CN115040436B - 具有光防护功效的护发素及其制备方法 - Google Patents
具有光防护功效的护发素及其制备方法 Download PDFInfo
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Abstract
本发明提一种具有光防护功效的护发素及其制备方法,该护发素采用特定配比的阳离子表面活性剂、增稠剂、杏仁油、茶树精油、月桂精油以及去离子水等复配制备而成,配伍性好,成分温和,可有效降低紫外光引起的头发蛋白质、脂质、色氨酸等物质的氧化损失。
Description
技术领域
本发明涉及护发技术领域,具体涉及一种具有光防护功效的护发素及其制备方法。
背景技术
工业科技社会的快速发展在改善人们生活的同时,产生的一些含氯和含溴的物质也会造成臭氧层的破环,大大降低其吸收紫外线的能力,增加了日常生活中紫外线的辐射量。实验表明,日光中的紫外线(90%~95%的UVA和5%~10%的UVB)辐射易损伤头发表面毛鳞片和内部各种组成物质。UVB可断裂毛小皮中的二硫键,降解氨基酸,氧化脂质,损伤头发内部结构,使头发变得更脆,易断裂。UVA则会通过内源性光敏剂之间的相互作用产生自由基活性氧类物质,导致头发中蛋白质和色素氧化分解。
发明内容
基于此,有必要提供一种具有光防护功效的护发素及其制备方法,能够针对紫外线导致的头发损害起到一定的防护作用。
本发明采用如下技术方案:
本发明提供一种具有光防护功效的护发素(pH为4-5),按总量100份计,主要由如下重量份的原料混合制备而成:1~5份阳离子表面活性剂,0.5~5份增稠剂,2~10份杏仁油,0.05~0.3份青花花香香精,0.01~1份稳定剂,0.01~1份防腐剂,以及余量的去离子水;其中,所述的阳离子表面活性剂为十六烷基三甲基氯化铵、十八烷基三甲基氯化铵、二十二烷基三甲基氯化铵中的至少一种;所述增稠剂为玉米淀粉、瓜尔豆胶、鲸蜡硬脂醇中的至少一种。
优选地,所述的阳离子表面活性剂为二十二烷基三甲基氯化铵。
优选地,所述具有光防护功效的护发素还包括茶树精油和月桂精油,杏仁油与茶树精油的重量比为2~10:1~6,杏仁油与月桂精油的重量比为2~10:1~6。
优选地,所述增稠剂为鲸蜡硬脂醇。
优选地,所述稳定剂选自羟乙基纤维素、乙二胺四乙酸二钠、柠檬酸的混合物,杏仁油与羟乙基纤维素、乙二胺四乙酸二钠、柠檬酸的重量比为6:0.5:0.05:0.1。
优选地,所述具有光防护功效的护发素由下述重量份的原料制备而成:二十二烷基三甲基氯化铵3份,鲸蜡硬脂醇3份,羟乙基纤维素0.5份,杏仁油2~6份,杏仁油2~5份,茶树精油3~5份,乙二胺四乙酸二钠0.05份,柠檬酸0.1份,尼泊金乙酯0.2份,青花花香香精0.2份,其余成分为去离子水。
本发明还提供上述所述具有光防护功效的护发素的制备方法,包括如下步骤:将阳离子表面活性剂、增稠剂、羟乙基纤维素加入少量水,加热溶解,作为A相;将稳定剂和防腐剂用余量去离子水溶解,作为B相;将溶解后的A相和B相混合,搅拌,防止产生气泡,降温至50℃以下,加入包含杏仁油的油相,继续搅拌均匀,加入青花花香香精,冷却得成品。
优选地,所述A相的加热溶解温度为75~85℃。
优选地,将A相和B相混合后从搅拌速度控制在250r/min~350r/min,防止产生气泡。
与现有技术相比,本发明的有益效果是:
本发明的护发素采用特定配比的阳离子表面活性剂、增稠剂、杏仁油、茶树精油、月桂精油以及去离子水等复配制备而成,配伍性好,成分温和,可有效降低紫外光引起的头发蛋白质、脂质、色氨酸等物质的氧化损失,起到光防护效果。
具体实施方式
下面结合具体实施例对本发明作进一步的详细说明,以使本领域的技术人员更加清楚地理解本发明。
以下各实施例,仅用于说明本发明,但不止用来限制本发明的范围。基于本发明中的具体实施例,本领域普通技术人员在没有做出创造性劳动的情况下,所获得的其他所有实施例,都属于本发明的保护范围。
在本发明实施例中,若无特殊说明,所有原料组分均为本领域技术人员熟知的市售产品;在本发明实施例中,若未具体指明,所用的技术手段均为本领域技术人员所熟知的常规手段。
试验例1
本试验例提供一种护发素,其制备方法包括如下步骤:
S1,准备如下重量份的原料:二十二烷基三甲基氯化铵4份,鲸蜡硬脂醇2份,杏仁油4份,茶树精油5份,月桂精油5份,甘油2份,乙二胺四乙酸二钠0.05份,羟乙基纤维素0.5份,柠檬酸0.1份,尼泊金乙酯0.2份,青花花香香精0.2份,其余成分为去离子水,共计100份。
S2,将二十二烷基三甲基氯化铵、鲸蜡硬脂醇和羟乙基纤维素,加入少量水,置于80±5℃恒温水浴锅中溶解,记为A相。
S3,将乙二胺四乙酸二钠、柠檬酸、尼泊金乙酯用余量去离子水溶解作为B相。
S4,将溶解后的A相、B相两混合,并以300r/min缓慢搅拌,防止产生气泡,待降温至至45℃左右加入已按比例称量的油相(含杏仁油、茶树精油、月桂精油以及甘油),继续搅拌均匀,加入青花花香香精,冷却得成品(pH值为4-5)。
试验例2
本试验例提供一种护发素,其制备方法步骤与试验例1相同,区别仅在于:鲸蜡硬脂醇3份,茶树精油3份,月桂精油3份。
试验例3
本试验例提供一种护发素,其制备方法步骤与试验例1相同,区别仅在于:二十二烷基三甲基氯化铵3份,鲸蜡硬脂醇3份,杏仁油2份,茶树精油4份。
试验例4
本试验例提供一种护发素,其制备方法步骤与试验例1相同,区别仅在于:二十二烷基三甲基氯化铵3份,鲸蜡硬脂醇3份,杏仁油8份,茶树精油2份。
试验例5
本试验例提供一种护发素,其制备方法步骤与试验例1相同,区别仅在于:二十二烷基三甲基氯化铵3份,鲸蜡硬脂醇3份,杏仁油6份,茶树精油3份,月桂精油3份。
对比例1
本试验例提供一种护发素,其制备方法步骤与试验例5相同,区别仅在于:不含杏仁油。
对比例2
本试验例提供一种护发素,其制备方法步骤与试验例5相同,区别仅在于:不含茶树精油和月桂精油。
对比例3
本试验例提供一种护发素,其制备方法步骤与试验例5相同,区别仅在于:不含杏仁油、茶树精油和月桂精油。
对比例4
本试验例提供一种护发素,其制备方法步骤与试验例5相同,区别仅在于:用等量的硅油替代杏仁油。
对比例5
本试验例提供一种护发素,其制备方法步骤与试验例5相同,区别仅在于:用等量的小麦胚芽油替代杏仁油。
选取上述实施例与对比例制备的护发素效果测试。
用温水冲洗发束,头发购自亚洲人健康黑发。每束头发按0.5gk12/1g头发的比例(K12质量分数为3%)涂抹,顺着发束方向揉搓发泡2min左右。冲洗干净,擦干头发至不滴水。按0.5g护发素/1g头发的比例涂抹均匀,静置20min。温水洗净,擦干至不滴水,吹风机冷风吹干,连续使用10天。
将经过试验例1以及对比例1至5的护发素处理的头发放于紫外灯下3.5cm处同时进行照射48h(辐射光:UVA,辐照度200μW/cm2;UVB,辐照度350μW/cm2),测试0h、48h蛋白质损失量、脂质过氧化度,色氨酸含量、拉伸强度。
其中,蛋白质含量检测的方法步骤为:(1)考马斯亮蓝染液的配制:取10mg考马斯亮蓝G250加入5mL90%乙醇(v/v)溶解,加入10mL85%(w/v)磷酸(市售磷酸≥85%),蒸馏水定容100mL过滤备用。(2)牛血清白蛋白(BSA)标液的配制:100mgBSA,蒸馏水定容到100ml,稀释10倍得到0.1mg/mL的牛血清白蛋白标准稀释液。(3)蛋白质标准曲线的绘制:依次移取0.0、0.2、0.4、0.6、0.8、1.0mL的0.1mg/mLBSA标准液至10mL试管中,蒸馏水定容至1mL,依次加入5mL考马斯亮蓝染液,涡旋混匀15s,静置2min,595nm下在紫外可见分光度计下测定吸光度。以蛋白质浓度C为横坐标,吸光度ABS为纵坐标,绘制标准曲线。标准曲线方程为y=6.9703x+0.0159,线性相关系数为0.9945。(4)取照射0h、48h的样品剪碎至0.5cm,依次取80mg左右,加入3mL的5%的十二烷基硫酸钠(SDS),在45℃、420W下超声4h后取1mL上层液,加入5mL考马斯亮蓝染液,涡旋15s混匀,静置2min后在595nm下测其吸光度。
脂质含量检测的方法步骤为:(1)0.5%硫代巴比妥酸(TBA)的配制:0.5g硫代巴比妥酸蒸馏水定容至100mL,90℃加热至完全澄清。(2)7.5%三氯乙酸的配制:7.5三氯乙酸(TCA)置于100mL容量瓶中,加入0.1g乙二胺四乙酸(EDTA),蒸馏水定容至100mL。(3)丙二醛(MDA)标准溶液的配制:0.0315g1,1,3,3-四乙氧基丙烷蒸馏水定容到100mL得100μg/mL丙二醛标准液,稀释100倍后得到1μg/mL丙二醛标准稀释液。(4)丙二醛标准曲线的绘制:依次移取0.0、0.2、0.4、0.6、0.8、1.0mL的1μg/mL的MDA标准稀释液至10毫升试管中,蒸馏水定容至1mL,依次分别加入4mL7.5%的三氯乙酸和5mL0.5%的硫代巴比妥酸,涡旋混匀15s,置于90℃下加热40min冷却后,532nm下在紫外可见分光度计下测定吸光度。以丙二醛浓度C为横坐标,吸光度ABS为纵坐标,绘制标准曲线。标准曲线方程为y=2.1724x+0.0030,线性相关系数为0.9991。取照射0h、48h的样品剪碎至0.5cm,依次取100mg左右,分别加入10mL甲醇在30℃、420W下超声10min后取8mL上层液分别加入10mL的7.5%三氯乙酸(TCA),摇床振荡30min,过滤后取滤液5mL依次加入5mL的0.5%硫代巴比妥酸(TBA),涡旋15s混匀,置于90℃下加热40min冷却,532nm下在紫外可见分光度计下测定吸光度。
色氨酸含量检测的方法步骤为:(1)色氨酸水解液的配制:取22g氢氧化钠用少量水溶解,取少量水溶解0.5g可溶性淀粉后加入NaOH溶液中定容至100mL即可配制含质量分数0.5%可溶性淀粉的5.5mol/L的氢氧化钠溶液(色氨酸水解液)。(2)pH10.5缓冲液的配制:0.5mol/L的NaH2PO4(29.99g的NaH2 PO4溶于500mL水)与0.5mol/L的NaOH(10g的NaOH溶于500mL水)以体积比为8.5∶10混合。(3)色氨酸标准溶液的配制:取10mg L-色氨酸溶于pH10.5的缓冲液中,缓冲液定容至100mL可得0.1mg/mL的色氨酸标准溶液,稀释5倍,可得0.02mg/mL的色氨酸标准稀释溶液。(4)色氨酸标准曲线的绘制:依次移取0、0.2、0.4、0.6、0.8、1.2、1.6mL的0.02mg/mL色氨酸标准稀释,用pH10.5的缓冲溶液定容至25mL。选择280nm作为激发波长,激发光谱狭缝宽度为3nm,发射光谱狭缝宽度为5nm,在270-550nm波长范围快速扫描得到色氨酸的荧光发射光谱。在最大发射波长360nm处测定荧光强度值,以色氨酸浓度C为横坐标,相对荧光强度au为纵坐标绘制标准曲线。标准曲线方程为y=1940633x-77.45094,线性相关系数为0.9985。(5)照射0h、48h的样品剪碎至0.5cm,依次取15mg左右,加入3mL色氨酸水解液,氮吹5min,抽真空后封口置于110℃烘箱水解20h,避光冷却至室温。在25mL比色管中加入3mL的6mol/L盐酸,加入水解物,用蒸馏水冲洗水解管直至冲洗完全,全部转入25mL容量瓶,用蒸馏水定容。取1mL样品液用pH10.5缓冲液的定容至5mL,和标曲用相同的条件在荧光光谱仪下测定其相对荧光强度进行定量分析。
头发拉伸强度测定的方法步骤为:取照射0h、48h的样品取相同部位剪成5cm,将头发固定在夹具之间。测定条件为Pre-Test Speed:1.67mm/sec、Test Speed:3.33mm/sec,夹具之间保持30mm,每组头发取20根进行测试,记录拉伸强度。
具体来讲,本紫外光试验中,紫外辐射可使蛋白质之间的二硫键断裂,产生小分子蛋白和多肽,水溶性增大。考马斯亮蓝法可测得溶解于水中蛋白质的量,其代表头发蛋白的损失量,进而可反映头发的损伤程度,统计结果如下表所示:
48h紫外照射下的头发蛋白质损失量变化
由上表可以看出,48h紫外照射后,相对于对比例1-5,应用试验例5的护发素后头发中的蛋白质损失率最低,表明其具有良好的保护头发蛋白质的作用。
具体来讲,头发中含有1.9%-5%的内部脂质存在于皮层细胞、角质层细胞和细胞间隙,称为细胞膜络合物,它易被紫外线甚至可见光降解氧化产生成丙二醛。48h紫外照射下的头发试验中,丙二醛生成量测试结果统计见下表:
48h紫外照射下的头发丙二醛生成量变化
由上表可以看出,48h紫外照射后,相对于对比例1-5,应用试验例5的护发素后丙二醛生成量增加率相对较低,表明其具有良好的光防护效果。
具体来讲,以色氨酸为代表的芳香族氨基酸(如酪氨酸、苯丙氨酸等)在UVB波段尤其295nm-315nm的紫外光下最不稳定,容易生成光分解产物犬尿氨酸,外观表现为头发变黄。48h紫外照射下的头发试验中,头发色氨酸含量变化统计见下表:
48h紫外照射下的头发色氨酸含量变化
由上表可以看出,48h紫外照射后,相对于对比例1-5,应用试验例5的护发素后色氨酸损失率相对较低,表明其具有良好的光防护效果。同时可以发现,替换油的种类或只使用单一的杏仁油也有一定保护效果,但无法达到同时含杏仁油、月桂精油、茶树精油的护发素的光防护效果。
具体来讲,头发主要由蛋白质和脂质构成,α-螺旋角蛋白可赋予头发良好的弹性和伸缩性。头发拉长到一定程度时,α-螺旋消失导致弹性丧失,头发断裂。在UV照射下,由于光氧化、C-S和S-S键断裂、脱羧和脱氨基导致头发更脆、更硬、更干燥,吸水能力降低,拉伸强度下降。针对头发拉伸强度的测试结果见下表:
48h紫外照射下的头发拉伸强度变化
由上表可以看出,48h紫外照射后,相对于对比例1-5,应用试验例5的护发素后,头发拉伸强度降低率最小,表明含杏仁油、月桂精油、茶树精油三者复配可有效保护头发的拉伸性能。
试验例6
本试验例还进一步探究不同表面活性剂(二十二烷基三甲基氯化铵、十六烷基三甲基氯化铵、十八烷基三甲基氯化铵和司盘60)对护发素的性能的影响,其制备方法步骤与试验例5相同,检测对比效果如下表:
不同表面活性剂对护发素性能的影响
由上表可知,不同表面活性剂对护发素的质地及对头发的抗拉伸效果都有影响,二十二烷基三甲基氯化铵在相同配方下具有一定的增稠效果,可减少增稠剂用量达到理想状态,且对头发的调理效果较好。
试验例7
本试验例探究不同增稠剂(鲸蜡硬脂醇、玉米淀粉、瓜尔豆胶)对护发素的性能的影响,其制备方法步骤与试验例5相同,检测对比效果如下表:
不同增稠剂对护发素性能的影响
由上表可以看出,不同增稠剂对护发素的质地及头发的抗拉伸效果都有影响,鲸蜡硬脂醇增稠效果明显优于玉米淀粉和瓜尔豆胶,且溶解性较好。在相同配方下可使护发素形成乳白色膏体状态,柔滑水润。
试验例8
本试验例探究不同杏仁油与精油配比对自由基清除性能的影响,检测方法为向2.5mL 65μmol/L DPPH溶液中加入0.5mL已用无水乙醇稀释到稀释度为1%的试样(空白对照用等量无水乙醇代替),用力摇匀。于室温下放置30min后于光径1cm比色皿中测定DPPH·混合液在517nm处吸光值,用2.5mL乙醇与0.5mL试样混合液调零,以扣除试样本身颜色的影响。
DPPH清除率%=(A0-A样)/A0×100
检测对比效果如下表:
不同杏仁油、精油配比对DPPH清除率的影响
含油1wt%的油无水乙醇溶液 | DPPH清除率(%) |
仅含杏仁油 | 9.0623 |
仅含月桂精油 | 8.2344 |
仅含茶树精油 | 3.0159 |
杏仁油、月桂精油茶树精油的质量比8:2:5 | 49.0134 |
杏仁油、月桂精油茶树精油的质量比6:3:3 | 64.0379 |
杏仁油、月桂精油茶树精油的质量比4:5:5 | 69.7472 |
杏仁油、月桂精油茶树精油的质量比2:4:5 | 67.6145 |
由上表可以看出,杏仁油、月桂精油、茶树精油混合物的DPPH自由基清除效果优于单一油脂的自由基清除效果,说明该杏仁油与月桂精油、茶树精油组合能够协同增效,具有较好自由基清除效果。
在此有必要指出的是,以上实施例仅限于对本发明的技术方案做进一步的阐述和说明,并不是对本发明的技术方案的进一步的限制,本发明的方法仅为较佳的实施方案,并非用于限定本发明的保护范围。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种具有光防护功效的护发素,其特征在于,按总量100份计,由如下重量份的原料混合制备而成:二十二烷基三甲基氯化铵4份,鲸蜡硬脂醇2份,杏仁油4份,茶树精油5份,月桂精油5份,甘油2份,乙二胺四乙酸二钠0.05份,羟乙基纤维素0.5份,柠檬酸0.1份,尼泊金乙酯0.2份,青花花香香精0.2份,以及余量的去离子水。
2.一种具有光防护功效的护发素,其特征在于,按总量100份计,由如下重量份的原料混合制备而成:二十二烷基三甲基氯化铵3份,鲸蜡硬脂醇3份,杏仁油6份,茶树精油3份,月桂精油3份,甘油2份,乙二胺四乙酸二钠0.05份,羟乙基纤维素0.5份,柠檬酸0.1份,尼泊金乙酯0.2份,青花花香香精0.2份,以及余量的去离子水。
3.一种如权利要求1或2所述具有光防护功效的护发素的制备方法,其特征在于,包括如下步骤:
将二十二烷基三甲基氯化铵、鲸蜡硬脂醇、羟乙基纤维素加入少量水,加热溶解,作为A相;
将乙二胺四乙酸二钠、柠檬酸、尼泊金乙酯用余量去离子水溶解,作为B相;
将溶解后的A相和B相混合,搅拌,防止产生气泡,降温至50℃以下,加入包含杏仁油、茶树精油、月桂精油、甘油的油相,继续搅拌均匀,加入青花花香香精,冷却得成品。
4.根据权利要求3所述的具有光防护功效的护发素的制备方法,其特征在于,所述A相的加热溶解温度为75~85℃。
5.根据权利要求3所述的具有光防护功效的护发素的制备方法,其特征在于,将A相和B相混合后搅拌速度控制在250 r/min ~350r/min,防止产生气泡。
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