水、海藻糖，加热至75℃并搅拌均匀，作为水相备用；
2)将配方量的霍霍巴油、乳木果油、鲸蜡基葡萄糖苷、橄榄油、小麦胚芽油、辛酸癸酸甘油酯、野大豆籽提取物、维生素E醋酸酯混合后加热至75℃，搅拌均匀作为油相备用；
3)将步骤2)制备的油相加入步骤1)制备的水相中，搅拌均匀后均质3分钟；
4)搅拌冷却至35～40℃，加入配方量的山茶花提取液、苯氧乙醇、乙基己基甘油、精油，搅拌均匀，出锅，检测合格后灌装。
实施例32：化妆品性能评价
采用Courage+Khazaka electronic GmbH(CK)公司的皮肤测试仪，分别对实施例15～20制备的化妆品进行皮肤外观及皱纹测试。
(一)、皮肤外观测试
护肤过程涉及多个步骤，护肤步骤一般为：洗脸，拍化妆水，拍乳液，凝露，涂面霜，睡前使用睡眠面膜，因此，需要使用本发明的实施例17～31的所有化妆品。现考察使用本发明的含有山茶花提取液的护肤品进行护肤前后的皮肤情况，分别对试验者使用前、使用45天及使用90天时进行拍照及红外线拍摄，如图5和图6所示。由图5和图6可以看
出，使用前试验者皮肤黑斑较多，肤色暗沉且肤色不均匀，使用一段时间后皮肤底层色素变得均匀，皮肤色斑明显减少，肤质变得匀称，说明以本发明的山茶花提取液为活性组分的化妆品具有优异的美白，淡斑功效。
(二)、皮肤皱纹测试
采用红外线拍摄对局部皮肤进行皱纹测试，测试结果如图7和图8所示，其中白色圈内表示皱纹。由图7和图8对比可以看出，使用含有山茶花提取液护肤品后，皮肤皱纹面积明显减少；仪器分析表明，使用前测试皮肤的皱纹面积比率为3.362％，使用后降低至1.430％，说明本发明的含有山茶花提取液的护肤品具有良好的抗衰老、抗皱纹功效。
本发明的上述化妆品单独使用或与其他化妆品搭配使用，同样具有美白、淡斑、抗衰老的功效。
以上对本发明的具体实施例进行了详细描述，但其只作为范例，本发明并不限制于以上描述的具体实施例。对于本领域技术人员而言，任何对该发明进行的等同修改和替代也都在本发明的范畴之中。因此，在不脱离本发明的精神和范围下所作的均等变换和修改，都应涵盖在本发明的范围内。
Claims (15)
- 一种山茶花提取液的制备方法，其特征在于，包括如下制备步骤：1)、新鲜山茶花和/或新鲜山茶花花蕾剔除杂质并切碎成小段，作为原料备用；2)、将一定量的原料置入超声釜中，加入与原料质量比为1:3～30的溶剂，搅拌均匀后加入一定量的无机酸和/或有机酸，调节pH值至1.3～3.0，浸泡10～30min；3)、然后超声处理30～60min，控制超声频率为20～25KHz，超声功率为1.0～2.0KW，超声温度为15～50℃，然后过滤，灭菌并检测，得到山茶花提取液。
- 如权利要求1所述的山茶花提取液的制备方法，其特征在于，所述步骤1)中的小段的长度为0.5～3cm。
- 如权利要求1所述的山茶花提取液的制备方法，其特征在于，所述步骤2)中的所述无机酸和/或有机酸的加入量为溶剂质量的0.25-2.5％。
- 如权利要求1所述的山茶花提取液的制备方法，其特征在于，所述步骤2)中的溶剂为水、乙醇、1,3-丙二醇、1,2-丙二醇、甘油、1,3-丁二醇和山梨醇中的一种或几种。
- 如权利要求1所述的山茶花提取液的制备方法，其特征在于，所述步骤2)中的无机酸为盐酸和乙酸中的一种或两种。
- 如权利要求1所述的山茶花提取液的制备方法，其特征在于，所述步骤2)中的有机酸为植酸、柠檬酸、抗坏血酸和乳酸中的一种或几种。
- 如权利要求1～6中任一项所述的制备方法得到的山茶花提取液。
- 如权利要求7所述的山茶花提取液，其特征在于，所述山茶花提取液含有如下抗氧化组分：山奈酚：0.43～4.52ppm，槲皮素：1.09～8.17ppm，槲皮苷：45.62～197.81ppm。
- 如权利要求7所述的山茶花提取液在制备以山茶花提取液为活性组分的化妆品中的应用。
- 如权利要求7所述的山茶花提取液在制备具有抗氧化功效的化妆品中的应用。
- 一种由权利要求7所述的山茶花提取液为活性组分制备的美白化妆水，其特征在于，由如下重量份的组分组成：山茶花提取液2.0～10.0份、植物舒敏剂1.0～3.0份、甘油2.0～5.0份、1,3-丁二醇2.0～6.0份、海藻糖0.2～5.0份、甜菜碱0.2～2.0份、银耳多糖0.005～0.4份、透明质酸钠0.005～0.2份、苯氧乙醇0.3～0.6份、乙基己基甘油0.1～0.3份、精油0.1～0.3份，余量的水。
- 一种由权利要求7所述的山茶花提取液为活性组分制备的抗衰老美白凝露，其特征在于，由如下重量份的组分组成：山茶花提取液1.0～10.0份、植物舒敏剂1.0～3.0份、甘油2.0～6.0份、1,3-丙二醇2.0～6.0份、海藻糖0.2～5.0份、甜菜碱0.2～2.0份、透明质酸钠0.005～0.2份，黄原胶0.5～1.0份、EDTA二钠0.05～0.20份、苯氧乙醇0.3～0.6份、乙基己基甘油0.1～0.3份、精油0.1～0.3份，余量的水。
- 一种由权利要求7所述的山茶花提取液为活性组分制备的抗衰老美白乳液，其特征在于，由如下重量份的组分组成：山茶花提取液1.0～8.0份、葡萄籽油5.0～11.0份、橄榄油7.0～12.0份、甘油2.0～6.0份、1,3-丙二醇2.0～6.0份、辛酸癸酸甘油酯1.5～4.0份、野大豆籽提取物0.5～1.0份、卡波姆0.2～0.8份、透明质酸钠0.005～0.1份、苯氧乙醇0.3～0.6份、乙基己基甘油0.1～0.3份、精油0.1～0.3份、氢氧化钠(33％溶液)0.2～0.8份，余量的水。
- 一种由权利要求7所述的山茶花提取液为活性组分制备的抗氧化美白睡眠面膜，其特征在于，由如下重量份的组分组成：山茶花提取液2.0～15.0份、甘油1.0～4.0份、1,3-丙二醇2.0～6.0份、1,3-丁二醇2.0～6.0份、海藻糖0.5～2.0份、银耳多糖0.005～0.3份、丙烯酰二甲基牛磺酸胺/VP共聚物0.4～0.9份、透明质酸钠0.005～0.2份、EDTA二钠0.05～0.2份、苯氧乙醇0.3～0.6份、乙基己基甘油0.1～0.3份、精油0.1～0.3份，余量的水。
- 一种由权利要求7所述的山茶花提取液为活性组分制备的抗氧化美白面霜，其特征在于，由如下重量份的组分组成：山茶花提取液2.0～6.0份、霍霍巴油5.0～12.0份、乳木果油4.0～8.0份、鲸蜡基葡萄糖苷2.5～6.0份、橄榄油1.0～5.0份、小麦胚芽油2.0～5.0份、甘油2.0～5.0份、1,3-丙二醇2.0～6.0份、辛酸癸酸甘油酯1.0～5.0份、海藻糖0.5～4.0份、野大豆籽提取物0.5～1.0份、维生素E醋酸酯0.05～0.5份、透明质酸钠0.005～0.1份、银耳多糖0.005～0.2份、苯氧乙醇0.3～0.6份、乙基己基甘油0.1～0.3份、精油0.1～0.3份，余量的水。
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| CN114028294A (zh) * | 2021-12-06 | 2022-02-11 | 中南民族大学 | 一种精华液、面膜及其制备方法 |
| CN116270340A (zh) * | 2023-02-13 | 2023-06-23 | 佛山市奥姿美生物科技有限公司 | 一种高效渗透的舒缓抗衰老组合物的制备方法及其应用 |
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