CN115531253B - 一种淡香型香水及其制备方法 - Google Patents
一种淡香型香水及其制备方法 Download PDFInfo
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- CN115531253B CN115531253B CN202210526095.5A CN202210526095A CN115531253B CN 115531253 B CN115531253 B CN 115531253B CN 202210526095 A CN202210526095 A CN 202210526095A CN 115531253 B CN115531253 B CN 115531253B
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Abstract
本发明公开了一种淡香型香水，本发明的淡香型香水含有石楠花精油。发明人创造性的通过在提取时在提取液中加入醋酸水溶液可完全消除石楠花的腥臭异味，并且本发明的提取工艺能够避免提取花青素等水溶性成分。通过加入醋酸水溶液的特殊工艺，可使得制备得到的香水有更好的人群接受度。
Description
技术领域
本发明属于化妆品领域，具体涉及一种淡香型香水及其制备方法。
背景技术
随着生活水平的逐步提高，人们对化妆品的需求也越来越高，香水由之前的奢侈物品变成了大众的常用物品。香水是一种混合了香精油、固定剂与酒精的液体，用来让物体(通常是人体部位)拥有持久且悦人的气味。香精油是取自于花草植物的蒸馏，每种香水都含有三种香调：前调、中调、后凋。随着人们生活水平的提高，对于香水的使用也愈加频繁，香水的种类多样但一般过于老套，从而限制了香水的发展。
浙江省是植物资源相当丰富，全省约有高等植物4550余中，其中可以开花的植物有三千余种，花瓣精油是制备天然香水的重要原料，因此，浙江具有成本低廉、种类丰富的天然香水提取资源。
石楠，学名Photinia serrulata Lindl.，英文名称为Photinia，别名千年红、扇骨木等。石楠是蔷薇科石楠属常绿灌木或小乔木，原产于中国，在浙江、江苏、江西等地区分布广泛。花期4—5月，果期10月。圆形树冠，叶丛浓密，嫩叶红色，花白色、密生，冬季果实红色，鲜艳著目，是常见的栽培树种。石楠的叶和根可供药用，为强壮剂、利尿剂，有镇静解热等作用。传统中药领域对石楠的应用主要是用石楠叶，石楠叶具有祛风止痛的功效，但是石楠花的应用较少。石楠花在花季开放时香气过于浓烈，存在一种刺鼻气味，其原因是石楠花中含有一种三甲胺的物质，具有腥臭气味，这大大限制了石楠花作为香水的应用。
石楠花已有制备成化妆品的进展，CN106138870A公开了一种含有石楠叶的中药面膜，具有治疗痤疮的功效，但其使用了十余味中药，成分复杂，制备困难，不适合商业化使用。
目前市场上存在多种留香持有的香水，但是总体的留香水平还并不是很高；另外，消费者还存在着对留香持久的天然香水的诉求，目前市场上留香持有的天然香水品种也较少。
虽然已有专利公开了采用石楠叶制备化妆品，但是现有技术还未见采用石楠花制备香水的专利记载。
有鉴于此，有必要开发一种以天然香料为主要原料，香味持久留香的香水。
发明内容
本发明的目的在于提供一种绿色天然、留香持久的淡香型香水，具体涉及一种含有石楠花精油的香水。并且本发明还解决了石楠花具有腥臭异味不能直接用于制作香水的技术缺陷。
一方面，本发明提供了一种淡香型香水，其含有石楠花精油。
作为对本发明的进一步限定，所述的石楠花精油在提取过程中经过酸处理。
作为本发明的酸处理的方法，可以采用有机酸或无机酸，无机酸可以为稀盐酸、稀硫酸、磷酸等；有机酸可以为醋酸、酒石酸、柠檬酸、苯甲酸、草酸等；本发明选择的酸优选有机酸，尤其是醋酸。有机酸的酸性温和，不会破坏花香的基香。无机酸也可作为本发明石楠花精油提取过程中使用的酸，但是无机酸会破坏花香的基香，效果不如有机酸好。
在有机酸处理的技术上，本发明的石楠花精油进一步可以采用多种方法进行精制，常规的精油制备方法制备得到的石楠花精油均可满足本发明石楠花香水的制备，石楠精油可以采用分子蒸馏法、水蒸气蒸馏法、冷浸法或二氧化碳超临界萃取法等方法制备，优选可按照如下方法制备：
步骤一：将石楠花干燥后粉碎至粒径为100～300目的颗粒。更优选的，粉碎至粒径为200～300目的颗粒，石楠花干燥至含水量为5%-10%。
步骤二：粉碎后的石楠花用非极性有机溶剂提取2～3次，过滤后合并滤液得过滤液；所述的非极性有机溶剂为乙酸乙酯、二氯甲烷、乙醚、石油醚或其混合物。优选的，为乙酸乙酯和石油醚的混合物，乙酸乙酯的体积占总的非极性有机溶剂的体积为50％～99％，更优选为75％～95％。
步骤三：向步骤二得到的过滤液中加入0.5-2%醋酸水溶液，搅拌后沉淀30min-1h，过滤，得石楠花提取液；醋酸水溶液优选1%醋酸水溶液。醋酸水溶液的加入量为过滤液的5%-40%，优选15%。本发明名的1%醋酸水溶液为质量比，即醋酸质量占醋酸水溶液总质量百分比。
步骤四：采用分子蒸馏法对所述石楠花提取物进行分离，将步骤三得到的石楠花提取液放入分子蒸馏装置中，逐渐减少真空度值，所述真空度范围为10-2-102Pa，依次得到首段、中段和尾段提取物；其中，首段提取物指真空提取5-20min的产物，尾段提取物指真空提取75min至结束的产物，中段提取物指20-75min的提取产物，中段产物即为本发明的石楠花精油。
作为对本发明的进一步限定，所述的淡香型香水中石楠花精油在香水中的含量为0.01wt％～8wt％，优选为0.05wt％～5wt％。
作为对本发明的进一步限定，所述的淡香型香水中石楠精油按照如下方法制备：
步骤一：将10g石楠花干燥后粉碎至粒径为200目的颗粒，石楠花干燥至含水量为8%。
步骤二：粉碎后的石楠花用非极性有机溶剂提取2次，过滤后合并滤液得过滤液；所述的非极性有机溶剂为乙酸乙酯和石油醚的混合物，乙酸乙酯的体积占总的非极性有机溶剂的体积为90％。
步骤三：向步骤二得到的过滤液中加入过滤液的15%的1%醋酸水溶液，搅拌后沉淀30min，过滤，得石楠花提取液。
步骤四：采用分子蒸馏装置对所述石楠花提取物进行分离，逐渐减少真空度的值，所述真空度范围为10-2-102Pa，依次得到首段、中段和尾段提取物，弃去首段和尾段提取物，仅保留中段产物；其中，首段提取物指真空提取5-20min的产物，尾段提取物指真空提取75min至结束的产物，中段提取物指20-75min的提取产物，中段产物即为本发明的石楠花精油。
石楠花中含有味道腥臭味的三甲胺及其他刺激性气味的碱性物质，在香水制备领域，具有腥臭味的原料是不适合制备香水的，石楠花资源丰富，原料成本低。采用醋酸水溶液水洗后，三甲胺及其他刺激性气味的碱性物质和醋酸会成盐后沉淀析出，通过过滤除去。本发明采用非极性有机溶剂可以高效率提取脂溶性的香味物质，并且能够避免提取花青素等水溶性物质，使得本发明石楠花精油香味浓郁，并且使得本发明的石楠花精油具有透明的优良颜色，适合制备香水。因此，本发明的生产工艺可有效去除石楠花中的三甲胺及其他刺激性味道腥臭的物质，使得本发明的石楠花精油能够满足化妆品的要求，尤其是适合香水的制备。
进一步，本发明公开一种淡香型石楠花精油香水，由以下重量的原料组成：石楠花精油3-10份，乙醇90-300份，玫瑰香精1-5份、紫罗兰酮1-5份、香豆素1-5份，苯乙醇2-6份，苯乙醛1-5份，乙酸苄酯1-5份。制备方法包括以下步骤：
1）石楠花精油按上述提取方法得到；
2)将乙醇倒入玻璃瓶内，依次将石楠花精油、玫瑰香精、紫罗兰酮和香豆素加入，搅拌均匀。
3)然后将苯乙醇、苯乙醛和乙酸苄酯加入到步骤2）的溶液中即得淡香型石楠花精油香水。
除此之外，本发明的石楠花精油可以和多种香精香料搭配制备不同风格的香水，如淡香型玫瑰香水，淡香型风铃香水，淡香型
香豆素（Coumarin），分子式为C9H6O2，呈白色结晶固体，存在于黑香豆、香蛇鞭菊、野香荚兰、兰花中，具有新鲜干草香和香豆香，一般不作食用，可用于香水的制作。
香兰素，又名香草醛，化学名称为3-甲氧基-4-羟基苯甲醛，是从芸香科植物香荚兰豆中提取的一种有机化合物，为白色至微黄色结晶或结晶状粉末，微甜，溶于热水、甘油和酒精，在冷水及植物油中不易溶解。香气稳定，在较高温度下不易挥发。在空气中易氧化，遇碱性物质易变色。
玫瑰香精即乙酸三氯甲基苯甲酯，分子式是C10H9O2Cl3，有玫瑰香气，甜中带些青苦气息，还有些粉香、膏香气息。
紫罗兰酮（α-Ionone）是一种有机化合物，分子式为C13H20O，无色至微黄色液体。呈暖的木香和具有较强的紫罗兰香气。香味比p紫罗兰酮好。溶于乙醇、丙二醇、大多数非挥发性油和矿物油。天然品存在于金合欢油、桂花浸膏等中。主要用以配制香精。
本发明所用的石楠，学名Photinia serrulata Lindl.，英文名称为Photinia，别名千年红、扇骨木等。石楠为蔷薇科石楠属常绿灌木或小乔木，原产于中国。本发明所用的石楠的植物部位为花瓣。
本发明的石楠花精油可以用于制备淡香型香水，本发明的石楠花精油香水对香水的种类并无特殊的限制，尤其适合制备成淡香型香水。
石楠花具有腥臭异味，化妆品领域的常规认识是有腥臭异味的成分不能作为化妆品的主要活性成分之一，尤其是不能作为香水的活性成分，发明人创造性的通过在提取工艺中在提取液中加入醋酸水溶液可完全消除石楠花的腥臭异味，并且本发明的提取工艺能够避免提取花青素等水溶性成分，取得了预料不到的技术效果。通过加入醋酸水溶液的特殊工艺，可使得制备得到的香水有更好的人群接受度。并且经过酸处理的石楠花精油具有较好的色泽，适合制备成高端香水。
说明书附图
附图1为本发明实施例5和市售香水的留香实验结果。
具体实施例
下面结合具体的实施例对发明内容作进一步的解释和说明，但是，它们并不构成对本发明范围的限制或限定。
本发明的实施例所用的原料和实验设备可通过商业化购买渠道获得，如部分原料可采购自江苏普乐司生物科技有限公司；香味测试可采用德国Airsens 公司PEN3 型电子鼻。
实施例1
步骤一：将10g石楠花干燥后粉碎至粒径为200目的颗粒，石楠花干燥至含水量为8%。
步骤二：粉碎后的石楠花用200ml乙酸乙酯占比90%的乙酸乙酯和石油醚的混合有机溶剂提取2次，过滤后合并滤液得过滤液。
步骤三：向步骤二得到的过滤液中加入占过滤液的15%的1%醋酸水溶液，搅拌后沉淀30min，过滤，得石楠花提取液。
步骤四：采用分子蒸馏装置对所述石楠花提取液进行分离，逐渐减少真空度的值，先在102Pa真空度提取5-20min时间段得首段提取物0.11g，接着在1Pa真空度提取20-75min时间段得中段提取物0.15g，最后在在10-2Pa真空度从75min到提取结束得尾段提取物0.25g，中段提取物即为本发明的石楠花精油。
实施例2
步骤一：将10g石楠花干燥后粉碎至粒径为100目的颗粒，石楠花干燥至含水量为10%。
步骤二：粉碎后的石楠花用300ml乙酸乙酯占比80%的乙酸乙酯和石油醚的混合有机溶剂提取2次，过滤后合并滤液得过滤液。
步骤三：向步骤二得到的过滤液中加入占过滤液的10%的1%醋酸水溶液，搅拌后沉淀30min，过滤，得石楠花提取液。
步骤四：采用分子蒸馏装置对所述石楠花提取液进行分离，逐渐减少真空度的值，先在102Pa真空度提取5-20min时间段得首段提取物0.15，接着在1Pa真空度提取20-75min时间段得中段提取物0.19g，最后在在10-2Pa真空度从75min到提取结束得尾段提取物0.33g，中段提取物即为本发明的石楠花精油。
实施例3
步骤一：将1kg石楠花干燥后粉碎至粒径为300目的颗粒，石楠花干燥至含水量为5%。
步骤二：粉碎后的石楠花用2L乙酸乙酯占比95%的乙酸乙酯和石油醚的混合有机溶剂提取2次，过滤后合并滤液得过滤液。
步骤三：向步骤二得到的过滤液中加入占过滤液的15%的1%醋酸水溶液，搅拌后沉淀30min，过滤，得石楠花提取液。
步骤四：采用分子蒸馏装置对所述石楠花提取液进行分离，逐渐减少真空度的值，先在102Pa真空度提取5-20min时间段得首段提取物83g，接着在1Pa真空度提取20-75min时间段得中段提取物132g，最后在在10-2Pa真空度从75min到提取结束得尾段提取物216g，中段提取物即为本发明的石楠花精油。
对照例1
步骤一：将10g石楠花干燥后粉碎至粒径为200目的颗粒，石楠花干燥至含水量为8%。
步骤二：粉碎后的石楠花用200ml乙酸乙酯占比90%的乙酸乙酯和石油醚的混合有机溶剂提取2次，过滤后合并滤液得过滤液。
步骤三：采用分子蒸馏装置对步骤二得到的石楠花提取液进行分离，逐渐减少真空度的值，先在102Pa真空度提取5-20min时间段得首段提取物0.18，接着在1Pa真空度提取20-75min时间段得中段提取物0.27g，最后在在10-2Pa真空度提75min到提取结束得尾段提取物0.35g，中段提取物即为本发明的石楠花精油。
实施例4
淡香型石楠花精油香水，含有下述重量份的原料：石楠花精油3份，乙醇90份，玫瑰香精1份、紫罗兰酮1份、香豆素1份，苯乙醇2份，苯乙醛1份，乙酸苄酯1份。上述淡香型香水制备方法包括以下步骤：1）石楠花精油按照实施例1制备得到；2)将乙醇倒入玻璃瓶内，依次将石楠花精油、玫瑰香精、紫罗兰酮和香豆素加入，搅拌均匀；3)然后将苯乙醇、苯乙醛和乙酸苄酯加入到步骤2的溶液中即得淡香型石楠花精油香水。
实施例5
淡香型石楠花精油香水，含有下述重量份的原料：石楠花精油10份，乙醇300份，玫瑰香精5份、紫罗兰酮5份、香豆素5份，苯乙醇6份，苯乙醛5份，乙酸苄酯5份。
上述淡香型香水制备方法包括以下步骤：1）石楠花精油按照实施例2制备得到；
2)将乙醇倒入玻璃瓶内，依次将石楠花精油、玫瑰香精、紫罗兰酮和香豆素加入，搅拌均匀。
3)然后将苯乙醇、苯乙醛和乙酸苄酯加入到步骤2的溶液中即得淡香型石楠花精油香水。
对照例2
淡香型石楠花精油香水，含有下述重量份的原料：石楠花精油3份，乙醇90份，玫瑰香精1份、紫罗兰酮1份、香豆素1份，苯乙醇2份，苯乙醛1份，乙酸苄酯1份。
上述淡香型香水制备方法包括以下步骤：1）石楠花精油按照对照例1制备得到；
2)将乙醇倒入玻璃瓶内，依次将石楠花精油、玫瑰香精、紫罗兰酮和香豆素加入，搅拌均匀；3)然后将苯乙醇、苯乙醛和乙酸苄酯加入到步骤2的溶液中即得淡香型石楠花精油香水。
实验例1感官实验评价
参照《化妆品功效宣称评价试验技术导则》（2021年 第50号）进行感官评价实验。选择如下评价标准：在商业街随机选择30名15-60周岁年龄段的人群为成员，男女各半，每人分别对本发明实施例4和对照例2制备的香水进行感官实验，进行感官评分，评分标准如下：总分10分，分为很好，较好，勉强接受，不能接受4个等级。分数和等级的对应情况为：≧8为很好；<8，≧6为较好；<6，≧4为勉强接受；<4为不能接受。评价的指标有3个：气味、舒适度和色泽，其比例均占33.3%。取每一项指标30受试人打出分值的平均分，所有指标加权得分即为感官评分，感官评价见下表。
从实验结果显示，石楠花精油本身含有刺激性腥臭味，直接制备成香水消费者难以接受，采用醋酸水溶液可以有效去除石楠花精油中的刺激性气味，使消费者更能接受；并且经过酸处理的石楠花精油具有较好的色泽，适合制备成高端香水。并且本发明的含石楠花精油的香水具有较好的人群接受度。
试验例2 留香实验
留香参照《纬平针织物参数与留香性能构效关系研究》进行留香实验。准备市售纯棉面料，裁剪为长10cm 宽10cm 的方形作为实验样本。准备1000 mL 烧杯作为实验容器，先把未滴香水的纯棉面料平铺于烧杯内并用塑料薄膜密封15 min 后用电子鼻进行空白测量实验。进行留香实验时，将市售纯棉面料平铺于烧杯底部，将50 μL 实施例5的香水及市售迪奥小姐花漾淡香氛（30ml，国妆网备进字（沪）2020009738）溶液以少量多次的形式均匀滴在试样上，分别敞开1、2 h、3h、4h、5h、6h后，通过双层保鲜膜覆盖于烧杯上对试样进行密闭处理。密闭15 min，运用香味检测仪（日本COSMOS，型号XP-329IIIR）对烧杯顶部空气进行气味浓度检测。每组实验重复检测三次，得到平均结果，降低误差，用于分析。所有实验均在恒温（（20±3） ℃）、恒湿（（55±5） %）状态下进行。留香实验的结果参见说明是附图1。
结果显示，本发明的淡香味香水和市售的淡香味香水相比，留香更持久，取得了娱乐不到的技术效果。
本发明实施例作进一步的说明，但不能用来限制本发明的保护范围，对于本发明香水的其他范围或其他化妆品的具体实施方式，可参照本发明的技术原理以及实施例的操作来实施，仍在本发明的保护范围内。
Claims (4)
1.一种淡香型香水，其特征在于，含有石楠花精油，所述石楠花精油的制备方法包括：
步骤一：将石楠花干燥后粉碎至粒径为100～300目的颗粒；石楠花干燥至含水量为5%-10%；
步骤二：粉碎后的石楠花用非极性有机溶剂提取2～3次，合并滤液得过滤液；所述的非极性有机溶剂为乙酸乙酯、石油醚的混合物；乙酸乙酯的体积占总的非极性有机溶剂的体积为50％～99％；
步骤三：向步骤二得到的过滤液中加入0.5-2%醋酸水溶液，搅拌后沉淀30min-1h，过滤，得石楠花提取液；醋酸水溶液的加入量占过滤液体积的5%-40%；
步骤四：采用分子蒸馏法对所述石楠花提取物进行分离，将步骤三得到的石楠花提取液放入分子蒸馏装置中，逐渐减少真空度值，所述真空度范围为10-2-102Pa，依次得到首段、中段和尾段提取物；其中，首段提取物指真空提取5-20min的产物，尾段提取物指精准提取75min至结束的产物，中段提取物指20-75min的提取产物，取中段提取物即为石楠花精油。
2.如权利要求1所述的淡香型香水，其特征在于，包括下述重量份的原料：石楠花精油3-10份，乙醇90-300份，玫瑰香精1-5份、紫罗兰酮1-5份、香豆素1-5份，苯乙醇2-6份，苯乙醛1-5份，乙酸苄酯1-5份。
3.如权利要求2所述的淡香型香水，其特征在于，所述淡香型香水的制备方法包括以下步骤：
1）按照如权利要求1所述的石楠花精油的制备方法制备石楠花精油；
2)将乙醇倒入玻璃瓶内，依次将石楠花精油、玫瑰香精、紫罗兰酮和香豆素加入，搅拌均匀；
3)然后将苯乙醇、苯乙醛和乙酸苄酯加入到步骤2）的溶液中即得淡香型石楠花精油香水。
4.一种石楠花精油的制备方法，其特征在于，包括如下制备方法：
步骤一：将石楠花干燥后粉碎至粒径为100～300目的颗粒；石楠花干燥至含水量为5%-10%；
步骤二：粉碎后的石楠花用非极性有机溶剂提取2～3次，合并滤液得过滤液；所述的非极性有机溶剂为乙酸乙酯、石油醚的混合物；乙酸乙酯的体积占总的非极性有机溶剂的体积为50％～99％；
步骤三：向步骤二得到的过滤液中加入0.5-2%醋酸水溶液，搅拌后沉淀30min-1h，过滤，得石楠花提取液；醋酸水溶液的加入量占过滤液体积的5%-40%；
步骤四：采用分子蒸馏法对所述石楠花提取物进行分离，将步骤三得到的石楠花提取液放入分子蒸馏装置中，逐渐减少真空度值，所述真空度范围为10-2-102Pa，依次得到首段、中段和尾段提取物；其中，首段提取物指真空提取5-20min的产物，尾段提取物指精准提取75min至结束的产物，中段提取物指20-75min的提取产物，取中段提取物即为石楠花精油。
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