CN117084958A - 一种复配型天然中药材提取物防晒霜及其制备、检测方法 - Google Patents
一种复配型天然中药材提取物防晒霜及其制备、检测方法 Download PDFInfo
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Abstract
本发明涉及护肤品技术领域,特别是一种复配型天然中药材提取物防晒霜及其制备、检测方法。本发明提供一种天然中药材提取物配置的防晒霜,同时给出防晒霜的制备工艺以满足批量产品质量稳定,为保证防晒霜的防晒效果给出具体测定的方案。具体效果为:1、原料廉价易得,成本低;2、工艺简单,反应条件温和,对人体不产生额外伤害,此点明显优于现有防晒产品,生产能耗低绿色环保;3、后加工和处理工艺便捷容易;4、产物的收率高,品质好。
Description
技术领域
本发明涉及护肤品技术领域,特别是一种复配型天然中药材提取物防晒霜及其制备、检测方法。
背景技术
现有技术及市销的防晒型护肤产品多由防晒功能性化学成分配制,虽然在防晒上具有一定功效,但其他性能指标不佳,同时防晒型护肤产品暴露在阳光紫外线下,部分使用者对防晒功能的化学添加剂会出现过敏现象。防晒霜的整体使用效果不理想。
以专利号CN 115252454 A、名称《一种防晒霜及其制备方法》的发明为例,该技术制备方法与本发明接近,均为油相制备至高温后与水相混合冷却至室温制得,该技术的主要防晒成分为化学成分四氢嘧啶(Ectoine)和羟基四氢嘧啶(5-hydroxyectoine),并添加天然植物提取物作为乳化剂辅助美白、抗衰、抗氧化、保湿等,试验例进行了人群斑贴试验、感官理化指标及卫生指标的检验。该专利使用“脱氢乙酸钠”这一化学品为防腐剂,加入标准符合国家安全要求,但从长期使用的角度来说,针对损伤性皮肤、敏感性、特殊体质人群等,化学防腐剂渗入皮肤日久可能会引起过敏反应甚至肝、肾和中枢神经***的损伤。而本发明使用天然的化妆品文化植物防腐剂牡丹根皮提取物,利用了传统中药的阵痛、抗敏、消炎作用,再通过其与丙二醇的复配增加其与其他成分的溶解度,避免了传统化妆品化学防腐剂可能造成的危害。此外,该专利主要从安全性和吸收效果等角度对防晒霜进行了评价,未提供防晒霜的紫外吸收效果(防晒效果)相关数据。
本申请研究采用多种复配的天然植物应用于防晒霜,以解决现有技术中存在的不足满足市场需求,通过在***溶剂中及3M胶带薄膜中的紫外吸光度进行了检测与比较,从而获得了紫外吸收效果较好的天然中药材提取物复配的防晒霜。
发明内容
本发明旨在提供一种工艺简单,反应条件温和,无化学添加防腐剂、无化学、物理防晒成分以天然中药材提取物复配为基底的防晒霜制备方法。
现有化学防晒剂存在光稳定性差和小分子渗入皮肤造成化学残留等缺点,而且如果选择的是含有铅、汞成份的防晒剂,长期使用会造成皮肤的依赖性,对皮肤细胞和结构造成破损。而天然中药材(即植物)防晒剂,对皮肤作用温和,刺激性小,安全性高,且资源丰富,可弥补化学防晒剂的缺点。
一种复配型天然中药材提取物防晒霜,包括如下重量份成分组成:天然植物复配提取液10-15份、硬脂酸10-15份、单硬脂酸甘油酯0.5-2份、十六醇0.5-2份、白油0.5-2份、丙二醇5-10份、氢氧化钾0.1-1份、香精0.1-1份、牡丹根皮提取物0.1-1份、氢氧化钠0.1-1份、去离子水60-80份。
所述天然植物复配提取液10份、硬脂酸11.7份、单硬脂酸甘油酯0.7份、十六醇0.7份、白油0.7份、丙二醇7份、氢氧化钾0.4份、香精0.2份、牡丹根皮提取物0.2份、氢氧化钠0.1份、去离子水68.3份;牡丹根皮提取物中牡丹根皮质量体积比m/v%大于等于6%,pH值4.0±1,比重1.02±0.05,凝固点-20摄氏度。
所述天然植物复配提取液由鼠尾草、红景天、红花或银杏提取液组成。
所述天然植物复配提取液由鼠尾草和红景天提取物按质量比1:1混合制得;或红景天和红花提取物按质量比1:1混合制得;或银杏和红花提取物按质量比1:1混合制得。
一种复配型天然中药材提取物防晒霜的制备方法,包括如下步骤:
(1)油相的制备:按质量分数称取硬脂酸、单硬脂酸甘油酯、十六醇、白油、丙二醇于90℃恒温水浴锅中搅拌均匀;
(2)水相的制备:按质量分数称取天然植物1:1复配提取液、氢氧化钾、氢氧化钠,去离子水置于90℃恒温水浴锅中搅拌均匀至全部溶解;
(3)在90℃恒温水浴下将油相倒入水相,立刻搅拌均匀得二者混合物乳液,将混合乳液拿出水浴锅室温冷却至40℃-50℃,至触感温热、质地粘稠时,按质量分数加入香精和牡丹根皮提取物;
(4)冷却至室温,搅拌均质后,得到均匀的霜剂,灭菌装罐。
一种复配型天然中药材提取物防晒霜的检测方法,包括如下步骤:精密称取每份天然中药复配防晒霜样品100±1 mg,无水乙醇与无水***按体积比v/v 1:1的混合溶剂,天然中药复配防晒霜样品与混合溶剂混合,超声溶解定容配制成防晒霜含量为2.0 mg/ml的防晒霜母液,将母液加水稀释40倍,并通过0.45 μm的滤膜过滤后制得成品,成品倒入光径1 cm的石英比色池,在紫外可见分光光度计上测定200-450 nm波长范围的紫外吸光度值。上述方法充分溶解了发挥紫外吸收功能的成分,检测灵敏度更高。
另一种复配型天然中药材提取物防晒霜的检测方法,包括如下步骤:将3M胶带剪成1cm×4cm大小,粘贴在载玻片上;精密称取16±1 mg 上每份天然中药材复配防晒霜样品并将样品均匀涂抹在3M胶带上;将载玻片置于35°C干燥箱中干燥30min;将涂有待测样品的3M胶带从载玻片上轻轻取下粘贴在石英比色皿透光侧表面上,置于紫外可见光分光光度计光路中,取另一贴有3M胶带的石英比色皿置于参比光路中,扫描280~400nm的紫外吸光度。本测定法适用于所有固体、半固体、乳液状及本申请制备的天然中药材复配防晒霜,检测时能够保持产品的原相态。
本发明提供一种天然中药材提取物配置的防晒霜,同时给出防晒霜的制备工艺以满足批量产品质量稳定,为保证防晒霜的防晒效果给出具体测定的方案。具体效果为:1、原料廉价易得,成本低;2、工艺简单,反应条件温和,对人体不产生额外伤害,此点明显优于现有防晒产品,生产能耗低绿色环保; 3、后加工和处理工艺便捷容易;4、产物的收率高,品质好。
附图说明
图1为天然植物复配UVA及UVB区紫外平均吸光度值对比效果图
图2为防晒霜微生物限度检查平皿实验展示图;
图3为紫外灯照射后小鼠表皮损伤情况示意图。
具体实施方式
一种复配型天然中药材提取物防晒霜,包括如下重量份成分组成:天然植物复配提取液10-15份、硬脂酸10-15份、单硬脂酸甘油酯0.5-2份、十六醇0.5-2份、白油0.5-2份、丙二醇5-10份、氢氧化钾0.1-1份、香精0.1-1份、牡丹根皮提取物0.1-1份、氢氧化钠0.1-1份、去离子水60-80份。
所述天然植物复配提取液10份、硬脂酸11.7份、单硬脂酸甘油酯0.7份、十六醇0.7份、白油0.7份、丙二醇7份、氢氧化钾0.4份、香精0.2份、牡丹根皮提取物0.2份、氢氧化钠0.1份、去离子水68.3份;牡丹根皮提取物中牡丹根皮质量体积比m/v%大于等于6%,pH值4.0±1,比重1.02±0.05,凝固点-20摄氏度。
所述天然植物复配提取液由鼠尾草、红景天、红花或银杏提取液组成。
所述天然植物复配提取液由鼠尾草和红景天提取物按质量比1:1混合制得;或红景天和红花提取物按质量比1:1混合制得;或银杏和红花提取物按质量比1:1混合制得。
一种复配型天然中药材提取物防晒霜的制备方法,包括如下步骤:
(1)油相的制备:按质量分数称取硬脂酸、单硬脂酸甘油酯、十六醇、白油、丙二醇于90℃恒温水浴锅中搅拌均匀;
(2)水相的制备:按质量分数称取天然植物1:1复配提取液、氢氧化钾、氢氧化钠,去离子水置于90℃恒温水浴锅中搅拌均匀至全部溶解;
(3)在90℃恒温水浴下将油相倒入水相,立刻搅拌均匀得二者混合物乳液,将混合乳液拿出水浴锅室温冷却至40℃-50℃,至触感温热、质地粘稠时,按质量分数加入香精和牡丹根皮提取物;
(4)冷却至室温,搅拌均质后,得到均匀的霜剂,灭菌装罐。
一种复配型天然中药材提取物防晒霜的检测方法,包括如下步骤:精密称取每份天然中药复配防晒霜样品100±1 mg,无水乙醇与无水***按体积比v/v 1:1的混合溶剂,天然中药复配防晒霜样品与混合溶剂混合,超声溶解定容配制成防晒霜含量为2.0 mg/ml的防晒霜母液,将母液加水稀释40倍,并通过0.45 μm的滤膜过滤后制得成品,成品倒入光径1 cm的石英比色池,在紫外可见分光光度计上测定200-450 nm波长范围的紫外吸光度值。上述方法充分溶解了发挥紫外吸收功能的成分,检测灵敏度更高。
另一种复配型天然中药材提取物防晒霜的检测方法,包括如下步骤:将3M胶带剪成1cm×4cm大小,粘贴在载玻片上;精密称取16±1 mg 上每份天然中药材复配防晒霜样品并将样品均匀涂抹在3M胶带上;将载玻片置于35°C干燥箱中干燥30min;将涂有待测样品的3M胶带从载玻片上轻轻取下粘贴在石英比色皿透光侧表面上,置于紫外可见光分光光度计光路中,取另一贴有3M胶带的石英比色皿置于参比光路中,扫描280~400nm的紫外吸光度。本测定法适用于所有固体、半固体、乳液状及本申请制备的天然中药材复配防晒霜,检测时能够保持产品的原相态。
本专利所选取的原料价低易得,天然中药提取物均拥有稳定的供货渠道,反应条件温和,无需使用高压反应釜等工艺要求过高的反应容器,产品质地均匀,紫外吸收(防晒)效果好。
名词说明:1.紫外线分UVB、UVA两种。2.UVB的伤害和防护已经得到彻底的研究,它可以使皮肤在短时间内晒伤、晒红(对一般人来说是25分钟左右),现市场上绝大多数防晒品是UVB型的,SPF就是UVB防护能力的标志。3.UVA是可怕的阳光杀手,它藉着波长比较长,穿透能力强的本领,可以穿透皮肤表层,深入真皮以下组织,可以破坏胶原蛋白,一般强度的阳光UVA照射在皮肤上,约经过2-4小时,皮肤就会出现比较稳定的黑化。
附表一:三种复配型天然防晒霜提取物液体紫外测定法吸收数据
附表二:三种复配型天然中药材防晒霜液体紫外测定法下UVA及UVB区平均紫外吸收值
。
附表三:三种复配型天然中药防晒霜3M胶带测定法紫外吸收数据
。
附表四:三种复配型天然中药材防晒霜3M胶带测定法下UVA及UVB区平均紫外吸收值
。
实施例一:
本发明采用1:1复配提取液10%、硬脂酸11.7%、单硬脂酸甘油酯0.7%、十六醇0.7%、白油0.7%、丙二醇7%、、氢氧化钾0.4%、香精0.2%、牡丹根皮提取物0.2%,氢氧化钠0.1%及去离子水余量制备而成。
(1)油相的制备:按质量分数称取硬脂酸(11.7%)、单硬脂酸甘油酯(0.7%)、十六醇(0.7%)、白油(0.7%)、丙二醇(7%)于90℃恒温水浴锅中搅拌均匀;
(2)水相的制备:按质量分数称取红花:红景天(1:1复配提取液)10%,或红景天:鼠尾草(1:1复配提取液)10%,或红花:银杏(1:1复配提取液)10%、氢氧化钾0.4%、氢氧化钠0.1%,去离子水置于90℃恒温水浴锅中搅拌均匀至全部溶解。
(3)在90℃恒温水浴下将油相倒入水相,立刻搅拌均匀得二者混合物乳液,将混合乳液拿出水浴锅室温冷却至40℃-50℃(触感温热,质地粘稠)时,按质量分数加入香精0.2%和牡丹根皮提取物0.2%。
(4)冷却至室温,搅拌均质后,得到均匀的霜剂,灭菌装罐。
(5)精密称定每份天然中药复配防晒霜样品100 mg,添加无水乙醇:无水***按1:1(v:v)的混合溶剂超声溶解后在50 ml容量瓶定容作为母液。将母液利用容量瓶稀释40倍,并通过0.45 μm的滤膜过滤后,倒入光径1 cm的石英比色池,以无水乙醇:无水***1:1(v:v)混合溶剂为参比,在紫外-可见分光光度计上测定200-450 nm波长范围的紫外吸光度值。
(6)将290-320nm的紫外吸光度值按下列公式计算防晒霜的SPF值
实施例二:
本发明采用1:1复配提取液10%、硬脂酸11.7%、单硬脂酸甘油酯0.7%、十六醇0.7%、白油0.7%、丙二醇7%、、氢氧化钾0.4%、香精0.2%、牡丹根皮提取物0.2%,氢氧化钠0.1%及去离子水余量制备而成。
(1)按实施例一的方案(1)-(4)制备三种天然中药材复配的防晒霜样品。
(2)将3M胶带剪成1cm×4cm大小,粘贴在载玻片上。用分析天平精确称取16mg上述三种防晒霜样品并将样品均匀涂抹在3M胶带上。将载玻片置于35°C干燥箱中干燥30min。将涂有待测样品的3M胶带从载玻片上轻轻取下粘贴在石英比色皿透光侧表面上,置于紫外可见光分光光度计光路中,取另一贴有3M胶带的石英比色皿置于参比光路中,扫描280~400nm的紫外吸光度。
(3)将290-320nm的紫外吸光度值按下列公式计算防晒霜的SPF值
两种实施例中复配中药材SPF值见附表二
复配中药材 | 红花/红景天 | 红花/银杏 | 红景天/鼠尾草 |
实例一 SPF值 | 26.22 | 18.63 | 23.70 |
实例二 SPF值 | 12.21 | 6.59 | 12.36 |
实施例三
根据上述SPF值结果,选用红花:红景天提取液复配的自制天然防晒霜进行下述实施例。
本发明采用1:1红花:红景天复配提取液10%、硬脂酸11.7%、单硬脂酸甘油酯0.7%、十六醇0.7%、白油0.7%、丙二醇7%、、氢氧化钾0.4%、香精0.2%、牡丹根皮提取物0.2%,氢氧化钠0.1%及去离子水余量制备而成。
(1)油相的制备:按质量分数称取硬脂酸(11.7%)、单硬脂酸甘油酯(0.7%)、十六醇(0.7%)、白油(0.7%)、丙二醇(7%)于90℃恒温水浴锅中搅拌均匀;
(2)水相的制备:按质量分数称取红花:红景天(1:1复配提取液)10%,氢氧化钾0.4%、氢氧化钠0.1%,去离子水置于90℃恒温水浴锅中搅拌均匀至全部溶解。
(3)在90℃恒温水浴下将油相倒入水相,立刻搅拌均匀得二者混合物乳液,将混合乳液拿出水浴锅室温冷却至40℃-50℃(触感温热,质地粘稠)时,按质量分数加入香精0.2%和牡丹根皮提取物0.2%。
(4)冷却至室温,搅拌均质后,得到均匀的霜剂,灭菌装罐。
(5)使用平板计数培养基,配制固体平板计数培养基。
(6)防晒霜稀释液的制备:取上述(1)-(3)步骤中制备的防晒霜样品1 g加1 ml灭菌液体石蜡、1 ml灭菌吐温80、7 ml灭菌生理盐水,均质3-5 min。用灭菌吸管吸取1:10稀释的检测样品3 ml,分别注入到三个灭菌平皿内,每皿1 ml。另取1 ml注入到9 ml灭菌生理盐水试管中,更换一只吸管,并充分混匀,使成1:100稀释液。吸取3 ml,分别注入到三个灭菌平皿内,每皿1 ml,同理制成1:1000稀释倍数。
(5)将灭菌并降温至45~50°C的培养基倾注平皿内,每皿约15 ml,另倾注一个不加样的灭菌空平皿,作空白对照。随即转动平皿,使样品与培养基充分混合均匀,待琼脂凝固后,转动平皿,置37℃培养箱内培养48 h。
(6)按GB7918.1-87《化妆品微生物标准检验方法》总则检验自制防晒霜的微生物生长情况。
经检验,制备的防晒霜经1:10、1:100、1:1000稀释液在37℃培养箱中培养96 小时候经显微镜观察均无菌落长出,符合国家标准。另将培养皿密封常温(非无菌环境下)放置30天后,于显微镜中观察,仍无菌落长出,符合化妆品微生物限度标准。
实施例四
(1)按实施例一的方案(1)-(4)制备红花-红景天复配的防晒。
(3)使用平板计数培养基,配制固体平板计数培养基。
(4)防晒霜稀释液的制备:取上述(1)-(3)步骤中制备的防晒霜样品1 g加1 ml灭菌液体石蜡、1 ml灭菌吐温80、7 ml灭菌生理盐水,均质3-5 min。用灭菌吸管吸取1:10稀释的检测样品3 ml,分别注入到三个灭菌平皿内,每皿1 ml。另取1 ml注入到9 ml灭菌生理盐水试管中,更换一只吸管,并充分混匀,使成1:100稀释液。吸取3 ml,分别注入到三个灭菌平皿内,每皿1 ml,同理制成1:1000稀释倍数。
(5)取四只BALB/c小鼠编号1,2,3,4,并用脱毛仪去除背部毛发,分为涂抹区和空白对照区,1号小鼠不涂抹任何产品,2号小鼠涂抹普通护肤霜,3号小鼠涂抹市售成品防晒霜,4号小鼠涂抹天然植物防晒霜。模拟人体照太阳光条件,将小鼠置于320nm紫外光下,持续2天,每天8小时,于每天紫外光照结束后对其拍照。
与1号对照组小鼠相比,涂抹护肤成分,商用防晒霜和自制防晒霜均能有效保护小鼠表皮皮肤的红肿痛痒,说明产生的保护膜能起到反射紫外光照射的作用,但因紫外照射时间不长且强度较低,也无法保证每时每刻每只小鼠受到的光照强度均等,故而无法区分润肤霜,自制防晒霜与商用防晒霜对小鼠耐受紫外吸收效果的区别。
Claims (7)
1.一种复配型天然中药材提取物防晒霜,其特征在于包括如下重量份成分组成:天然植物复配提取液10-15份、硬脂酸10-15份、单硬脂酸甘油酯0.5-2份、十六醇0.5-2份、白油0.5-2份、丙二醇5-10份、氢氧化钾0.1-1份、香精0.1-1份、牡丹根皮提取物0.1-1份、氢氧化钠0.1-1份、去离子水60-80份。
2.根据权利要求1所述的一种复配型天然中药材提取物防晒霜,其特征在于:所述天然植物复配提取液10份、硬脂酸11.7份、单硬脂酸甘油酯0.7份、十六醇0.7份、白油0.7份、丙二醇7份、氢氧化钾0.4份、香精0.2份、牡丹根皮提取物0.2份、氢氧化钠0.1份、去离子水68.3份;牡丹根皮提取物中牡丹根皮质量体积比m/v%大于等于6%,pH值4.0±1,比重1.02±0.05,凝固点-20摄氏度。
3.根据权利要求1所述的一种复配型天然中药材提取物防晒霜,其特征在于:所述天然植物复配提取液由鼠尾草、红景天、红花或银杏提取液组成。
4.根据权利要求3所述的一种复配型天然中药材提取物防晒霜,其特征在于:所述天然植物复配提取液由鼠尾草和红景天提取物按质量比1:1混合制得;或红景天和红花提取物按质量比1:1混合制得;或银杏和红花提取物按质量比1:1混合制得。
5.根据权利要求1至4任一项所述的一种复配型天然中药材提取物防晒霜的制备方法,其特征在于包括如下步骤:
(1)油相的制备:按质量分数称取硬脂酸、单硬脂酸甘油酯、十六醇、白油、丙二醇于90℃恒温水浴锅中搅拌均匀;
(2)水相的制备:按质量分数称取天然植物1:1复配提取液、氢氧化钾、氢氧化钠,去离子水置于90℃恒温水浴锅中搅拌均匀至全部溶解;
(3)在90℃恒温水浴下将油相倒入水相,立刻搅拌均匀得二者混合物乳液,将混合乳液拿出水浴锅室温冷却至40℃-50℃,至触感温热、质地粘稠时,按质量分数加入香精和牡丹根皮提取物;
(4)冷却至室温,搅拌均质后,得到均匀的霜剂,灭菌装罐。
6.根据权利要求1至4任一项所述的一种复配型天然中药材提取物防晒霜的检测方法,其特征在于包括如下步骤:精密称取每份天然中药复配防晒霜样品100±1 mg,无水乙醇与无水***按体积比v/v 1:1的混合溶剂,天然中药复配防晒霜样品与混合溶剂混合,超声溶解定容配制成防晒霜含量为2.0 mg/ml的防晒霜母液,将母液加水稀释40倍,并通过0.45 μm的滤膜过滤后制得成品,成品倒入光径1 cm的石英比色池,在紫外可见分光光度计上测定200-450 nm波长范围的紫外吸光度值。
7.根据权利要求1至4任一项所述的一种复配型天然中药材提取物防晒霜的检测方法,其特征在于包括如下步骤:将3M胶带剪成1cm×4cm大小,粘贴在载玻片上;精密称取16±1mg 上每份天然中药材复配防晒霜样品并将样品均匀涂抹在3M胶带上;将载玻片置于35°C干燥箱中干燥30min;将涂有待测样品的3M胶带从载玻片上轻轻取下粘贴在石英比色皿透光侧表面上,置于紫外可见光分光光度计光路中,取另一贴有3M胶带的石英比色皿置于参比光路中,扫描280~400nm的紫外吸光度。
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