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CN106511198A - Sanguis Draconis extract, and preparation method and application thereof - Google Patents

Sanguis Draconis extract, and preparation method and application thereof Download PDF

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CN106511198A
CN106511198A CN201611080951.XA CN201611080951A CN106511198A CN 106511198 A CN106511198 A CN 106511198A CN 201611080951 A CN201611080951 A CN 201611080951A CN 106511198 A CN106511198 A CN 106511198A
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dragon
blood
extract
preparation
extraction
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邓玉林
戴荣继
孟薇薇
陈艳
李亚琼
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Beijing Institute of Technology BIT
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005Antimicrobial preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/74Biological properties of particular ingredients
    • A61K2800/78Enzyme modulators, e.g. Enzyme agonists
    • A61K2800/782Enzyme inhibitors; Enzyme antagonists

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Abstract

本发明公开了一种龙血竭提取物及其制备方法与应用。该龙血竭提取物的制备方法包括如下步骤:采用有机溶剂对龙血竭进行提取,所得提取液即为所述龙血竭提取物;所述有机溶剂为多元醇或白油。本发明克服了现有技术中采用乙醇、甲醇、丙酮、乙酸乙酯等有机溶剂提取龙血竭,提取物提取率不高或需浓缩后再添加于化妆品中,与化妆品基质相容性差,稳定性差、致敏性高等问题。本发明龙血竭提取物与化妆品基质相容性好,可直接添加于化妆品中;产品稳定性好,对于高温,低温,光照等恶劣条件都很稳定;提取率高,龙血竭原料损失少,达到了对龙血竭原料的最大化利用。另外,除了抗氧化、抗衰老作用,还具有显著的祛痘和美白作用。The invention discloses a dragon's blood extract, a preparation method and application thereof. The preparation method of the dragon's blood extract comprises the following steps: using an organic solvent to extract the dragon's blood, and the obtained extract is the dragon's blood extract; the organic solvent is polyhydric alcohol or white oil. The present invention overcomes the problems in the prior art of using organic solvents such as ethanol, methanol, acetone, and ethyl acetate to extract dragon's blood, and the extraction rate of the extract is not high or needs to be concentrated before being added to cosmetics, which has poor compatibility with the cosmetic base and is stable. Poor sex, high allergenicity and other issues. The dragon's blood extract of the present invention has good compatibility with the cosmetic matrix, and can be directly added to cosmetics; the product has good stability, and is stable against high temperature, low temperature, light and other harsh conditions; the extraction rate is high, and the loss of the dragon's blood raw material is small , reaching the maximum utilization of the raw material of dragon's blood. In addition, in addition to anti-oxidation and anti-aging effects, it also has significant acne-removing and whitening effects.

Description

一种龙血竭提取物及其制备方法与应用A kind of dragon's blood extract and its preparation method and application

技术领域technical field

本发明涉及一种中药提取物及其制备方法与应用,具体涉及一种龙血竭提取物及其制备方法与应用。The invention relates to a traditional Chinese medicine extract and its preparation method and application, in particular to a dragon's blood extract and its preparation method and application.

背景技术Background technique

龙血竭是百合科植物剑叶龙血树Dranaena cochinchinensis(Lour.)S.C.Chen的含脂木材经提取得到的树脂,主要产自广西和云南等地区。《本草纲目》记载其具有性温平,味甘咸,以及无毒等特性,主要功效为活血化瘀、收敛止血等。龙血竭的化学组成十分复杂,含黄酮类、简单酚类、甾体、萜类、烃类等多种类别化合物。Dracaena cochinchinensis (Lour.) S.C.Chen is a resin extracted from the lipid-containing wood of the Liliaceae plant, Dranaena cochinchinensis (Lour.) S.C. Chen. It is mainly produced in Guangxi and Yunnan. "Compendium of Materia Medica" records that it has the characteristics of warm and flat, sweet and salty, and non-toxic. Its main functions are promoting blood circulation, removing blood stasis, astringent and hemostasis. The chemical composition of dragon's blood is very complex, including flavonoids, simple phenols, steroids, terpenes, hydrocarbons and other types of compounds.

不同的工艺条件得到的龙血竭提取物中有效成分的含量不同,其药效用途均有差别,如CN 101559149 A中公开了一种龙血竭及龙血竭提取物用于制备辐射保护药物的用途,该龙血竭提取物是指龙血竭总酚和龙血竭总黄酮;CN 1857570 A公开了中药龙血竭黄酮类提取物的制备工艺方法,该提取物具有较强的α-葡萄糖苷酶抑制活性与促胰岛素分泌功能,可起到降血糖的作用。The contents of active ingredients in the extracts of dragon's blood obtained under different process conditions are different, and their medicinal effects and uses are all different. For example, CN 101559149 A discloses a kind of dragon's blood and its extracts for the preparation of radiation protection drugs The use of the dragon's blood extract refers to the total phenols of the dragon's blood and the total flavonoids of the dragon's blood; CN 1857570 A discloses a preparation process of the flavonoid extract of the traditional Chinese medicine dragon's blood, and the extract has a strong α- Glucosidase inhibitory activity and insulin secretion-stimulating function can play a role in lowering blood sugar.

在化妆品的研究和开发过程中,中药提取物作为功能添加剂,是制备具有特殊功效化妆品重要的物质基础。但是,由于这些化妆品生产所必需的各种中草药添加剂精制提取技术还不够完善、科技含量不高以及有效成分缺乏现代科学依据等原因,使得目前国内市场上销售的许多中药功能性化妆品使用效果不明显。已有/已报道的化妆品用龙血竭提取物的制备工艺也存在与化妆品基质相容性差,稳定性差、致敏性高、提取率低或需浓缩后再添加于化妆品等诸多问题。In the research and development process of cosmetics, traditional Chinese medicine extracts, as functional additives, are an important material basis for the preparation of cosmetics with special effects. However, due to the imperfect extraction technology of various Chinese herbal medicine additives necessary for the production of these cosmetics, the low technological content and the lack of modern scientific basis for active ingredients, many functional cosmetics of Chinese medicine currently sold in the domestic market have no obvious use effect. . The existing/reported preparation process of Dracaena extract for cosmetics also has many problems such as poor compatibility with cosmetic matrix, poor stability, high allergenicity, low extraction rate or need to be concentrated before adding to cosmetics.

发明内容Contents of the invention

本发明的目的是提供一种龙血竭提取物及其制备方法与应用,该方法采用多元醇或白油为有机溶剂,提取率高,制备得到的龙血竭提取物对人体肌肤刺激性小,致敏性低,与化妆品基质相容性好,稳定性好,并具有抗菌、祛痘、抗氧化、抗衰老、美白的功效。The object of the present invention is to provide a dragon's blood extract and its preparation method and application. The method uses polyol or white oil as an organic solvent, and the extraction rate is high, and the prepared dragon's blood extract is less irritating to human skin , low allergenicity, good compatibility with cosmetic matrix, good stability, and has antibacterial, anti-acne, anti-oxidation, anti-aging, whitening effects.

本发明提供的龙血竭提取物的制备方法,它包括如下步骤:采用有机溶剂对龙血竭进行提取,所得提取液即为所述龙血竭提取物;所述有机溶剂为多元醇或白油。The preparation method of the dragon's blood extract provided by the invention comprises the following steps: using an organic solvent to extract the dragon's blood, and the obtained extract is the dragon's blood extract; the organic solvent is a polyhydric alcohol or white Oil.

上述的制备方法中,所述龙血竭可为龙血竭原料药;所述龙血竭的粒径可为10目~200目,具体可为40~60目、60~100目、50~80目、40目、50目、60目、80目或100目。In the above preparation method, the dragon's blood can be the raw material drug of dragon's blood; the particle size of the dragon's blood can be 10 mesh to 200 mesh, specifically 40 to 60 mesh, 60 to 100 mesh, 50 to 100 mesh. 80 mesh, 40 mesh, 50 mesh, 60 mesh, 80 mesh or 100 mesh.

上述的制备方法中,所述多元醇优选化妆品中使用的,对肌肤刺激性小的多元醇,如1-2-丙二醇、1,3-丙二醇、1,3-丁二醇、丙三醇等。In the above-mentioned preparation method, the polyol is preferably used in cosmetics and is less irritating to the skin, such as 1-2-propanediol, 1,3-propanediol, 1,3-butanediol, glycerin, etc. .

上述的制备方法中,所述白油的牌号可为15#或26#。所述牌号根据40℃运动粘度的大小来划分。In the above-mentioned preparation method, the grade of the white oil can be 15# or 26#. The grades are classified according to the kinematic viscosity at 40°C.

上述的制备方法中,所述提取可为浸渍提取或回流提取;所述浸渍提取的具体步骤如下:在所述龙血竭中加入所述有机溶剂进行浸泡,经过滤后,收集滤液即可得到所述龙血竭提取物。In the above preparation method, the extraction can be immersion extraction or reflux extraction; the specific steps of the immersion extraction are as follows: add the organic solvent to the dragon's blood for soaking, and after filtering, collect the filtrate to obtain The dragon's blood extract.

上述的制备方法中,每1g所述龙血竭中加入1~1000g所述有机溶剂即料液比可为1:(1~1000),具体可为每1g所述龙血竭中加入20~500g、20~200g、20~100g、20~50g、50~500g、50~200g、50~100g、100~500g、100~200g、200~500g、20g、50g、100g、200g或500g所述有机溶剂,即料液比具体可为1:(20~500)、1:(20~200)、1:(20~100)、1:(20~50)、1:(50~500)、1:(50~200)、1:(50~100)、1:(100~500)、1:(100~200)、1:(200~500)、1:20、1:50、1:100、1:200或1:500。In the above preparation method, 1-1000 g of the organic solvent is added to every 1 g of the dragon's blood, that is, the solid-liquid ratio can be 1: (1-1000), specifically, 20-100 g of the above-mentioned dragon's blood can be added to each 1 g of the dragon's blood. The organic Solvent, that is, the ratio of solid to liquid can be 1: (20-500), 1: (20-200), 1: (20-100), 1: (20-50), 1: (50-500), 1 :(50~200), 1:(50~100), 1:(100~500), 1:(100~200), 1:(200~500), 1:20, 1:50, 1:100 , 1:200 or 1:500.

上述的制备方法中,所述提取的温度可为25~180℃,具体可为80~150℃、80~95℃、80~100℃、80~110℃、95~150℃、95~110℃、95~100℃、100~110℃、100~150℃、110~150℃、80℃、95℃、100℃、110℃或150℃,每次提取的时间可为10~1440分钟,具体可为30~120分钟、30~60分钟、30~90分钟、60~90分钟、60~120分钟、90~120分钟、30分钟、60分钟、90分钟或120分钟。In the above preparation method, the extraction temperature can be 25-180°C, specifically 80-150°C, 80-95°C, 80-100°C, 80-110°C, 95-150°C, 95-110°C , 95-100°C, 100-110°C, 100-150°C, 110-150°C, 80°C, 95°C, 100°C, 110°C or 150°C, the time for each extraction can be 10-1440 minutes. 30 to 120 minutes, 30 to 60 minutes, 30 to 90 minutes, 60 to 90 minutes, 60 to 120 minutes, 90 to 120 minutes, 30 minutes, 60 minutes, 90 minutes or 120 minutes.

上述的制备方法中,所述提取的次数可为1~3次,具体可为1~2次、2~3次、1次、2次或3次。In the above preparation method, the number of extractions may be 1-3 times, specifically 1-2 times, 2-3 times, 1 time, 2 times or 3 times.

由上述的制备方法制备得到的龙血竭提取物,也在本发明的保护范围内。该龙血竭提取物中龙血竭总酚的质量百分含量为0.01~25%。The dragon's blood extract prepared by the above preparation method is also within the protection scope of the present invention. The mass percent content of total phenols in the dragon's blood extract is 0.01-25%.

上述龙血竭提取物在直接作为具有下述1)-8)中的至少一种功能的产品中的应用或在制备具有下述1)-8)中至少一种功能的产品中的应用,也在本发明的保护范围内:The above-mentioned dragon's blood extract is used directly as a product with at least one function in the following 1)-8) or in the preparation of a product with at least one function in the following 1)-8), Also within the protection scope of the present invention:

1)抑制痤疮致病菌;1) Inhibit acne pathogenic bacteria;

2)祛痘;2) acne;

3)清除DPPH自由基;3) Scavenge DPPH free radicals;

4)清除ABTS自由基;4) Remove ABTS free radicals;

5)抗氧化;5) anti-oxidation;

6)抗衰老;6) anti-aging;

7)抑制酪氨酸酶的活性;7) inhibit the activity of tyrosinase;

8)美白。8) Whitening.

上述的应用中,所述产品具体可为化妆品,所述化妆品可以是膏霜状、凝胶状或水剂状等多种能被人接受的制剂形式。In the above-mentioned applications, the product may be cosmetics, and the cosmetics may be in the form of various acceptable preparations such as cream, gel or water.

本发明龙血竭提取物与化妆品基质相容性好,可直接添加于化妆品中,无论添加到水剂、凝胶还是膏霜中,都没有降粘、破乳等情况出现,除了抗氧化、抗衰老作用,还具有显著的祛痘和美白作用。The dragon's blood extract of the present invention has good compatibility with cosmetic bases, and can be directly added to cosmetics. No matter it is added to water, gel or cream, there is no viscosity reduction or demulsification. In addition to anti-oxidation, Anti-aging effect, also has significant acne and whitening effect.

本发明具有如下有益效果:The present invention has following beneficial effect:

本发明克服了现有技术中采用乙醇、甲醇、丙酮、乙酸乙酯等有机溶剂(非化妆品常用溶剂)提取龙血竭,提取物提取率不高或需浓缩后再添加于化妆品中,与化妆品基质相容性差,稳定性差、致敏性高等问题。The present invention overcomes the use of organic solvents such as ethanol, methanol, acetone, and ethyl acetate (non-commonly used solvents for cosmetics) to extract dragon's blood in the prior art, and the extraction rate of the extract is not high or needs to be concentrated before being added to cosmetics. Poor matrix compatibility, poor stability, high allergenicity and other issues.

本发明龙血竭提取物与化妆品基质相容性好,可直接添加于化妆品中,无论添加到水剂、凝胶还是膏霜中,都没有降粘、破乳等情况出现;产品稳定性好,对于高温,低温,光照等恶劣条件都很稳定;提取率高(达到95%以上),龙血竭原料损失少,达到了对龙血竭原料的最大化利用。另外,除了抗氧化、抗衰老作用,还具有显著的祛痘和美白作用。The dragon's blood extract of the present invention has good compatibility with cosmetic bases, and can be directly added to cosmetics. No matter it is added to water, gel or cream, there is no viscosity reduction or demulsification; the product has good stability. , is very stable against harsh conditions such as high temperature, low temperature, and light; the extraction rate is high (reaching more than 95%), and the raw material loss of dragon's blood is small, and the maximum utilization of the raw material of dragon's blood is reached. In addition, in addition to anti-oxidation and anti-aging effects, it also has significant acne-removing and whitening effects.

具体实施方式detailed description

下述实施例中所使用的实验方法如无特殊说明,均为常规方法。The experimental methods used in the following examples are conventional methods unless otherwise specified.

下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。The materials and reagents used in the following examples can be obtained from commercial sources unless otherwise specified.

卡伯U20(Carbopol Ultrez 20聚合物),INCI名称:Acrylates/C10-30AlkylAcrylate Crosspolymer。Carbopol U20 (Carbopol Ultrez 20 polymer), INCI name: Acrylates/C10-30 AlkylAcrylate Crosspolymer.

MTI为购自广东中鹏化工有限公司的产品,产品名称为MTI化妆品防腐剂,其活性组分为甲基异噻唑啉酮、碘丙炔基丁基甲铵酸脂。MTI is a product purchased from Guangdong Zhongpeng Chemical Co., Ltd., the product name is MTI cosmetic preservative, and its active components are methylisothiazolinone and iodopropynyl butyl carbamate.

NMF-50,化学名称为三甲基甘氨酸。NMF-50, the chemical name is trimethylglycine.

HEC(Hydroxyethyl Cellulose),化学名称为羟乙基纤维素,规格为羟乙基纤维素HHR250。HEC (Hydroxyethyl Cellulose), the chemical name is hydroxyethyl cellulose, and the specification is hydroxyethyl cellulose HHR250.

DM100,化学名称为聚二甲基硅氧烷。DM100, the chemical name is polydimethylsiloxane.

混醇,化学名称为十六十八醇。Mixed alcohol, the chemical name is cetostearyl alcohol.

LGP为购自广东中鹏化工有限公司的产品,产品名称为LGP化妆品防腐剂,活性成分为DMDM乙内酰脲、甲基异噻唑啉酮(MIT)、碘丙炔醇丁基氨甲酸酯(IPBC)LGP is a product purchased from Guangdong Zhongpeng Chemical Co., Ltd., the product name is LGP cosmetic preservative, and the active ingredients are DMDM hydantoin, methylisothiazolinone (MIT), iodopropynyl butylcarbamate (IPBC)

透明汉生胶,化学名称为黄原胶。Transparent xanthan gum, the chemical name is xanthan gum.

下述实施例中,龙血竭提取物中总酚含量的测定方法如下:In the following examples, the assay method of total phenolic content in the extract of Dragon's blood is as follows:

a.对照品溶液制备a. Preparation of reference substance solution

精密称量龙血素B标准品8.82mg,置于100mL容量瓶中,加无水乙醇定容,摇匀,即得龙血素B含量为0.0882mg/ml的溶液。Precisely weigh 8.82 mg of the standard product of dragon blood B, place it in a 100 mL volumetric flask, add absolute ethanol to constant volume, and shake well to obtain a solution with the content of dragon blood B of 0.0882 mg/ml.

b.标准曲线绘制b. Standard curve drawing

取龙血素B对照品(0.0882mg/ml)0.5、0.6、0.75、1.0、1.3、1.5ml,分别置于10ml容量瓶中,加无水乙醇定容,摇匀。以无水乙醇做空白,在选定波长280nm下测定吸光度。以吸收度为横坐标,对照品浓度C(mg/mL)为纵坐标,绘制标准曲线。Take 0.5, 0.6, 0.75, 1.0, 1.3, and 1.5ml of the reference substance of ascarin B (0.0882mg/ml), place them in 10ml volumetric flasks, add absolute ethanol to volume, and shake well. Absorbance was measured at a selected wavelength of 280 nm with absolute ethanol as a blank. With absorbance as the abscissa and reference substance concentration C (mg/mL) as the ordinate, draw a standard curve.

c.总酚含量测定c. Determination of total phenol content

精密取样品配制成适宜浓度溶液,在选定波长280nm下测定吸收度,根据建立的标准曲线进行总酚含量的计算。Precisely take samples to prepare a suitable concentration solution, measure the absorbance at a selected wavelength of 280nm, and calculate the total phenol content according to the established standard curve.

下述实施例中龙血竭提取液得率根据龙血竭提取液总酚含量、投料量以及提取后提取液总量进行计算。计算公式如下:In the following examples, the yield of dragon's blood extract is calculated according to the total phenol content of the dragon's blood extract, the feeding amount and the total amount of the extract after extraction. Calculated as follows:

式(1)中,各物理量代表的含义及单位如下:In formula (1), the meanings and units of each physical quantity are as follows:

C:提取液总酚含量,mg/mLC: total phenol content of the extract, mg/mL

V:提取液总体积,mLV: total volume of extract, mL

M:制作提取液使用的龙血竭原药中总酚的质量,g。M: the mass of total phenols in the raw drug of dragon's blood used in making the extract, g.

实施例1、制备龙血竭提取物Embodiment 1, preparation dragon's blood extract

将龙血竭粉碎至60目,按照1:50的比例(质量比)加入1,2-丙二醇,在95℃下浸泡1小时,提取完成之后,用过滤纸板过滤,所得滤液即为龙血竭提取物。Crush dragon's blood to 60 mesh, add 1,2-propanediol according to the ratio (mass ratio) of 1:50, soak at 95°C for 1 hour, after the extraction is completed, filter with filter paper, and the obtained filtrate is dragon's blood Extract.

本实施例中,料液比为1:50,提取温度为95℃,时间为1小时,提取次数为1次。所得提取液总酚含量为0.91%,提取率为95%。In this example, the ratio of solid to liquid is 1:50, the extraction temperature is 95° C., the extraction time is 1 hour, and the extraction frequency is 1 time. The total phenol content of the obtained extract is 0.91%, and the extraction rate is 95%.

实施例2、制备龙血竭提取物Embodiment 2, preparation dragon's blood extract

将龙血竭粉碎至100目,按照1:20的比例(质量比)加入1,3-丙二醇,在80℃下浸泡1.5小时,提取完成后,用过滤纸板过滤,收集滤液,将得到的滤渣重复上次操作,合并所有滤液即为龙血竭提取物。Crush dragon's blood to 100 mesh, add 1,3-propanediol according to the ratio (mass ratio) of 1:20, soak at 80°C for 1.5 hours, after the extraction is completed, filter with filter paper, collect the filtrate, and filter Repeat the last operation, and combine all the filtrates to obtain the dragon's blood extract.

本实施例中,料液比为1:20,提取温度为80℃,时间为1.5小时,提取次数为2次。所得提取液总酚含量为1.2%,提取率为96%。In this example, the ratio of solid to liquid is 1:20, the extraction temperature is 80°C, the extraction time is 1.5 hours, and the extraction frequency is 2 times. The total phenol content of the obtained extract is 1.2%, and the extraction rate is 96%.

实施例3、制备龙血竭提取物Embodiment 3, preparation dragon's blood extract

将龙血竭粉碎至40目,按照1:100的比例(质量比)加入1,3-丁二醇,在100℃下浸泡0.5小时,提取完成之后,用过滤纸板过滤,所得滤液即为龙血竭提取物。Crush dragon's blood to 40 mesh, add 1,3-butanediol according to the ratio (mass ratio) of 1:100, soak at 100°C for 0.5 hours, after the extraction is completed, filter with filter paper, and the obtained filtrate is dragon Blood extract.

本实施例中,料液比为1:100,提取温度为100℃,时间为0.5小时,提取次数为1次。所得提取液总酚含量为0.32%,提取率为92%。In this example, the ratio of solid to liquid is 1:100, the extraction temperature is 100° C., the extraction time is 0.5 hour, and the extraction frequency is 1 time. The total phenol content of the obtained extract was 0.32%, and the extraction rate was 92%.

实施例4、制备龙血竭提取物Embodiment 4, preparation dragon's blood extract

将龙血竭粉碎至80目,按照1:200的比例(质量比)加入丙三醇,在110℃下浸泡1.5小时,提取完成后,用过滤纸板过滤,收集滤液;将得到的滤渣重复上述操作,合并滤液即为龙血竭提取物。Crush dragon's blood to 80 mesh, add glycerol according to the ratio (mass ratio) of 1:200, soak at 110°C for 1.5 hours, after the extraction is completed, filter with filter paper to collect the filtrate; repeat the above steps for the obtained filter residue Operation, the combined filtrate is the dragon's blood extract.

本实施例中,料液比为1:200,提取温度为110℃,时间为1.5小时,提取次数为2次。所得提取液总酚含量为0.10%,提取率为90%。In this example, the ratio of solid to liquid is 1:200, the extraction temperature is 110° C., the extraction time is 1.5 hours, and the extraction frequency is 2 times. The total phenol content of the obtained extract is 0.10%, and the extraction rate is 90%.

实施例5、制备龙血竭提取物Embodiment 5, preparation dragon's blood extract

将龙血竭粉碎至50目,按照1:500的比例(质量比)加入15#白油,在150℃下浸泡2小时,提取完成之后,用过滤纸板过滤,收集滤液;将得到的滤渣重复上述操作,所得滤渣再次重复上述操作,合并所有滤液即为龙血竭提取物。Crush dragon's blood to 50 mesh, add 15# white oil according to the ratio (mass ratio) of 1:500, soak at 150°C for 2 hours, after the extraction is completed, filter with filter paper to collect the filtrate; repeat the obtained filter residue The above operation, the obtained filter residue repeats the above operation again, and all the filtrates are combined to obtain the dragon's blood extract.

本实施例中,料液比为1:500,提取温度为150℃,时间为2小时,提取次数为3次。所得提取液总酚含量为0.03%,提取率为85%。In this example, the ratio of solid to liquid is 1:500, the extraction temperature is 150° C., the extraction time is 2 hours, and the extraction frequency is 3 times. The total phenol content of the obtained extract is 0.03%, and the extraction rate is 85%.

实施例6、龙血竭提取物在制备化妆品中的应用Embodiment 6, the application of dragon's blood extract in the preparation of cosmetics

(1)龙血竭提取物稳定性试验(1) Stability test of dragon's blood extract

取实施例1中制得的龙血竭提取物100g分别装于四个透明样品瓶中置于不同环境下,定期取四瓶样品同时观察状态。四瓶样品分别放置于室内阳光照射处,38度培养箱中,-20度冰箱冷冻室,室温阴凉处,于一周,两周,一个月时间分别观察其状态变化极小,表明龙血竭提取物具有很好的稳定性。Get 100 g of the dragon's blood extract prepared in Example 1 and put them in four transparent sample bottles respectively and place them in different environments, and take four bottles of samples regularly to observe the state simultaneously. The four bottles of samples were placed in a sunny place indoors, in a 38-degree incubator, in a -20-degree refrigerator freezer, and in a cool place at room temperature. After one week, two weeks, and one month, the state changes were observed to be minimal, indicating that the extraction of dragon's blood material has good stability.

取实施例2中制的的龙血竭提取物100g分别装于四个透明样品瓶中置于不同环境下,定期取四瓶样品同时观察状态。四瓶样品分别放置于室内阳光照射处,38度培养箱中,-20度冰箱冷冻室,室温阴凉处,于一周,两周,一个月时间分别观察其状态变化极小,表明龙血竭提取物具有很好的稳定性。Get 100 g of the dragon's blood extract prepared in Example 2 and put them in four transparent sample bottles respectively under different environments, and regularly take four bottles of samples to observe the state simultaneously. The four bottles of samples were placed in a sunny place indoors, in a 38-degree incubator, in a -20-degree refrigerator freezer, and in a cool place at room temperature. After one week, two weeks, and one month, the state changes were observed to be minimal, indicating that the extraction of dragon's blood material has good stability.

取实施例3中制的的龙血竭提取物100g分别装于四个透明样品瓶中置于不同环境下,定期取四瓶样品同时观察状态。四瓶样品分别放置于室内阳光照射处,38度培养箱中,-20度冰箱冷冻室,室温阴凉处,于一周,两周,一个月时间分别观察其状态变化极小,表明龙血竭提取物具有很好的稳定性。Get 100 g of the dragon's blood extract prepared in Example 3 and put them in four transparent sample bottles respectively under different environments, and regularly take four bottles of samples to observe the state simultaneously. The four bottles of samples were placed in a sunny place indoors, in a 38-degree incubator, in a -20-degree refrigerator freezer, and in a cool place at room temperature. After one week, two weeks, and one month, the state changes were observed to be minimal, indicating that the extraction of dragon's blood material has good stability.

取实施例4中制的的龙血竭提取物100g分别装于四个透明样品瓶中置于不同环境下,定期取四瓶样品同时观察状态。四瓶样品分别放置于室内阳光照射处,38度培养箱中,-20度冰箱冷冻室,室温阴凉处,于一周,两周,一个月时间分别观察其状态变化极小,表明龙血竭提取物具有很好的稳定性。Get 100 g of the dragon's blood extract prepared in Example 4 and put them in four transparent sample bottles respectively under different environments, and take four bottles of samples regularly to observe the state simultaneously. The four bottles of samples were placed in a sunny place indoors, in a 38-degree incubator, in a -20-degree refrigerator freezer, and in a cool place at room temperature. After one week, two weeks, and one month, the state changes were observed to be minimal, indicating that the extraction of dragon's blood material has good stability.

取实施例5中制的的龙血竭提取物100g分别装于四个透明样品瓶中置于不同环境下,定期取四瓶样品同时观察状态。四瓶样品分别放置于室内阳光照射处,38度培养箱中,-20度冰箱冷冻室,室温阴凉处,于一周,两周,一个月时间分别观察其状态变化极小,表明龙血竭提取物具有很好的稳定性。Get 100 g of the dragon's blood extract prepared in Example 5 and put them in four transparent sample bottles respectively under different environments, and take four bottles of samples regularly to observe the state simultaneously. The four bottles of samples were placed in a sunny place indoors, in a 38-degree incubator, in a -20-degree refrigerator freezer, and in a cool place at room temperature. After one week, two weeks, and one month, the state changes were observed to be minimal, indicating that the extraction of dragon's blood material has good stability.

(2)龙血竭提取物的体外抑菌试验(2) In vitro antibacterial test of dragon's blood extract

选择痤疮致病菌,痤疮丙酸杆菌和金黄色葡萄球菌作为测试菌种。痤疮丙酸杆菌Propionibacterium acnes的ATCC编号为10312,公众可从ATCC购买得到。金黄色葡萄球菌Staphylococcus aureus的ATCC编号为10384,公众可从ATCC购买得到。The acne pathogenic bacteria, Propionibacterium acnes and Staphylococcus aureus, were selected as test strains. Propionibacterium acnes has the ATCC number 10312 and is commercially available from the ATCC. Staphylococcus aureus has ATCC number 10384 and is commercially available from ATCC.

配置含菌约1×106CFU/mL的菌悬液。将滤纸剪切为直径6mm圆片并经160℃干热灭菌2h,用无菌镊子分别将滤纸片放入抑菌原液(实施例1-实施例5所制备得到的龙血竭提取物)中浸泡1h后取出。分别取0.2mL菌悬液于对应无菌已凝固培养基中,用无菌玻璃三角筢均匀进行涂布为含菌平板,将浸泡好的滤纸片置于平皿中央,并作空白对照,进行三组平行试验,放入厌氧或生化培养箱中37℃培养24小时。Prepare a bacterial suspension containing approximately 1×10 6 CFU/mL of bacteria. Cut the filter paper into discs with a diameter of 6mm and sterilize them by dry heat at 160°C for 2 hours, and put the filter paper into the antibacterial stock solution (the extract of dragon’s blood prepared in Example 1-Example 5) with sterile tweezers Take out after soaking for 1 hour. Take 0.2mL of bacterial suspension in the corresponding sterile solidified medium, and use a sterile glass triangle to evenly spread it into a flat plate containing bacteria, place the soaked filter paper in the center of the plate, and use it as a blank control, and carry out three Groups of parallel experiments were placed in an anaerobic or biochemical incubator at 37°C for 24 hours.

取出观察抑菌圈,结果如表1所示。抑菌圈的出现证明龙血竭提取物分别对痤疮丙酸杆菌和金黄色葡萄球菌有一定的抑制作用,抑菌圈直径越大,抑菌活性越强。Take out and observe the inhibition zone, the results are shown in Table 1. The appearance of the antibacterial zone proves that the extract of dragon's blood has a certain inhibitory effect on Propionibacterium acnes and Staphylococcus aureus, and the larger the diameter of the antibacterial zone, the stronger the antibacterial activity.

表1、龙血竭提取液抑菌圈数据表Table 1. Data table of antibacterial zone of dragon's blood extract

注:“<6”表示没有抑菌圈。Note: "<6" means no inhibition zone.

(3)龙血竭提取物的抗氧化功效评价(3) Antioxidant efficacy evaluation of dragon's blood extract

1)DPPH自由基清除能力测定1) Determination of DPPH free radical scavenging ability

DPPH是一种早期合成的有机自由基,常用来评估抗氧化物的供氢能力,它在有机溶剂中非常稳定,呈紫色,而且在517nm处有一个特征吸收峰,当遇到自由基清除剂时,DPPH的孤对电子被配对而使其退色,也就是在最大吸收波长处的吸光值变小。因此,可通过测定吸光值的变化来评价样品对DPPH自由基的清除效果。DPPH is an early synthesized organic free radical, which is often used to evaluate the hydrogen-donating ability of antioxidants. It is very stable in organic solvents, it is purple in color, and has a characteristic absorption peak at 517nm. When it encounters a free radical scavenger When , the lone pair of electrons of DPPH is paired to make it fade, that is, the light absorption value at the maximum absorption wavelength becomes smaller. Therefore, the scavenging effect of the sample on DPPH free radicals can be evaluated by measuring the change of the absorbance value.

待测液:将实施例1-实施例5中制备得到的龙血竭原液分别用无菌水配制含0.30%原液的稀释液。采用无菌水作为空白对照、15μg/mL维生素C溶液作为对照。Solution to be tested: use sterile water to prepare dilutions containing 0.30% of the stock solution of Dracaena jacquardii stock solution prepared in Examples 1-5. Sterile water was used as the blank control, and 15 μg/mL vitamin C solution was used as the control.

取0.1mL的待测液与5.8mL DPPH溶液混匀为A;取0.2mL的无水乙醇与5.8mL DPPH溶液混匀为B;取5.8mL的无水乙醇与0.2mL的待测液混匀为C;反应30min后,在517nm下分别测定A、B、C的吸光度值。Mix 0.1mL of the solution to be tested with 5.8mL of DPPH solution to form A; mix 0.2mL of absolute ethanol with 5.8mL of DPPH solution to form B; mix 5.8mL of absolute ethanol with 0.2mL of the solution to be tested It is C; after reacting for 30 minutes, measure the absorbance values of A, B, and C respectively at 517 nm.

计算方法: Calculation method:

不同实施例制备得到的的龙血竭提取物稀释得到的0.3%龙血竭提取液及对照对DPPH自由基清除率如表3所示。Table 3 shows the scavenging rate of 0.3% dragon's blood extract obtained by diluting the dragon's blood extract prepared in different examples and the control to DPPH free radicals.

表3、龙血竭提取液DPPH自由基清除率Table 3. DPPH free radical scavenging rate of dragon's blood extract

2)ABTS自由基清除能力测定2) Determination of ABTS free radical scavenging ability

ABTS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测定ABTS的吸光度即可测定并计算出样品的总抗氧化能力。ABTS is oxidized to green ABTS+ under the action of an appropriate oxidant, and the production of ABTS+ will be inhibited in the presence of antioxidants. The total antioxidant capacity of the sample can be determined and calculated by measuring the absorbance of ABTS at 734nm.

向A组试管依次加入500μL待测液,将500μL乙醇水溶液加入B组试管,加完试剂及时盖帽,涡旋混匀。将500μL ABTS自由基储备溶液依次加入A试管和B试管中,加完试剂及时盖帽,涡旋混匀。反应10min后在734nm检测吸光值。向C组试管依次加入500μL待测液和500μL乙醇水溶液涡旋混匀,734nm处测吸光值。Add 500 μL of the test solution to the test tubes of group A in turn, add 500 μL of ethanol aqueous solution to the test tubes of group B, cover the caps in time after adding the reagents, and vortex to mix. Add 500 μL of ABTS free radical stock solution to test tube A and test tube B in turn, cover the cap in time after adding the reagent, and vortex to mix. After 10 min of reaction, the absorbance was detected at 734 nm. Add 500 μL of the solution to be tested and 500 μL of ethanol aqueous solution to the test tubes of group C in sequence, vortex and mix well, and measure the absorbance at 734 nm.

计算方法: Calculation method:

待测液:将实施例1-实施例5制备得到的龙血竭原液采用无菌水分别配制为0.10%的稀释度。采用无菌水作为空白对照。采用0.001%维生素C溶液作为对照。Solution to be tested: the Dracaena dracaena stock solutions prepared in Examples 1-5 were prepared with sterile water to a dilution of 0.10%. Sterile water was used as blank control. A 0.001% vitamin C solution was used as a control.

不同实施例制备得到的龙血竭提取物稀释得到的0.10%的龙血竭提取液及对照对ABTS自由基清除率如表4所示。Table 4 shows the scavenging rate of ABTS free radicals of the 0.10% Dracaena extract obtained by diluting the Dracaena extract prepared in different examples and the control.

表4、龙血竭提取液ABTS自由基清除率Table 4. ABTS free radical scavenging rate of dragon's blood extract

通过以上实验数据可知,龙血竭提取物具有较强的抗氧化能力,可清除自由基,促进细胞代谢,增强细胞活力,改善机体的结构和功能,提高机体生命力,从而延缓细胞老化,发挥其抗衰老的作用。From the above experimental data, it can be seen that the extract of dragon's blood has strong antioxidant capacity, can scavenge free radicals, promote cell metabolism, enhance cell vitality, improve the structure and function of the body, and increase the vitality of the body, thereby delaying cell aging and exerting its potential. Anti-aging effect.

(4)龙血竭提取物的美白作用(4) Whitening effect of dragon's blood extract

酪氨酸酶属氧化还原酶,是黑色素合成的主要限速酶,其活性大小决定黑色素形成的数量,目前市场上销售的许多美白、祛斑产品都是以抑制酪氨酸酶活性达到美白作用,故对酪氨酸酶抑制作用的强弱是评价增白化妆品的主要指标。Tyrosinase is an oxidoreductase, which is the main rate-limiting enzyme for melanin synthesis. Its activity determines the amount of melanin formed. Many whitening and freckle products currently on the market achieve whitening effects by inhibiting tyrosinase activity. Therefore, the strength of the inhibitory effect on tyrosinase is the main indicator for evaluating whitening cosmetics.

L-酪氨酸在酪氨酸酶的作用下生成多巴,多巴被酪氨酸酶进一步作用生成多巴醌,最后经过一系列生化过程生成黑色素。其中多巴醌在475nm波长处有最大吸收峰,通过单位时间内,测定其吸光度,间接反应酶的活力大小,经过计算得到酪氨酸酶的抑制率。L-tyrosine generates dopa under the action of tyrosinase, and dopa is further acted by tyrosinase to generate dopaquinone, and finally melanin is generated through a series of biochemical processes. Among them, dopaquinone has a maximum absorption peak at a wavelength of 475nm, and its absorbance is measured per unit time, and the activity of the indirect reaction enzyme is calculated to obtain the inhibition rate of tyrosinase.

实验分为四组,在各组中按照表5中组分用量准确加入磷酸缓冲液、L-酪氨酸酶溶液及待测液,混匀,于37℃保温10min。The experiment was divided into four groups. In each group, phosphate buffer solution, L-tyrosinase solution and test solution were accurately added according to the dosage of the components in Table 5, mixed evenly, and kept at 37°C for 10 minutes.

磷酸盐缓冲液:称取71.63gNa2HPO4·12H2O,用去离子充分溶解定容于1000mL容量瓶中,配制成0.2mol/LNa2HPO4溶液;称取31.20g NaH2PO4·2H2O,用去离子水充分溶解定容于1000mL容量瓶中,配制成0.2mol/LNaH2PO4溶液;两者按照1:1比例混合,配制成pH值为6.8的磷酸盐缓冲液。酪氨酸酶溶液:按照酶活力单位为200U/mL称量一定量的酪氨酸酶,用磷酸盐缓冲液溶解,定容于所需体积的容量瓶中,存于冰箱中备用。其中,在温度为25℃,pH为6.5,波长为280nm时,每分钟引起吸光度下降0.001为一个活力单位(U)。Phosphate buffer solution: Weigh 71.63g Na 2 HPO 4 12H 2 O, fully dissolve it with deionization and set the volume in a 1000mL volumetric flask, and prepare a 0.2mol/L Na 2 HPO 4 solution; weigh 31.20g NaH 2 PO 4 . 2H 2 O was fully dissolved in deionized water and settled in a 1000mL volumetric flask to prepare a 0.2mol/L NaH 2 PO 4 solution; the two were mixed at a ratio of 1:1 to prepare a phosphate buffer solution with a pH value of 6.8. Tyrosinase solution: Weigh a certain amount of tyrosinase according to the enzyme activity unit of 200U/mL, dissolve it in phosphate buffer, dilute it in a volumetric flask of required volume, and store it in the refrigerator for later use. Among them, when the temperature is 25°C, the pH is 6.5, and the wavelength is 280nm, the decrease of absorbance by 0.001 per minute is an activity unit (U).

在A组和C组中加入酪氨酸酶溶液混匀,反应10min,反应结束后立即在475nm出测定四组吸光度值。Add tyrosinase solution to group A and group C and mix well, react for 10 minutes, measure the absorbance value of four groups at 475nm immediately after the reaction.

表5、测试液组分用量表Table 5, test solution component dosage table

计算方法: Calculation method:

待测液:将实施例1-5制备得到的龙血竭提取物原液分别用无菌水配制含1.0%原液的稀释液。采用无菌水作为空白对照。采用0.1%熊果苷溶液作为对照。Solution to be tested: the stock solution of Dracaena japonicus extract prepared in Examples 1-5 was respectively prepared with sterile water into dilutions containing 1.0% of the stock solution. Sterile water was used as blank control. A 0.1% arbutin solution was used as a control.

不同实施例制备得到的龙血竭提取物稀释得到的1.0%龙血竭提取液及对照对酪氨酸酶的抑制率如表6所示。Table 6 shows the tyrosinase inhibition rate of the 1.0% dragon's blood extract obtained by diluting the dragon's blood extract prepared in different examples and the control.

表6、龙血竭提取液酪氨酸酶抑制率Table 6. Inhibition rate of tyrosinase in dragon's blood extract

由上述结果可以看出,在化妆品的适宜添加浓度范围内,龙血竭提取液呈现出很好的酪氨酸酶抑制能力,龙血竭提取液是一款优秀的植物天然美白成分。It can be seen from the above results that within the appropriate concentration range of cosmetics, the extract of dragon's blood exhibits good tyrosinase inhibitory ability, and the extract of dragon's blood is an excellent plant natural whitening ingredient.

(5)龙血竭提取物的安全性评价(5) Safety evaluation of dragon's blood extract

1)毒理学检测(皮肤刺激性试验)1) Toxicology testing (skin irritation test)

本实验采用5%龙血竭提取液(分别由实施例1-5中制备得到的龙血竭提取物原液采用无菌水稀释得到)作为测试品,根据《化妆品卫生规范》2007版要求进行皮肤刺激性试验,实验结果见表7所示。In this experiment, 5% dragon's blood extract (respectively obtained by diluting the stock solution of dragon's blood extract prepared in Examples 1-5 with sterile water) was used as a test product, and skin Stimulation test, the experimental results are shown in Table 7.

表7、皮肤刺激性试验数据(实施例1)Table 7, skin irritation test data (embodiment 1)

表8、皮肤刺激性试验数据(实施例2)Table 8, skin irritation test data (embodiment 2)

表9、皮肤刺激性试验数据(实施例3)Table 9, skin irritation test data (embodiment 3)

表10、皮肤刺激性试验数据(实施例4)Table 10, skin irritation test data (embodiment 4)

表11、皮肤刺激性试验数据(实施例5)Table 11, skin irritation test data (embodiment 5)

实验数据表明,5%龙血竭提取液未见刺激性反应,顺利通过皮肤刺激性试验,符合要求。The experimental data showed that the 5% dragon's blood extract had no irritating reaction, passed the skin irritation test smoothly, and met the requirements.

2)人体安全性检测(人体皮肤斑贴试验)2) Human body safety testing (human skin patch test)

本实验采用5%浓度龙血竭提取液(分别由实施例1-5中制备得到的龙血竭提取物原液采用无菌水稀释得到)作为测试品,根据《化妆品卫生规范》2007版要求进行皮肤封闭性斑贴试验,参与实验人数为30人,试验数据见表8所示。This experiment uses 5% concentration of dragon's blood extract (respectively obtained by diluting the stock solution of dragon's blood extract prepared in Examples 1-5 with sterile water) as a test product, according to the requirements of "Hygienic Standards for Cosmetics" 2007 edition In the skin-occlusive patch test, the number of participants in the experiment was 30, and the test data are shown in Table 8.

表12、人体皮肤斑贴试验数据(实施例1)Table 12, human skin patch test data (embodiment 1)

表13、人体皮肤斑贴试验数据(实施例2)Table 13, human skin patch test data (embodiment 2)

表14、人体皮肤斑贴试验数据(实施例3)Table 14, human skin patch test data (embodiment 3)

表15、人体皮肤斑贴试验数据(实施例4)Table 15, human skin patch test data (embodiment 4)

表16、人体皮肤斑贴试验数据(实施例5)Table 16, human skin patch test data (embodiment 5)

实验数据表明,5%龙血竭提取液无人体皮肤不良反应,顺利通过人体皮肤斑贴实验,符合要求。Experimental data show that the 5% dragon's blood extract has no adverse reactions on human skin, and successfully passed the human skin patch test, meeting the requirements.

因此,通过毒理学检测和人体安全性检测,证明龙血竭提取液在适当浓度范围内使用对人体没有刺激及任何不良反应,将龙血竭提取液添加入化妆品中使用是安全可靠的。Therefore, through toxicology testing and human safety testing, it has been proved that the extract of dragon's blood has no stimulation or any adverse reaction to the human body when used in an appropriate concentration range, and it is safe and reliable to add the extract of dragon's blood to cosmetics.

实施例7、龙血竭提取物化妆品的制备(水剂状)Embodiment 7, the preparation of dragon's blood extract cosmetic (aqueous form)

一、配方1. Formula

配方1:龙血竭提取物(实验1)1.0%,去离子水87.5%,NMF-50 5.0%,山梨醇2.0%,尿囊素0.1%,丙三醇4.0%,透明汉生胶0.1%,LGP 0.3%。Formula 1: Dragon's blood extract (experiment 1) 1.0%, deionized water 87.5%, NMF-50 5.0%, sorbitol 2.0%, allantoin 0.1%, glycerol 4.0%, transparent xanthan gum 0.1% , LGP 0.3%.

配方2:龙血竭提取物(实验2)1.5%,去离子水87%,NMF-50 5.0%,山梨醇2.0%,尿囊素0.1%,丙三醇4.0%,透明汉生胶0.1%,LGP 0.3%。Formula 2: Dragon's blood extract (experiment 2) 1.5%, deionized water 87%, NMF-50 5.0%, sorbitol 2.0%, allantoin 0.1%, glycerol 4.0%, transparent xanthan gum 0.1% , LGP 0.3%.

配方3:龙血竭提取物(实验3)2%,去离子水87%,NMF-50 4.5%,山梨醇2.0%,尿囊素0.1%,丙三醇4.0%,透明汉生胶0.1%,LGP 0.3%。Formula 3: Dragon's Blood Extract (Experiment 3) 2%, Deionized Water 87%, NMF-50 4.5%, Sorbitol 2.0%, Allantoin 0.1%, Glycerol 4.0%, Transparent Xanthan Gum 0.1% , LGP 0.3%.

配方4:龙血竭提取物(实验4)2.5%,去离子水87%,NMF-50 4.5%,山梨醇2.0%,尿囊素0.1%,丙三醇3.5%,透明汉生胶0.1%,LGP 0.3%。Formula 4: Dragon's Blood Extract (Experiment 4) 2.5%, Deionized Water 87%, NMF-50 4.5%, Sorbitol 2.0%, Allantoin 0.1%, Glycerol 3.5%, Transparent Xanthan Gum 0.1% , LGP 0.3%.

配方5:龙血竭提取物(实验5)3%,去离子水87%,NMF-50 4.5%,山梨醇1.5%,尿囊素0.1%,丙三醇3.5%,透明汉生胶0.1%,LGP 0.3%。Formula 5: Dragon's Blood Extract (Experiment 5) 3%, Deionized Water 87%, NMF-50 4.5%, Sorbitol 1.5%, Allantoin 0.1%, Glycerol 3.5%, Transparent Xanthan Gum 0.1% , LGP 0.3%.

二、制备方法2. Preparation method

表16、水剂状龙血竭提取物化妆品的原料配方Table 16. Raw material formula of water-like dragon's blood extract cosmetics

如表16所示,将A相所有成分按比例称重,混合,搅拌加热到95℃保温30min后,降温到60℃添加B相,搅拌均匀,灌装即可。As shown in Table 16, weigh all the ingredients of phase A in proportion, mix them, stir and heat to 95°C for 30 minutes, then cool down to 60°C and add phase B, stir evenly, and fill.

实施例8、龙血竭提取物化妆品的制备(凝胶状)Embodiment 8, preparation of dragon's blood extract cosmetic (gel)

一、配方1. Formula

配方1:龙血竭提取物(实验1)1.0%,去离子水88.5%,山梨醇2%,丙三醇4.0%,1,3-丁二醇4.0%,卡伯U20 0.3%,MTI0.15%,NAON 0.05%。Formula 1: Dragon's Blood Extract (Experiment 1) 1.0%, Deionized Water 88.5%, Sorbitol 2%, Glycerol 4.0%, 1,3-Butanediol 4.0%, Kappa U20 0.3%, MTI0. 15%, NAON 0.05%.

配方2:龙血竭提取物(实验2)1.5%,去离子水88.2%,山梨醇2%,丙三醇3.7%,1,3-丁二醇4.0%,卡伯U20 0.3%,MTI0.2%,NAON 0.1%。Formula 2: Dragon's Blood Extract (Experiment 2) 1.5%, Deionized Water 88.2%, Sorbitol 2%, Glycerol 3.7%, 1,3-Butanediol 4.0%, Kappa U20 0.3%, MTI0. 2%, NAON 0.1%.

配方3:龙血竭提取物(实验3)2%,去离子水88.2%,山梨醇2%,丙三醇3.7%,1,3-丁二醇3.5%,卡伯U20 0.3%,MTI0.2%,NAON 0.1%。Formula 3: Dragon's Blood Extract (Experiment 3) 2%, Deionized Water 88.2%, Sorbitol 2%, Glycerol 3.7%, 1,3-Butanediol 3.5%, Kappa U20 0.3%, MTI0. 2%, NAON 0.1%.

配方4:龙血竭提取物(实验4)2.5%,去离子水88%,山梨醇2%,丙三醇3.5%,1,3-丁二醇3.3%,卡伯U20 0.3%,MTI0.2%,NAON 0.2%。Formula 4: Dragon's Blood Extract (Experiment 4) 2.5%, Deionized Water 88%, Sorbitol 2%, Glycerol 3.5%, 1,3-Butanediol 3.3%, Kappa U20 0.3%, MTI0. 2%, NAON 0.2%.

配方5:龙血竭提取物(实验5)3%,去离子水88%,山梨醇2%,丙三醇3.3%,1,3-丁二醇3.0%,卡伯U20 0.3%,MTI0.2%,NAON 0.2%。Formula 5: Dragon's Blood Extract (Experiment 5) 3%, Deionized Water 88%, Sorbitol 2%, Glycerol 3.3%, 1,3-Butanediol 3.0%, Kappa U20 0.3%, MTI0. 2%, NAON 0.2%.

二、制备方法2. Preparation method

表17、凝胶状龙血竭提取物化妆品的原料配方Table 17. Raw material formula of gel-like dragon's blood extract cosmetics

如表17所示,将A相所有成分按比例称重,混合,搅拌加热到95℃保温30min后,降温到60℃添加B相,搅拌均匀后添加C相,搅拌均匀,抽真空,灌装即可。As shown in Table 17, weigh all the ingredients of phase A in proportion, mix them, stir, heat to 95°C and keep it warm for 30 minutes, then cool down to 60°C and add phase B, stir well, add phase C, stir well, vacuumize, and fill That's it.

实施例9、龙血竭提取物化妆品的制备(膏霜)Embodiment 9, the preparation of dragon's blood extract cosmetic (cream)

一、配方1. Formula

配方1:龙血竭提取物(实验1)1.0%,去离子水73.6%,丙三醇5.0%,NMF-505.0%,HEC 0.1%,山梨醇2.0%,D-泛醇1.0%,单甘酯2.0%,白油7.0%,DM100 2.0%,混醇1.0%,LGP 0.3%。Formula 1: Dragon's blood extract (experiment 1) 1.0%, deionized water 73.6%, glycerin 5.0%, NMF-50 5.0%, HEC 0.1%, sorbitol 2.0%, D-panthenol 1.0%, monoglycerin 2.0% ester, 7.0% white oil, 2.0% DM100, 1.0% mixed alcohol, 0.3% LGP.

配方2:龙血竭提取物(实验2)1.5%,去离子水73%,丙三醇5.5%,NMF-50 4.5%,HEC 0.2%,山梨醇2.0%,D-泛醇1.0%,单甘酯2.0%,白油7.0%,DM100 2.0%,混醇1.0%,LGP 0.3%。Formula 2: Dragon's blood extract (experiment 2) 1.5%, deionized water 73%, glycerol 5.5%, NMF-50 4.5%, HEC 0.2%, sorbitol 2.0%, D-panthenol 1.0%, mono Glyceride 2.0%, white oil 7.0%, DM100 2.0%, mixed alcohol 1.0%, LGP 0.3%.

配方3:龙血竭提取物(实验3)2%,去离子水73%,丙三醇5.5%,NMF-50 4.0%,HEC 0.2%,山梨醇2.0%,D-泛醇1.0%,单甘酯2.0%,白油7.0%,DM100 2.0%,混醇1.0%,LGP 0.3%。Formula 3: Dragon's blood extract (experiment 3) 2%, deionized water 73%, glycerol 5.5%, NMF-50 4.0%, HEC 0.2%, sorbitol 2.0%, D-panthenol 1.0%, mono Glyceride 2.0%, white oil 7.0%, DM100 2.0%, mixed alcohol 1.0%, LGP 0.3%.

配方4:龙血竭提取物(实验4)2.5%,去离子水73%,丙三醇5.0%,NMF-50 4.0%,HEC 0.2%,山梨醇2.0%,D-泛醇1.0%,单甘酯2.0%,白油7.0%,DM100 2.0%,混醇1.0%,LGP 0.3%。Formula 4: Dragon's blood extract (experiment 4) 2.5%, deionized water 73%, glycerol 5.0%, NMF-50 4.0%, HEC 0.2%, sorbitol 2.0%, D-panthenol 1.0%, mono Glyceride 2.0%, white oil 7.0%, DM100 2.0%, mixed alcohol 1.0%, LGP 0.3%.

配方5:龙血竭提取物(实验5)3.0%,去离子水73%,丙三醇4.5%,NMF-50 4.0%,HEC 0.2%,山梨醇2.0%,D-泛醇1.0%,单甘酯2.0%,白油7.0%,DM100 2.0%,混醇1.0%,LGP 0.3%。Formula 5: Dragon's blood extract (experiment 5) 3.0%, deionized water 73%, glycerol 4.5%, NMF-50 4.0%, HEC 0.2%, sorbitol 2.0%, D-panthenol 1.0%, mono Glyceride 2.0%, white oil 7.0%, DM100 2.0%, mixed alcohol 1.0%, LGP 0.3%.

二、制备方法2. Preparation method

表18、膏霜状龙血竭提取物化妆品的原料配方Table 18. Raw material formula of cream-like dragon's blood extract cosmetics

如表18所示,将A相,B相分别将所有成分按比例称重,混合,搅拌加热到95℃保温30min后,均质30min后搅拌降温到60℃添加C相,搅拌均匀,抽真空,灌装即可。As shown in Table 18, weigh all the ingredients of phase A and phase B in proportion, mix them, stir and heat to 95°C for 30 minutes, homogenize for 30 minutes, stir and cool down to 60°C, add phase C, stir evenly, and vacuum , can be filled.

实施例10、临床试验Embodiment 10, clinical trial

(1)上述实施例制得的化妆品,选取18-25岁志愿者192名,随机分为16组,每组12人,连续试用30天(每人均仅使用相应的实施例或对比例化妆品,不再使用其他祛痘产品),对比分析评价上述各实施例中所制得的化妆品的祛痘效果,结果见表19。(1) For the cosmetics prepared in the above examples, 192 volunteers aged 18-25 were selected, randomly divided into 16 groups, 12 people in each group, and tried continuously for 30 days (each person only used the corresponding embodiment or comparative example cosmetics, Do not use other acne-removing products), comparative analysis and evaluation of the acne-removing effect of the cosmetics prepared in each of the above examples, the results are shown in Table 19.

测试区域:脸部长痘处。Test area: Acne on the face.

评价标准:显效,有效,无效。其中青春痘基本消除判断为显效;部分青春痘消除判断为有效;青春痘没有减少或减少不明显则判断为无效。Evaluation criteria: markedly effective, effective, and ineffective. Among them, the basic elimination of acne is judged to be markedly effective; the partial elimination of acne is judged to be effective; the acne is not reduced or the reduction is not obvious, and it is judged to be invalid.

对比例1:市售某品牌祛痘化妆品。Comparative example 1: A commercially available acne-removing cosmetic of a certain brand.

表19、各实施例中所制得的龙血竭提取物化妆品的祛痘效果Table 19, the acne-removing effect of the dried dragon's blood extract cosmetics prepared in each embodiment

组别group 有效efficient 显效markedly effective 无效invalid 实施例7(配方1)Embodiment 7 (recipe 1) 33 88 11 实施例7(配方2)Embodiment 7 (recipe 2) 33 99 00 实施例7(配方3)Embodiment 7 (recipe 3) 33 88 11 实施例7(配方4)Embodiment 7 (recipe 4) 33 66 33 实施例7(配方5)Embodiment 7 (recipe 5) 33 55 44 实施例8(配方1)Embodiment 8 (recipe 1) 66 66 00 实施例8(配方2)Embodiment 8 (recipe 2) 55 55 22 实施例8(配方3)Embodiment 8 (recipe 3) 55 55 22 实施例8(配方4)Embodiment 8 (recipe 4) 55 44 33 实施例8(配方5)Embodiment 8 (recipe 5) 44 44 44 实施例9(配方1)Embodiment 9 (recipe 1) 44 77 11 实施例9(配方2)Embodiment 9 (recipe 2) 44 77 11 实施例9(配方3)Embodiment 9 (recipe 3) 44 66 22 实施例9(配方4)Embodiment 9 (recipe 4) 44 66 22 实施例9(配方5)Embodiment 9 (recipe 5) 33 55 44 对比例1Comparative example 1 22 44 66

(2)上述实施例制得的化妆品,选取25-55岁的160名人员,随机分为16组,每组10人,连续试用30天(每人均仅使用相应的实施例或对比例化妆品,不再使用其他美白抗氧化产品),对比分析评价上述各实施例中所制得的化妆品的美白和抗氧化效果。其中,所述的美白和抗氧化效果为皮肤暗陈、色斑、皮肤粗糙等的改善情况,结果见表20。(2) For the cosmetics prepared in the above-mentioned examples, 160 persons aged 25-55 were selected, randomly divided into 16 groups, 10 people in each group, and tried for 30 days in a row (each person only used the corresponding embodiment or comparative example cosmetics, No longer using other whitening and anti-oxidation products), comparative analysis and evaluation of the whitening and anti-oxidation effects of the cosmetics prepared in each of the above examples. Among them, the whitening and anti-oxidation effects refer to the improvement of dark skin, pigmentation, rough skin, etc., and the results are shown in Table 20.

测试区域:脸部皮肤。Test area: facial skin.

评价标准:通过患者自述感受,及电脑比对皮肤纹理图鉴定皮肤改善程度。有效:肤色提亮,色斑颜色减淡,皮肤细腻度提高。无效:皮肤肤色、色斑及细腻度与试验前无任何变化。Evaluation criteria: The degree of skin improvement is identified through the patient's self-reported feelings and computer comparison with the skin texture map. Effective: brighten skin tone, lighten pigmentation spots, and improve skin fineness. Invalid: Skin color, pigmentation and fineness have no change from before the test.

对比例2:市售某品牌美白抗氧化化妆品。Comparative Example 2: Whitening and antioxidant cosmetics of a certain brand on the market.

表20、各实施例中所制得的龙血竭提取物化妆品的美白和抗氧化效果Table 20, the whitening and anti-oxidation effects of the dragon's blood extract cosmetics prepared in each embodiment

组别group 有效efficient 无效invalid 实施例7(配方1)Embodiment 7 (recipe 1) 1010 00 实施例7(配方2)Embodiment 7 (recipe 2) 99 11 实施例7(配方3)Embodiment 7 (recipe 3) 99 11 实施例7(配方4)Embodiment 7 (recipe 4) 88 22 实施例7(配方5)Embodiment 7 (recipe 5) 77 33 实施例8(配方1)Embodiment 8 (recipe 1) 1010 00 实施例8(配方2)Embodiment 8 (recipe 2) 99 11 实施例8(配方3)Embodiment 8 (recipe 3) 99 11 实施例8(配方4)Embodiment 8 (recipe 4) 99 11 实施例8(配方5)Embodiment 8 (recipe 5) 88 22 实施例9(配方1)Embodiment 9 (recipe 1) 1010 00 实施例9(配方2)Embodiment 9 (recipe 2) 1010 00 实施例9(配方3)Embodiment 9 (recipe 3) 99 11 实施例9(配方4)Embodiment 9 (recipe 4) 88 22 实施例9(配方5)Embodiment 9 (recipe 5) 77 33 对比例2Comparative example 2 44 66

Claims (10)

1.一种龙血竭提取物的制备方法,包括如下步骤:采用有机溶剂对龙血竭进行提取,所得提取液即为所述龙血竭提取物;所述有机溶剂为多元醇或白油。1. A preparation method for a dragon's blood extract, comprising the steps of: adopting an organic solvent to extract the dragon's blood, and the obtained extract is the described dragon's blood extract; the organic solvent is polyhydric alcohol or white oil . 2.根据权利要求1所述的制备方法,其特征在于:所述龙血竭的粒径为10目~200目。2. The preparation method according to claim 1, characterized in that: the particle size of the dragon's blood is 10 mesh to 200 mesh. 3.根据权利要求1或2所述的制备方法,其特征在于:所述多元醇为1-2-丙二醇、1,3-丙二醇、1,3-丁二醇和丙三醇中的任一种。3. The preparation method according to claim 1 or 2, characterized in that: the polyhydric alcohol is any one of 1-2-propanediol, 1,3-propanediol, 1,3-butanediol and glycerol . 4.根据权利要求1-3中任一项所述的制备方法,其特征在于:所述白油的牌号为15#或26#。4. The preparation method according to any one of claims 1-3, characterized in that: the grade of the white oil is 15# or 26#. 5.根据权利要求1-4中任一项所述的制备方法,其特征在于:所述提取为浸渍提取或回流提取。5. The preparation method according to any one of claims 1-4, characterized in that: the extraction is immersion extraction or reflux extraction. 6.根据权利要求1-5中任一项所述的制备方法,其特征在于:每1g所述龙血竭中加入1~1000g所述有机溶剂。6. The preparation method according to any one of claims 1-5, characterized in that 1-1000 g of the organic solvent is added to 1 g of the dragon's blood. 7.根据权利要求1-6中任一项所述的制备方法,其特征在于:所述提取的温度为25~180℃,每次提取的时间为10~1440分钟。7. The preparation method according to any one of claims 1-6, characterized in that: the temperature of the extraction is 25-180° C., and the time of each extraction is 10-1440 minutes. 8.根据权利要求1-7中任一项所述的制备方法,其特征在于:所述提取的次数为1~3次。8. The preparation method according to any one of claims 1-7, characterized in that: the number of extractions is 1-3 times. 9.权利要求1-8中任一项所述的制备方法制备得到的龙血竭提取物。9. The dragon's blood extract prepared by the preparation method described in any one of claims 1-8. 10.权利要求9所述的龙血竭提取物在直接作为具有下述1)-8)中的至少一种功能的化妆品中的应用或在制备具有下述1)-8)中至少一种功能的化妆品中的应用:10. The application of the dragon's blood extract described in claim 9 directly as a cosmetic having at least one function in the following 1)-8) or in the preparation of at least one of the following 1)-8) Functional Cosmetic Applications: 1)抑制痤疮致病菌;1) Inhibit acne pathogenic bacteria; 2)祛痘;2) acne; 3)清除DPPH自由基;3) Scavenge DPPH free radicals; 4)清除ABTS自由基;4) Scavenge ABTS free radicals; 5)抗氧化;5) anti-oxidation; 6)抗衰老;6) anti-aging; 7)抑制酪氨酸酶的活性;7) inhibit the activity of tyrosinase; 8)美白。8) Whitening.
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WO2019136105A1 (en) * 2018-01-02 2019-07-11 Skinkick, Llc Topical skin care compositions

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