CN113456559A - 一种具有抗氧化作用的百合花珠光着色剂及其制备方法 - Google Patents
一种具有抗氧化作用的百合花珠光着色剂及其制备方法 Download PDFInfo
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Abstract
针对可用于开发色彩丰富的珠光颜料的合成着色剂数量有限，同时满足新一代消费群体对彩妆产品功效性和安全性的需求，顺应循环经济和绿色护肤的发展趋势。利用橙色的百合花全粉粉末，本专利提供一种具有抗氧化作用的百合花珠光着色剂及其制备方法，按质量配比1:1称取百合花粉（D50：1~10μm）和珠光颜料（D50：10~60μm），按固含量16.7%室温下搅拌加入10%PVA溶液中，过5号筛后进行喷雾干燥，工艺参数：温度：200℃，蠕动泵：15 r/min通针：2s/次。实验证明百合花珠光着色剂具有显著抗氧化功效，且发挥作用的成分为总糖、多酚、总黄酮和总皂苷。制得的百合花珠光着色剂，其呈橘色带珠光效果，适合于添加入粉饼、粉底液、散粉、妆前乳等底妆系列的彩妆用品之中。
Description
技术领域
本发明属于化妆品领域，具体涉及一种具有抗氧化作用的百合花珠光着色剂及其制备方法。
背景技术
随着中国彩妆市场和颜值经济的蓬勃发展，中国彩妆渗透率越来越高，其中00后购买美妆护肤品渗透率已高达88％，38.3％的95后群体几乎每天化妆，化妆行为与人际交往已经密不可分。但新一代的消费群体在购买产品时最看重产品功效和成分安全性，其次为产品口碑和性价比。
珠光颜料是一种光学效应颜料，在受到阳光照射时，产生多层次的反射，反射光相互作用而呈现出五彩缤纷的光泽，将珠光材料作为着色剂应用于彩妆配方中可追溯至二十世纪六十年代。为开发出一系列的色彩与差异化效果的珠光颜料，通常在基材表面包覆金属氧化物或有机颜料，而有机颜料用于化妆品有着非常大的局限性。目前《化妆品技术安全规范》(2015年)中规定禁用着色剂20余种，限用着色剂达157种，有统计表明常用着色剂60多种，高频使用的大约20种。可使用的安全性着色剂原料品种较少。
天然着色剂来源于天然资源对人体的危害较低，我国中药材的原植物是天然着色剂的来源之一。提取得到的天然着色剂已尝试作为一种食品添加剂使用。百合花是一种药食兼用的花卉，在民间应用广泛。《本经逢原》记载：“白花者补脾肺，赤花者名山丹，散瘀血药用之”。李时珍在《本草纲目》记载“用生百合捣涂，二日即安。或用百合花晒干为末，调菜油涂搽亦有效。”治疗天疱湿疮。白花百合提取物也是护肤类化妆品中添加较多的一类成分，发挥抗氧化作用。此外百合花还有卷丹百合、细叶百合等色彩鲜艳的品种，具有开发成天然着色剂的潜力。
发明内容
本发明提供一种具有抗氧化功效的百合花珠光着色剂及其制备方法，丰富彩妆着色剂原料的品类，满足消费者对彩妆产品功效性和安全性的需求。
本发明提供的具有抗氧化作用的百合花珠光着色剂，采用百合花粉与珠光颜料按照质量配比1:1～4通过邦定剂结合而成，其中所述百合花粉粒度D50为0.1～100μm，所述珠光颜料粒度D50为10～1000μm，所述邦定剂为硼砂、聚乙烯醇(PVA)的水溶液，其中硼砂与PVA的质量比为0.0％～8.5％。
优选百合花粉粒度D50为1～10μm。优选珠光颜料粒度D50为10～60μm。优选百合花粉与珠光颜料的质量配比为1:1。优选邦定剂为10％PVA水溶液，即不含硼砂。
本发明还提供上述百合花珠光着色剂的制备方法，按如上方案称取百合花粉与珠光颜料，按固含量12.0％～20.0％边搅拌边加入邦定剂中，过筛后进行喷雾干燥。优选固含量为16.7％。
作为一种优选方案，喷雾干燥条件如下：温度200℃，蠕动泵15r/min，通针2s/次。
有益效果
本发明提供的百合花珠光颜料通过喷雾干燥法将百合花粉与珠光颜料邦定在珠光颜料表面，制得的百合花珠光着色剂，其呈橘色带珠光效果，色泽适合于添加入粉饼、粉底液、散粉、妆前乳等底妆系列的彩妆用品之中。通过对DPPH自由基、羟基自由基清除能力、总还原能力的测定，实验证实百合花珠光着色剂具有体外抗氧化能力，且经过复杂邦定工艺后并未降低百合花的抗氧化能力，反而增强了其抗氧化能力，其发挥作用的成分包括总糖、多酚、总黄酮和总皂苷。可以将其作为功能性着色剂用于粉饼的制备。
本发明将百合花全粉粉末与珠光颜料进行邦定制备一种着色剂，既丰富了珠光颜料的色谱，又兼顾了作为彩妆原料的着色剂的安全性和功效性，填补了草本珠光着色剂的空白，符合循环经济和绿色护肤的发展趋势。
附图说明
图1百合花粉、百合花珠光着色剂的粉末形态，其中(A)为百合花粉，(B)为百合花珠光着色剂，比色卡附旁
图2添加百合花珠光着色剂制备的粉饼
具体实施方式
下面结合具体实施例进一步说明本发明的技术解决方案，不是对本技术方案的限制。
实施例1一种具有抗氧化作用的百合花珠光着色剂的制备
按质量配比(1:1；1:2；1:4)称取百合花粉和珠光颜料，按固含量16.7％室温下边搅拌边加入10％PVA溶液中，过5号筛后进行喷雾干燥，工艺参数：温度：200℃，蠕动泵：15r/min，通针：2s/次。百合花粉粒度(D50)1～10μm，珠光颜料粒度(D50)10～60μm。通过邦定效果的涂布评价(表1)，1:1质量配比制备的着色剂橘色较深，呈现偏橘红色的珠光效果，可均匀涂布。未邦定处理的百合花全粉粉末(图1A)接近萱草色，由于其比表面积大，富含淀粉等成分，易于结块不便于直接作为原料使用。百合花珠光着色剂见图1B，色泽与百合花接近，但经过邦定处理后粒径均匀细腻、不易结块，用于皮肤表面后亲肤性、延展性、光泽度较百合花粉均有增强，且百合花粉:珠光颜料＝1:1(W/W)时效果最佳，可用于化妆品的制备。
表1：不同质量配比对百合花珠光着色剂邦定效果的影响
| 质量配比 | 评价 |
| 1：1 | 呈现橘色带有珠光光泽，可均匀涂开，延展性好 |
| 1：2 | 亮度较1:1有所提高，亲肤性差，邦定效果不佳 |
| 1：4 | 整体颜色偏白，百合花粉末和底粉邦定效果不佳，分离明显 |
实施例2固含量对邦定的影响
按质量配比1：1称取百合花粉和珠光颜料，按固含量12.0％；16.7％；20.0％在室温下边搅拌边加入10％PVA溶液中，过5号筛后进行喷雾干燥，工艺参数：温度：200℃，蠕动泵：15r/min通针：2s/次。所述百合花粉粒度(D50)为：1～10μm，珠光颜料粒度(D50)为10～60μm。实验结果表明(表2)，固含量较低为12.0％时，邦定的效果差，喷雾干燥法加剧对底粉珠光颜料的磨损；固含量较高为20.0％时，影响得率。最终选择固含量16.7％进行邦定。
表2：固含量对邦定的影响
| 固含量(％) | 得率(％) | 粒度(D<sub>50</sub>)μm |
| 12.0 | 27.23 | 29.7±0.46 |
| 16.7 | 28.55 | 38.0±0.61 |
| 20.0 | 20.07 | 38.9±0.32 |
实施例3邦定剂组成对制备过程和效果影响
按质量配比1：1称取百合花粉和珠光颜料，按固含量16.7％在室温下边搅拌边加入邦定剂1(硼砂/PVA＝0.0％，即10％PVA溶液)或邦定剂2(硼砂/PVA＝8.5％)中，过5号筛后进行喷雾干燥，工艺参数：温度：200℃，蠕动泵：15r/min通针：2s/次。百合花粉粒度(D50)为：1～10μm，珠光颜料粒度(D50)为10～60μm。实验结果可知(表3)，采用邦定剂2进行制备时，制备过程不顺利，涂布效果差。最终采用邦定剂1，即10％PVA溶液邦定。
表3：邦定剂组成对制备过程和效果影响
实施例4百合花珠光着色剂的成分测定
按质量配比1:1称取百合花粉和珠光颜料，按固含量16.7％在室温下边搅拌边加入10％PVA溶液中，过5号筛后进行喷雾干燥，工艺参数：温度：200℃，蠕动泵：15r/min通针：2s/次。所述百合花粉粒度(D50)为：1～10μm，珠光颜料粒度(D50)为10～60μm。
由于邦定剂为水溶性成分，故本品用于彩妆产品配方时工艺及基质减少水性介质。选择80％乙醇作提取溶剂。精密称取百合花珠光着色剂6.0g，按料液比1：5加入80％乙醇中，避光常温浸泡过夜。然后在50℃下超声2h，减压抽滤，得到滤液定容至50mL。精密称取百合花粉末3.0g，按料液比1：10加入80％乙醇中，同法制备提取液，平行制备3份。参照苯酚硫酸法、福林酚比色法、亚硝酸钠-硝酸铝法、香草醛-高氯酸显色法测定总糖、多酚、总黄酮、总皂苷的含量。
成分分析结果表明(表4)，百合花及百合花珠光着色剂中总糖含量最高，约为其他成分总和的5倍，以葡萄糖当量计，百合花中含有231.93mg/g总糖，百合花珠光着色剂中总糖为68.52mg/g。邦定过程中喷雾干燥温度为200℃，造成百合花珠光着色剂中温敏性成分多酚、总黄酮和总糖的含量减少，以总皂苷含量计算，邦定效率为35.98％。
表4：百合花珠光着色剂和百合花中的有效成分含量(n＝3)
实施例5百合花珠光着色剂的抗氧化评价
多种植物活性成分，如多酚、多糖等，能够通过清除自由基、与金属离子螯合、抑制体内多种氧化酶的活性而起到抗氧化作用。且这种抗氧化作用在动物体内主要表现为提高其生产性能和提升机体抗氧化损伤的能力，在体外则表现为清除特定自由基的能力。百合花珠光着色剂的抗氧化评价主要通过测定DPPH自由基清除率、邻二氮菲法测定羟基自由基清除率、铁氰化钾还原法测定总还原能力。
实验1：测定DPPH自由基清除率
将实施例4制备的样品溶液逐级稀释至4.0mg/mL、2.0mg/mL、1.0mg/mL、0.5mg/mL、0.25mg/mL。取2mL样品溶液于5mL离心管中，加入2mL的DPPH无水乙醇溶液混合均匀，室温条件下，避光反应30min。3000r/min离心10min，在517nm波长处测定吸光度值，记为Ai；以无水乙醇代替DPPH溶液，测定吸光值，记为Aj；以样品溶剂代替样品溶液，测定吸光值，记为A0，以Vc作为阳性对照。每个样本平行3份。按公式(1)计算DPPH自由基清除率。
如表5所示：百合花珠光着色剂、百合花和阳性对照Vc对DPPH自由基均有清除作用，且呈剂量依赖性，随着浓度增大而增强。以IC50值评价清除DPPH自由基的效果，IC50为0.94mg/mL的百合花和IC50为2.37mg/mL的百合花珠光着色剂均有较强的清除DPPH自由基效果，百合花珠光着色剂作为功能性原料添加进配方，赋予产品色彩的同时可以同时发挥抗氧化效用。同时根据实施例4中测定所得百合花珠光着色剂中百合花的邦定效率为35.98％，可知百合花粉与珠光颜料通过复杂的绑定工艺，得到封闭式的物理结构，在同等剂量下并未降低百合花的DPPH自由基清除能力，甚至其自由基清除能力还得到了一定程度的提高，将该原料应用于底妆等彩妆配方中，在达到传统化妆品修色效果的同时具有显著的抗氧化功效，该研究开发思路未见报道与市售产品。
表5：DPPH自由基清除能力(n＝3)
实验2：测定羟基自由基清除率
将实施例4制备的样品溶液逐级稀释至60.0mg/mL、50.0mg/mL、40.0mg/mL、30.0mg/mL、20.0mg/mL。在10mL离心管中依次加入1mL样品溶液、1mL邻二氮菲溶液、2mLPBS(pH7.40)、1mL硫酸亚铁和1mL双氧水混匀，37℃水浴60min，在510nm处测定吸光值A1；用1mL样品溶剂代替1mL样品溶液，测定的吸光度值为A2；用1mL样品溶剂代替1mL样品溶液，用1mL纯水代替双氧水，测得的吸光度值为A0；用2mL纯水代替双氧水和硫酸亚铁，用1mL无水乙醇代替邻二氮菲，测得的吸光值为A3，以Vc作为阳性对照。每个样本平行3份。按公式(2)计算羟基自由基清除率。
由表6可知：在所检测范围内，百合花珠光着色剂、百合花和阳性对照Vc对羟基自由基的清除率随浓度增加而加强，以IC50值评价清除羟基自由基的效果百合花(IC50＝21.88mg/mL)＞百合花珠光着色剂(IC50＝37.55mg/mL)。百合花成分中糖碳链上的氢原子易被羟自由基攫取结合成水，活性成分中的酚羟基结构可以与自由基通过抽氢反应发挥抗氧化作用，邦定的百合花珠光着色剂同样具备羟自由基清除能力。同样根据实施例4中测定所得百合花珠光着色剂中百合花的邦定效率为35.98％，在同等剂量下并未降低百合花的羟自由基清除能力，反而显著增强了其羟自由基清除能力。
表6：羟自由基清除能力(n＝3)
实验3：测定总还原能力
将实施例4制备的样品溶液稀释至6.0mg/mL、4.0mg/mL、2.0mg/mL、1.0mg/mL、0.5mg/mL。取1mL待测溶液于10mLEP管中，加入2.5mLPBS，再加入1mL铁氰化钾溶液，50℃水浴20min后，冰水浴10min，加入2.5mL三氯乙酸，于低速离心机中离心10min，转速为3500r/min，取上清液2.5mL于新的离心管，加入2.5mL纯水和0.5mLFeCl3后在室温条件下放置10min，测定700nm波长下的吸光度值，记为A1，以纯水代替FeCl3溶液测得的吸光度值，记为A2，以Vc作为阳性对照。每个样本平行3份。按公式(3)计算样品的还原能力。
还原能力＝A1-A2 (3)
由表7可知：百合花、百合花珠光着色剂和Vc的还原能力在实验浓度范围内均有良好的量效关系，百合花珠光着色剂在2.0mg/mL时A700nm为0.220，相当于百合花1.0mg/mL、阳性对照Vc12.50μg/mL的还原能力，根据实施例4中测定所得百合花珠光着色剂中百合花的邦定效率为35.98％，说明百合花按1：1质量配比制备成百合花珠光着色剂后，对Fe3+的还原能力未明显降低，反而有所升高，说明百合花珠光着色剂作为彩妆原料应用仍具备抗氧化效果。
表7：总还原能力效果(n＝3)
实施例6百合花珠光着色剂应用于粉饼制备
将实施例4的原料作为功能性着色剂用于制备粉饼，配方见表8。将原料A，C，D高速粉碎机中搅拌混匀4min；加入原料B继续搅拌混合4min，通过跌落测试和对色后，出料，混合后的粉末过筛，灭菌后进行压粉，包装，质检合格后得到成品(图2)。成品带有清淡百合花粉气味，具有轻微珠光效果，较好的亲肤性和延展性，可以快速遮盖面部瑕疵，均匀肤色。
表8：百合花珠光着色剂作为原料制备粉饼的配方
| 原料分组 | 原料名称 | 配方百分比(％) |
| A | 滑石粉 | 15.0 |
| A | 百合花珠光着色剂 | 25.0 |
| A | 合成云母粉 | 38.0 |
| A | 硬脂酸镁 | 10.0 |
| B | 硅粉 | 5.0 |
| A | 聚二甲基硅氧烷 | 6.0 |
| C | 苯氧乙醇 | 0.7 |
| D | CI77491 | 0.1 |
| D | CI77492 | 0.2 |
实施例7添加百合花珠光着色剂的粉饼的实验感官分析评价
招募10名20～30岁健康女性志愿者，于底妆最后一步使用实施例6制备的粉饼，使用后对产品的质感(粉质细腻度)、妆感、遮瑕力、亲肤性、持久度进行评价。以打分的方式(0-10分，分数越高，代表指标性能越好)。结果见表9，总体而言，将百合花珠光着色剂按照实施例6进行配方设计，使用后呈现较优的妆效，可通过改良配方进一步提高产品持妆效果。原料粒度小D50为38.0μm，在配方中占比高达25％，有助于粉饼粉质细腻清透。百合花草本珠光着色剂呈现的橘红色结合其蕴含珠光效果，可有效地发挥遮瑕效果。所有志愿者均未出现过敏闷痘等不良反应，并表示产品百合花粉的气味可接受。
表9：粉饼使用感官分析
Claims (7)
1.一种具有抗氧化作用的百合花珠光着色剂，其特征在于：采用百合花粉与珠光颜料按照质量配比1:1~4通过邦定剂结合而成，其中所述百合花粉粒度D50为0.1~100 μm，所述珠光颜料粒度D50为10~1000 μm，所述邦定剂为硼砂、聚乙烯醇PVA的水溶液，其中硼砂与PVA的质量比为0.0 %~8.5 %。
2.如权利要求1所述的百合花珠光着色剂，其特征在于：所述百合花粉粒度D50为1~10 μm，所述珠光颜料粒度D50为10~60 μm。
3.如权利要求1或2所述的百合花珠光着色剂，其特征在于：所述邦定剂为10 % PVA水溶液，即不含硼砂。
4.如权利要求1~3所述的百合花珠光着色剂，其特征在于：所述百合花粉与珠光颜料的质量配比为1:1。
5.权利要求1~4中任一项所述的百合花珠光着色剂的制备方法，其特征在于：称取百合花粉与珠光颜料，按固含量12.0 %~20.0 %边搅拌边加入邦定剂中，过筛后进行喷雾干燥。
6.权利要求5中所述的制备方法，其特征在于：所述固含量为16.7 %。
7.如权利要求5或6所述的制备方法，其特征在于：喷雾干燥条件如下：温度200 ℃，蠕动泵15 r/min，通针2 s/次。
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