CN114010562A - 一种控油祛痘组合物及其制备方法 - Google Patents
一种控油祛痘组合物及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种控油祛痘组组合物及其制备方法,属于化妆品领域,该组合物由含罗勒叶提取物、麝香草叶提取物、白珠树叶提取物、黄芩根提取物、乳酸薄荷酯、10‑羟基癸酸、以及添加剂制成;本发明提供的祛痘组合物,刺激性低,组分间各成分协同增效,有效抑制油脂过度分泌和收敛毛孔,从而抑制痘痘发生;本发明提供的祛痘组合物可添加在精华、面膜、面霜等中使用,通过不同的项的组分原料,采用不同的温度添加方法,保留了有效活性成分的活性,并且各组分之间充分混合均一,性能稳定,制备简单方便,易于规模化生产。
Description
技术领域
本发明涉及化妆品领域,具体涉及一种控油祛痘组合物及其制备方法。
背景技术
青春痘,又名痤疮,痤疮是一种常见的人类慢性炎症皮肤病,是一种好发于颜面、胸、背部的毛囊及皮脂腺的慢性炎症性皮肤病。主要的发病形式为青春痘、粉刺。痤疮具有多种皮肤损害形式,包括粉刺、丘疹、脓疱、结节等,因此,一直以来痤疮都是皮肤科的常见病及多发病。主要好发于青少年,对青少年的心理和社交影响很大。痤疮的病因较为复杂,现代医学认为痤疮的发病机制主要与皮脂分泌过多、毛囊皮脂腺导管堵塞、细菌感染和炎症反应等因素密切相关。进入青春期后人体内雄激素特别是睾酮的含量迅速升高,促进皮脂腺发育并产生大量皮脂。同时毛囊皮脂腺导管的角化异常造成导管堵塞,皮脂排出障碍,形成角质栓即微粉刺。毛囊中多种微生物尤其是痤疮丙酸杆菌大量繁殖,痤疮丙酸杆菌产生的脂酶分解皮脂生成游离脂肪酸,同时趋化炎症细胞和介质,最终诱导并加重炎症反应。痤疮具有病程长,易复发的特点,长期困扰着广大青少年。
目前,治疗痤疮的方法有很多,多以口服药物为主,或外用药物(或将其添加于护肤品或者化妆品中);口服的方式主要利用全身血液循环来全身给药,以达到治疗痤疮的功效,一般疗程较长、效果不佳,且副作用也较大;而目前市面上的外用药物,基本为抑菌杀菌剂,有些甚至使用氯霉素、克林霉素等抗生素,这类产品的特点是见效快,易反复,容易产生依赖性。经科学家的研究后,结果发现主要原因为皮肤的微生态环境受到了破坏。上述祛痘产品在抑杀有害菌群(主要是痤疮丙酸杆菌和金黄葡萄球菌)的同时,对皮肤表面的益生菌群有同样的杀灭作用,导致皮肤的微生态环境受到破坏,有益菌群竞争性抑制有害菌群的功能丧失,皮肤的菌落失去平衡,导致青春痘易反复,对祛痘产品产生依赖性。
要筛选出高效的祛痘功效添加剂,首先必须了解痤疮形成的机理。痤疮的形成与皮脂分泌过多、毛孔堵塞、角质过度角化、细菌过度生长、内分泌失调、遗传、饮食生活习惯等因素有关。具体来说,进入青春期后,雄性激素特别是睾酮的水平快速升高,睾酮在皮肤中经5-α还原酶的作用转化为二氢睾酮,后者与皮脂腺细胞的雄激素受体结合,促进皮脂腺发育并产生大量皮脂。由于痤疮患者的皮脂中亚油酸含量降低,毛囊周围的必需脂肪酸减少,促使毛囊孔角质化,进而使管口阻塞。皮脂排出的受阻又正好为毛囊中的痤疮丙酸杆菌创造了良好的局部厌氧环境,使这类厌氧菌大量繁殖,分解皮脂并产生游离脂肪酸,这些游离脂肪酸会刺激毛囊引起炎症。在闭塞的毛囊皮脂腺内部,由于炎症的发生,毛囊皮脂腺结构遭到破坏,形成结节、囊肿和粉瘤,最后破坏皮肤,形成疤痕,影响面部容貌,对青少年的心理和社交影响很大。为了解决现有技术存在的缺陷和不足,本发明公开了一种控油祛痘组合物及其制备方法,以满足现今人们对控油祛痘的使用需求。
发明内容
针对上述存在的问题,本发明提出了一种控油祛痘组合物及其制备方法。
为了实现上述的目的,本发明采用以下的技术方案:
一种控油祛痘组合物,其特征在于,所述组合物由以下重量份的原料制成:罗勒叶提取物1-10份、麝香草叶提取物1-10份、白珠树叶提取物1-10份、黄芩根提取物1-10份、乳酸薄荷酯1-10份、癸二酸1-5份、以及添加剂0.3-30份及水余量。
优选的,所述添加剂由重量份为防腐剂0.1-1份、保湿剂0.1-30份、乳化剂0.1-1份以及PH调节剂0.1-1份组成。
优选的,所述防腐剂由羟苯甲酯、羟苯丙酯、氯苯甘醚、甲基异噻唑啉酮、甲基氯异噻唑啉酮、苯氧乙醇、DMDM乙内酰脲、咪唑烷基脲、3-碘-2-丙炔基丁基氨基甲酸酯、乙基己基甘油、辛甘醇、辛酰羟肟酸、甘油辛酸酯、对羟基苯乙酮、1,2-己二醇中的一种或多种组成。
优选的,所述保湿剂由甘油、丙二醇、丁二醇、山梨醇、戊二醇、透明质酸钠、聚谷氨酸、海藻糖、甜菜碱中的一种或多种组成。
优选的,所述乳化剂由甘油硬脂酸酯、甘油硬脂酸酯柠檬酸酯、PEG-100硬脂酸酯、氢化卵磷脂、鲸蜡硬脂醇橄榄油酸酯、山梨坦橄榄油酸酯、十六烷基磷酸酯钾盐、吐温20、吐温60、聚甘油-10-硬脂酸酯中的一种或多种组成。
优选的,所述PH调节剂由三乙醇胺、碳酸氢钠、碳酸氢钾、氢氧化钠、氢氧化钾中的一种或多种组成。
优选的,一种控油祛痘组合物的制备方法,包括以下制备步骤:
(1)将罗勒叶用粉碎机25000R/min进行粉碎,得到罗勒叶粉碎物,然后按料液质量分数比为1:10-20,加入温度为60℃~90℃的石油醚,将提取温度控制在30-40℃,提取过程中进行30-60min的超声波处理,再进行过滤,进行真空浓缩至恒重,得罗勒叶提取物;
(2)将麝香草叶用粉碎机25000R/min进行粉碎,得到麝香草叶粉碎物,然后按料液质量分数比为1:10-20,加入温度为60℃~90℃的石油醚,将提取温度控制在30-40℃,提取过程中进行30-60min的超声波处理,再进行过滤,进行真空浓缩至恒重,得麝香草叶提取物;
(3)将白珠树叶用粉碎机25000R/min进行粉碎,得到白珠树叶粉碎物,按料液质量分数比为1:10-30,加入30-50%无水无醇,30-50%丁二醇和20-40%去离子水,将提取温度控制在50-60℃,提取过程中进行40-60min的超声波处理,提取结束后进行过滤,进行真空浓缩至恒重,得白珠树叶提取物;
(4)将黄芩根用粉碎机25000R/min进行粉碎,得到黄芩根粉碎物,按料液质量分数比为1:10-30,加入30-50%无水无醇,30-50%丁二醇和20-40%去离子水,将提取温度控制在50-60℃,提取过程中进行40-60min的超声波处理,提取结束后进行过滤,进行真空浓缩至恒重,得黄芩根提取物;
(5)将得到的提取物和其他组分按照重量份配比进行称取并与称取的防腐剂、保湿剂、乳化剂、乳酸薄荷酯、10-羟基癸酸以及PH调节剂进行混合,即得控油祛痘组合物。
本发明提供的各成分的功效如下:
罗勒(OCIMUM BASILICUM)叶提取物:罗勒叶,中药名,是唇形目、唇形科、罗勒属植物,为药食两用芳香植物,原产于非洲、美洲及亚洲热带地区。中国主要分布于新疆,吉林,河北,河南,浙江,江苏,安徽,江西,湖北,湖南,广东,广西,福建,台湾,贵州,云南及四川;味辛、甘,性温。有疏风行气,化湿消食、活血、解毒之功能。用于外感头痛、食胀气滞、脘痛、泄泻、月经不调、跌打损伤、蛇虫咬伤、皮肤湿疮、瘾疹痛痒等症的治疗。
麝香草(THYMUS VULGARIS)叶提取物:为唇形科植物,为药食两用芳香植物,作药用具有镇痉、驱风、强壮作用,主治炎症、痉挛性咳嗽、百日咳、喉头肿痛等。可作为食材,欧洲烹饪常用香料,味道辛香,用来加在炖肉、蛋或汤中;植物中含有牻牛儿醇、芳樟醇、α-松油醇、香荆芥酚、麝香草脑、松油醇-4。皂甙、熊果酸、齐墩果酸、咖啡酸、绿原酸、等成分。
平铺白珠树(GAULTHERIAPROCUMBENS)叶提取物:为杜鹃花科白珠树属植物,产江西(井冈山)、福建、台湾、广东、广西、贵州。中南半岛、菲律宾和马来西亚亦有。可入药,性味:辛;性温;功能主治:祛风除湿;通络止痛。主风湿痹痛;跌打损伤;同时植物中含有丰富的水杨苷,具有解热和镇痛作用,在体内可转化为水杨酸,从而有剥落角质的作用。
黄芩(SCUTELLARIABAICALENSIS)根提取物:黄芩,中药名,唇形科黄芩属植物,野生黄芩主要分布中国内蒙中东部和东北三省大部,河北承德,内蒙古赤峰等几个最具规模的主产区,是中国北方野生中药材的主要产地之一。栽培黄芩主要分布在山东、山西、陕西、甘肃四大产区。性味:味苦,性寒;主治用于湿温、暑湿,胸闷呕恶,湿热痞满,泻痢,黄疸,肺热咳嗽,高热烦渴,血热吐衄,痈肿疮毒,胎动不安。
本发明提供的控油祛痘组合物各成分通过优化组分对比,协同增强作用,有效抑制油脂过度分泌和收敛毛孔,从而抑制痘痘发生。
本发明提供的所述控油祛痘组合物可广泛用于化妆品中,如化妆品的水、精华、乳液、霜、面膜等等。
进一步地,本发明还提供了一种控油祛痘精华,含有有上述的控油祛痘组合物。
进一步的,所述控油祛痘精华中,还包括用于将所述控油祛痘组合物制成精华的辅料。
所述的抗衰老精华包括以下组分:
A项:去离子水、EDTA二钠,羟苯甲酯,甘油、丁二醇、丙烯酰二甲基牛磺酸铵/VP共聚物、氢化卵磷酯、透明质酸钠、
B项:辛酰羟肟酸、1,2-己二醇
C项:控油祛痘组合物
不同的原料,根据添加顺序,分为不同的项,经过加热搅拌处理后,降温,添加控油祛痘组合物,最后得到,成分均一的精华,吸于肌肤吸收,有效抑制油脂过度分泌和收敛毛孔,从而抑制痘痘发生。
进一步地,按上述控油祛痘精华的重量计,所述的控油祛痘精华包含以下重量百分比:
A项:EDTA二钠0.02,羟苯甲酯0.12,甘油3.5,丁二醇3.5,丙烯酰二甲基牛磺酸铵/VP共聚物0.5,氢化卵磷酯0.3,透明质酸钠0.05,去离子水到100;
B项:辛酰羟肟酸0.03,1,2-己二醇0.55;
C项:控油祛痘组合物;
本发明选用以上重量配比的各原料,制得的控油祛痘精华,质地温和,易吸收,有效抑制油脂过度分泌和收敛毛孔,从而抑制痘痘发生。
本发明对上述控油祛痘精华的制备方法,包括以下步骤:
将A项先投入主锅中,先开启慢均质,至全部溶胀完全无颗粒时,加热至85℃,保温30分钟,然后开启冷却水,开始冷却;
降温至60℃左右,把B项在另一容器中,加热至完全溶解,然后投入主锅中,搅拌均匀;
再降温至45℃然后投入C项,即投入控油祛痘组合物,搅拌3到5分钟,搅拌均匀;
检验合格后,出料过滤布150目。
由于采用上述的技术方案,本发明的有益效果是:
(1)本发明提供的控油祛痘组合物,各成分协同增效,有效抑制油脂过度分泌和收敛毛孔,从而抑制痘痘发生。
(2)本发明提供的控油祛痘精华,选用了不同配比关系的各种辅料,制得的精华,各组成稳定均一,易于吸收。
(3)本发明提供的控油祛痘组合物可添加在精华中使用,通过不同的项的组分原料,采用不同的温度添加方法,保留了有效活性成分的活性,并且各组分之间充分混合均一,性能稳定,制备简单方便,易于规模化生产。
(4)本发明的组分原料刺激性低,组分间协同增强作用,有效抑制油脂过度分泌和收敛毛孔,从而抑制痘痘发生。由于采用上述的技术方案,本发明的有益效果是:
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述。基于本发明的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
需要说明的是,本发明提供的技方案中所采用的原料,除特殊说明外,均通过常规手段制备或者通过商业渠道购买。
本发明提供的罗勒叶采购于:青岛朱雀贸易有限公司;
麝香草叶采购于:安国市芳草佳商贸有限公司;
白珠树叶采购于:毫州市天瑞药材商行;
黄芩根采购于:毫州市天瑞药材商行
乳酸薄荷脂采购于:广州市奥雪化工有限公司
10-羟基癸酸采购于:天元航材(营口)科技股份有限公司
本发明中提供了含白珠树叶提取物控油祛痘组合物及其制备方法,该抗控油祛痘组合物应用于护肤精华中,该精华包括有控油祛痘组合物。
该抗衰老精华包括以下四项组分:
A项:去离子水、EDTA二钠,羟苯甲酯,甘油、丁二醇、丙烯酰二甲基牛磺酸铵/VP共聚物、氢化卵磷酯、透明质酸钠、
B项:辛酰羟肟酸、1,2-己二醇
C项:控油祛痘组合物
其中含一种控油祛痘组合物的制备方法,包括以下制备步骤:
(1)将罗勒叶用粉碎机25000R/min进行粉碎,得到罗勒叶粉碎物;然后按料液质量分数比为1:10-20;加入石油醚(60℃~90℃),将提取温度控制在30-40℃,提取过程中进行30-60min的超声波处理,再进行过滤,进行真空浓缩至恒重,得罗勒叶提取物;
(2)将白珠树叶用粉碎机25000R/min进行粉碎,得到白珠树叶粉碎物,按料液质量分数比为1:10-30,加入30-50%无水无醇,30-50%丁二醇和20-40%去离子水,将提取温度控制在50-60℃,提取过程中进行40-60min的超声波处理,提取结束后进行过滤,进行真空浓缩至恒重,得白珠树叶提取物;
(3)将黄芩根用粉碎机25000R/min进行粉碎,得到黄芩根粉碎物,按料液质量分数比为1:10-30,加入30-50%无水无醇,30-50%丁二醇和20-40%去离子水,将提取温度控制在50-60℃,提取过程中进行40-60min的超声波处理,提取结束后进行过滤,进行真空浓缩至恒重,得黄芩根提取物;
(4)将得到的提取物和其他组分按照重量份配比进行称取并与称取的防腐剂、保湿剂、乳化剂以及PH调节剂进行混合,即得控油祛痘组合物
实施例1:
制备本实施例1添加有本发明控油祛痘组合物的精华:
其中,控油祛痘组合物中罗勒叶提取物重量比为20%、麝香草叶提取物重量比为20%、白珠树叶提取物重量比为20%、黄芩根提取物重量比为20%、乳酸薄荷酯重量比为18%、10-羟基癸酸的重量比为2%。
控油祛痘精华的具体制备步骤包括如下:
(1)将A项先投入主锅中,先开启慢均质,至全部溶胀完全无颗粒时,加热至85℃,保温30分钟,然后开启冷却水,开始冷却;
(2)降温至60℃左右,把B项在另一容器中,加热至完全溶解,然后投入主锅中,搅拌均匀;
(3)再降温至45℃然后投入C项,即投入控油祛痘组合物,搅拌3到5分钟,搅拌均匀,检验合格后,出料过滤布150目,得到本实施例1的控油祛痘精华。
实施例2:
制备本实施例2添加有本发明控油祛痘组合物的精华:
其中,控油祛痘组合物中罗勒叶提取物重量比为20%、麝香草叶提取物重量比为20%、白珠树叶提取物重量比为20%、黄芩根提取物重量比为20%、乳酸薄荷酯重量比为18%、10-羟基癸酸的重量比为2%。
其中,控油祛痘精华的具体制备步骤同实施例1的具体步骤。
实施例3:
制备本实施例3添加有本发明控油祛痘组合物的精华:
其中,控油祛痘组合物中罗勒叶提取物重量比为15%、麝香草叶提取物重量比为15%、白珠树叶提取物重量比为25%、黄芩根提取物重量比为25%、乳酸薄荷酯重量比为16%、10-羟基癸酸的重量比为4%。
其中,控油祛痘精华的具体制备步骤同实施例1的具体步骤。
实施例4:
制备本实施例4添加有本发明控油祛痘组合物的精华:
其中,控油祛痘组合物中罗勒叶提取物重量比为20%、麝香草叶提取物重量比为15%、白珠树叶提取物重量比为20%、黄芩根提取物重量比为30%、乳酸薄荷酯重量比为13%、10-羟基癸酸的重量比为2%。
其中,控油祛痘精华的具体制备步骤同实施例1的具体步骤。
实施例5:
制备本实施例5添加有本发明控油祛痘组合物的精华:
其中,控油祛痘组合物中罗勒叶提取物重量比为15%、麝香草叶提取物重量比为20%、白珠树叶提取物重量比为20%、黄芩根提取物重量比为30%、乳酸薄荷酯重量比为13%、10-羟基癸酸的重量比为2%。
其中,控油祛痘精华的具体制备步骤同实施例1的具体步骤。
实施例6:
制备本实施例6添加有本发明控油祛痘组合物的精华:
其中,控油祛痘组合物中罗勒叶提取物重量比为25%、麝香草叶提取物重量比为15%、白珠树叶提取物重量比为30%、黄芩根提取物重量比为20%、乳酸薄荷酯重量比为8%、10-羟基癸酸的重量比为2%。
其中,控油祛痘精华的具体制备步骤同实施例1的具体步骤。
实施例7:
制备本实施例7添加有本发明控油祛痘组合物的精华:
其中,控油祛痘组合物中罗勒叶提取物重量比为15%、麝香草叶提取物重量比为25%、白珠树叶提取物重量比为30%、黄芩根提取物重量比为20%、乳酸薄荷酯重量比为8%、10-羟基癸酸的重量比为2%。
其中,控油祛痘精华的具体制备步骤同实施例1的具体步骤。
实施例8:
制备本实施例8添加有本发明控油祛痘组合物的精华:
其中,控油祛痘组合物中罗勒叶提取物重量比为15%、麝香草叶提取物重量比为25%、白珠树叶提取物重量比为35%、黄芩根提取物重量比为15%、乳酸薄荷酯重量比为8%、10-羟基癸酸的重量比为2%。
其中,控油祛痘精华的具体制备步骤同实施例1的具体步骤。
实施例9:
制备本实施例9添加有本发明控油祛痘组合物的精华:
其中,控油祛痘组合物中罗勒叶提取物重量比为25%、麝香草叶提取物重量比为15%、白珠树叶提取物重量比为25%、黄芩根提取物重量比为30%、乳酸薄荷酯重量比为3%、10-羟基癸酸的重量比为2%。
其中,控油祛痘精华的具体制备步骤同实施例1的具体步骤。
实施例10:
制备本实施例10添加有本发明控油祛痘组合物的精华:
其中,控油祛痘组合物中罗勒叶提取物重量比为25%、麝香草叶提取物重量比为10%、白珠树叶提取物重量比为15%、黄芩根提取物重量比为35%、乳酸薄荷酯重量比为8%、10-羟基癸酸的重量比为2%。
其中,控油祛痘精华的具体制备步骤同实施例1的具体步骤。
对比例11:
制备本对比例11的精华:
本对比例11的精华的制备方法包括:
(1)将A项组分原料先投入主锅中,先开启慢均质,至全部溶胀完全无颗粒时,加热至85℃,保温30min,然后开启冷却水,开始冷却;
(2)降温至60℃,将B项组分原料加入另一容器中,加热至完全溶解,然后投入主锅中与A项组分原料搅拌均匀;
(3)然后降温至45℃,检验合格后,出料过滤布150目,即得本对比例11的精华。
对上述实施例以及对比例提供的控油祛痘精华进行功效评价:
1、抗刺激性实验:
鸡胚绒毛毛尿囊膜结构与眼结膜相似,绒毛尿囊膜血管实验方法通过观察受试物对血管的作用,评价潜在的刺激性,即孵化的10-14天胚龄的受精鸡胚中期绒毛尿囊膜,利用CAM血管系统完整、明显和透明的特点,将一定量受试物直接与CAM接触,作用一段时间之后观察CAM血管损伤,对不同的血管损伤程度进行评分,血管损伤越严重分值越大。本方法特别强调检测物的血管效应,如由此引发的鬼影血管、毛细血管充血、毛细血管出血等现象。NC值(正常使用浓度刺激值)是指,根据CAM血管效应对应的分值做出评分,取一组数据的平均值,确定刺激性的大小。
刺激性评价:
评分标准:
实施例刺激性评价:
从以上数据可以看得出,本实施例1-10中的NC值分数均较低,本发明的控油祛痘精华组合物,产品温和无刺激,对敏感肌的人群也非常适用,同时组合物还可以略降低产品的本身刺激性,减少产品对皮肤的不适应性,能维持皮肤的稳态与基础健康。
2、安全性测试
试验方法:选取年龄25-45岁志愿者110名。志愿者皮肤健康,无过敏体质或化妆品过敏史及无妊娠、哺乳期、30天内无参加药物临床试验,或正在参加其他化妆品人体安全性和功效试验者,分为11个小组,分别试用实施例1-10的控油祛痘精华精华和对比例11的精华,选用合格的斑试器,以封闭式斑贴实验方式,选用约控油祛痘精华0.02g样品滴于斑试器内,外用专用胶带贴于受试者手前臂内侧处48h,去除受试物后,分别在0.5、6、12、24、48h观察皮肤反应。按照《化妆品卫生规范》中皮肤反应分级标准记录其结果。
实验结果:人体皮肤斑贴测试结果显示:受组受试者通过实施例1-10的控油祛痘精华精华和对比例11的精华的测试,在0.5、6、12、24、48h观察皮肤反应,其中0例出现皮肤不良反应,说明添加了本发明的控油祛痘组合物的精华稳定安全,且在长期使用本发明产品过程中,未发现不良反应和刺激性。
3、抗氧化实验
(1)DPPH清除能力的测定
移取0.01mg/ml样液的乙醇溶液1mL样液,加入0.1mmol/L的DPPH反应液4mL,摇匀。避光反应30分钟后于517nm下测定吸光度A,试验重复三次,取其平均值;同时以乙醇代替样液测定吸光度A0,DPPH·自由基清除率计算公式如下
DPPH·清除率(%)=A0/(A0-A)×100。
式中:A0为对照组的吸光度;A为加样品的吸光度。
(2)ABTS清除能力的测定
移取0.01mg/ml样液的乙醇溶液1mL样液,加入0.1mmol/L的ABTS工作液反应液4mL,摇匀。避光反应10分钟后于734nm下测定吸光度A,取其平均值;同时以乙醇代替样液测定吸光度A0。
ABTS·清除率(%)=A0/(A0-A)×100。
式中:A0为对照组的吸光度;A为加样品的吸光度。
试验结果如下表:
实验结果:实施例1-10,DPPH自由基清除率和ABTS自由基清除率,明显大于对比例11;具有良好的抗氧化效果,可以预测在皮肤中能起到良好的抗氧化效果,从而能减轻痘痘的炎症时的氧化应激反应,从而减少痘痘的发生,以及减轻痘印的发生。
3、抑菌实验
(1)培养基的制备
称取琼脂15g/L,蛋白胨10g/L,脱水小牛脑浸粉12.5g/L,脱水牛心浸粉5g/L,氯化钠5g/L,葡萄糖2g/L,磷酸氯二钠2.5g/L,培养基按常规方法配制,调pH值为7.2~7.6。将培养基于锥形瓶中密封好后,放入灭菌锅中于121℃下灭菌30min,待冷却后,置于4℃冰箱中保存备用。
(2)菌悬液的制备
将标准菌株(金黄色葡萄珠菌ATC6538和痤疮丙菌杆菌ATC699)分别接种培养增菌,在常规培养条件下培养24h(痤疮丙酸杆菌用厌氧手套箱培养48h),吸取菌液用培养基稀释调整为0.5个麦氏比浊单位(约为1.5×108CFU//mL),将菌悬液用培养基继续稀释,用麦氏比浊仪将调整为1×106~105CFU/mL,备用。
(3)抑菌圈测定
在无菌操作条件下,分别取上述菌悬液,用涂布棒均匀涂抹在培养基上。再用无菌镊将牛津杯轻放在凝固的培养基表面,轻压牛津杯使接触良好。用一次性注射针吸取供试液(实施例1-10,对比例11,及市售同某堂控油祛痘膏作为对照组)于牛津杯中,37℃培养箱培养24h后取出(痤疮丙酸杆菌用厌氧手套箱培养48h),用卡尺准确测量各培养皿中供试液有效抑菌圈的直径。各样品重复3次。另外配制对照组:空白对照组(培养基)、阴性对照组(培养基、菌悬液、无菌水)、阳性对照组(培养基、菌悬液、红霉素1%),来观察细菌的生长情况、培养基和中草药对细菌生长的影响。
试验结果如下表:
实验结果:实施例1-10,金黄色葡萄球菌抑菌直径和痤疮丙酸杆菌抑菌直径/mm,明显大于对比例11和市售的产品;含有控油祛痘组合物的祛痘精华具有良好的祛痘杀菌效果,从而可以抑制痘痘的发生,及痘痘的治疗。
4、抗炎实验
测试方法:往手臂涂抹1%组胺溶液,涂抹面积为7cm2,每5min涂抹一次,每次涂抹0.02g,直至皮肤出组红疹。然后往红疹皮肤分别涂抹本发明实施例1-10例和对比例11及对照组市售同某堂控油祛痘膏,涂抹量为0.02g,均匀涂抹在红疹,然后按下计时器,记录每个红疹消失的时间。
实验结果:实施例1-10中,抗炎效果都比对比例11和对照组效果显著。综合可得添加了本发明的控油祛痘组合物的精华,具有很好的抗炎效果,可以减少皮肤的炎症,及在痘痘皮肤中的炎症,从而减少痘痘的发生,以及减轻痘印的发生。
5、控油及保湿功效测试
测试方法:选取年龄20-35岁油性肌肤志愿者。志愿者无妊娠、哺乳期、30天内无参加药物临床试验,或正在参加其他化妆品人体安全性和功效试验者195名,分为13个小组,每组15人,分别试用实施例1-10例,对比例11以及以及市场占有率大的护肤品为对照组做对比测试,使用方法为,每日早晚各使用一次,使用周期为2周。试用产品前对其面部皮肤进行数据采集和面部图像拍照分析,数据作为皮肤起始值,在使用前以及使用2周后。进行数据采集分析,数据作为皮肤结果值,测试环境温度为25℃,湿度为60%;每个数据测试三次,取平均值后,计算每组平均值,保留小数点后二位;用水分测试仪(Corneometer CM825)测试皮肤水分含量的变化,评估该产品对肌肤的保湿程度;用皮肤油脂含量测试仪Sebumeter,评估该产品的对皮肤油脂分泌情况;结果如下:
实验结果:实施例1-10中,对皮肤的保湿效果都比对比例11和对照组效果显著;同时实施例1-10中,对皮肤中油脂的抑制效果比对比例11和对照组效果显著;综合可得添加了本发明的控油祛痘组合物的精华,具有很好的皮肤保湿及抑制油脂分泌效果,可以减少皮肤的的油脂分泌,从而减少痘痘的发生。
6、实验例
测试方法:选取年龄20-35岁具有轻度或中度青春痘肌肤志愿者。志愿者无妊娠、哺乳期、30天内无参加药物临床试验,或正在参加其他化妆品人体安全性和功效试验者1300名,分为13个小组,每组100人,分别试用实施例1-10例,对比例11以及以及市场占有率大的护肤品为对照组做对比测试,使用方法为,每日早晚各使用一次,使用周期为10天,试用效果下如下表。
由以上结果可以看出,采用本发明的控油祛痘组合物的精华液对轻度或中度青春痘肌肤效果显著,比对照组和空白组,效果都显著;采用本发明的控油祛痘精华液各组分相互配合,协同增效,具有很好治疗痘痘功效。
以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (7)
1.一种控油祛痘组合物,其特征在于,所述组合物由以下重量份的原料制成:罗勒叶提取物1-10份、麝香草叶提取物1-10份、白珠树叶提取物1-10份、黄芩根提取物1-10份、乳酸薄荷酯1-10份、癸二酸1-5份、以及添加剂0.3-30份。
2.根据权利要求1所述的控油祛痘组合物,其特征在于,所述添加剂由重量份为防腐剂0.1-1份、保湿剂1-30份、乳化剂0.1-1份、PH调节剂0.1-1份及余量水组成。
3.根据权利要求2所述的控油祛痘组合物,其特征在于,所述防腐剂由羟苯甲酯、羟苯丙酯、氯苯甘醚、甲基异噻唑啉酮、甲基氯异噻唑啉酮、苯氧乙醇、DMDM乙内酰脲、咪唑烷基脲、3-碘-2-丙炔基丁基氨基甲酸酯、乙基己基甘油、辛甘醇、辛酰羟肟酸、甘油辛酸酯、对羟基苯乙酮、1,2己二醇中的一种或多种组成。
4.根据权利要求2所述的控油祛痘组合物,其特征在于,所述保湿剂由甘油、丙二醇、丁二醇、山梨醇、戊二醇、透明质酸钠、聚谷氨酸、海藻糖、甜菜碱中的一种或多种组成。
5.根据权利要求2所述的控油祛痘组合物,其特征在于,所述乳化剂甘油硬脂酸酯、甘油硬脂酸酯柠檬酸酯、PEG-100硬脂酸酯、氢化卵磷脂、鲸蜡硬脂醇橄榄油酸酯、山梨坦橄榄油酸酯、十六烷基磷酸酯钾盐、吐温20、吐温60、聚甘油-10-硬脂酸酯中的一种或多种组成。
6.根据权利要求2所述的控油祛痘组合物,其特征在于,所述PH调节剂由三乙醇胺、碳酸氢钠、碳酸氢钾、氢氧化钠、氢氧化钾中的一种或多种组成。
7.根据权利要求1-6任一所述的控油祛痘组合物的制备方法,其特征在于,包括以下制备步骤:
(1)将罗勒叶用粉碎机25000R/min进行粉碎,得到罗勒叶粉碎物,然后按料液质量分数比为1:10-20,加入温度为60℃~90℃的石油醚,将提取温度控制在30-40℃,提取过程中进行30-60min的超声波处理,再进行过滤,进行真空浓缩至恒重,得罗勒叶提取物;
(2)将麝香草叶用粉碎机25000R/min进行粉碎,得到麝香草叶粉碎物,然后按料液质量分数比为1:10-20,加入温度为60℃~90℃的石油醚,将提取温度控制在30-40℃,提取过程中进行30-60min的超声波处理,再进行过滤,进行真空浓缩至恒重,得麝香草叶提取物;
(3)将白珠树叶用粉碎机25000R/min进行粉碎,得到白珠树叶粉碎物,按料液质量分数比为1:10-30,加入60-80%无水无醇、20-50%丁二醇和10-30%去离子水,将提取温度控制在50-60℃,提取过程中进行40-60min的超声波处理,提取结束后进行过滤,进行真空浓缩至恒重,得白珠树叶提取物;
(4)将黄芩根用粉碎机25000R/min进行粉碎,得到黄芩根粉碎物,按料液质量分数比为1:10-30,加入60-80%无水无醇、20-50%丁二醇和10-30%去离子水,将提取温度控制在50-60℃,提取过程中进行40-60min的超声波处理,提取结束后进行过滤,进行真空浓缩至恒重,得黄芩根提取物;
(5)将得到的提取物和其他组分按照重量份配比进行称取并与称取的防腐剂、保湿剂、乳化剂、乳酸薄荷酯、10-羟基癸酸以及PH调节剂进行混合,即得控油祛痘组合物。
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