WO2020134936A1 - 食品级植物源性复合抑菌剂在化妆品中的应用 - Google Patents
食品级植物源性复合抑菌剂在化妆品中的应用 Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/31—Hydrocarbons
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
Definitions
- This application relates to the application of a natural antibacterial antiseptic material.
- Adding preservatives will inhibit the growth of these microorganisms, prevent the spoilage and deterioration of products, reduce the harm caused by product deterioration to the skin, and can effectively extend the shelf life of cosmetics.
- the para-hydroxy bacteriostatic agent has been shown to accumulate the possibility of carcinogenesis in adipose tissue, and it can also simulate a certain estrogen to increase the probability of female breast cancer induction.
- Formaldehyde slow-release bacteriostatic agents have the problems of volatility, poor thermal stability, and irritating odor, and ordinary consumers have a strong rejection of formaldehyde. Therefore, the use of chemical preservatives in cosmetics will have greater side effects on the human body.
- the cost of chemical preservatives is too high to be applied on a large scale in industry.
- This application is to solve the technical problem that the existing chemical preservatives in cosmetics have side effects on the human body and the cost is high and cannot be applied on a large scale in the industry, and to provide a food-grade plant-derived composite bacteriostatic agent in cosmetics application.
- the present application provides the application of food-grade plant-derived compound bacteriostatic agents in cosmetics, the food-grade plant-derived compound bacteriostatic agent is used as a preservative in the preparation of cosmetics, and the food-grade plant
- the added amount of the source compound bacteriostatic agent in cosmetics is 0.04%-0.08%;
- the food grade plant-derived compound bacteriostatic agent includes cinnamaldehyde, eugenol and trans-o-methoxycinnamaldehyde.
- the food-grade plant-derived composite bacteriostatic agent includes 15 parts to 85 parts of cinnamaldehyde, 3 parts to 60 parts of eugenol, and 3 parts to 15 parts of trans-o-methoxycinnamon in parts by weight aldehyde.
- the cosmetics include creams, lotions, essences, essence water or facial cleanser, and also include other cosmetics.
- the cosmetic is a cream
- the amount of food-grade plant-derived compound bacteriostatic agent added to the cream is 0.05% of the mass of the cream.
- the cosmetic is an emulsion
- the amount of food-grade plant-derived compound bacteriostatic agent added to the emulsion is 0.06% of the mass of the emulsion.
- the cosmetic is an essence
- the amount of the food-grade plant-derived compound bacteriostatic agent added to the essence is 0.05% of the quality of the essence.
- the cosmetic is essence water
- the amount of the food-grade plant-derived compound bacteriostatic agent added in the essence water is 0.04% to 0.08% of the mass of the essence.
- the cosmetic is a facial cleanser
- the amount of food-grade plant-derived compound bacteriostatic agent added to the facial cleanser is 0.05% of the quality of the facial cleanser
- the food-grade plant-derived compound bacteriostatic agent of the present application includes spices, Chinese herbal medicine, tea polyphenols, pectin hydrolysate, bamboo leaf extract, etc. They are direct extracts of natural plants and can prevent many kinds of bacteria, The growth of mold is an ideal natural antibacterial and antiseptic material. On this basis, this application uses plants with homology to extract cinnamaldehyde and eugenol, and adds one of trans-o-methoxycinnamaldehyde or caryophyllene. To prepare a food-grade plant-derived composite bacteriostatic agent.
- the composite bacteriostatic agent greatly enhances its bacteriostatic effect by giving full play to the synergistic effect between the components, has a broad bacteriostatic spectrum, and has an antioxidant effect. Good antiseptic effect, simple preparation process and low production cost;
- This application added food-grade plant-derived compound bacteriostatic agents in the production of cosmetics instead of traditional chemical preservatives.
- Food-grade plant-derived compound bacteriostatic agents are extracted from plants with the same food and medicine ingredients. Natural, the cosmetics prepared by using it are gentler, safer and non-irritating to the human body; and can effectively prolong the storage time of cosmetics. Compared with chemically synthesized preservatives, it can guarantee the shelf life of cosmetics within the shelf life Under similar conditions, the ingredients are safer, and long-term use will not cause side effects to the body.
- Fig. 1 is the antioxidant curve of the food-grade plant-derived compound bacteriostatic agent of Example 1; wherein, A represents the concentration of the food-grade plant-derived compound bacteriostatic agent-DPPH radical scavenging rate curve, and B in the figure represents the BHT Concentration-DPPH free radical scavenging curve graph, C in the figure represents the concentration of rosemary oil-DPPH free radical scavenging curve graph.
- the distillate was transferred to a separatory funnel and extracted twice with 40 L portions of ether. Discard the water layer, transfer the ether layer to a small test tube, add a small amount of anhydrous sodium sulfate to dry, after 20min, pour out the extract, and heat and distill off the ether in a fume hood with a water bath to obtain a plant extract containing cinnamaldehyde;
- the resulting distillate was placed in a separatory funnel and extracted twice with ethyl acetate (20 L each time).
- the upper ethyl acetate extracts were combined (the upper ethyl acetate extract contained eugenol), followed by ethyl acetate removal , To obtain a plant extract containing eugenol.
- the stirring pot Preheat the stirring pot to 60°C, preheat for 5 minutes, adjust the rotation speed to 15r/min, open the stirring pot, add the plant extract containing cinnamaldehyde, the plant extract containing eugenol, and trans ortho Methoxycinnamaldehyde (purchased from Shanghai Zhenzhun Biological Technology Co., Ltd.) totaling 100kg, adjust the speed of the stirring pot to 100r/min, stir for 50 minutes, and then divide into separate pieces to obtain a food-grade plant-derived composite bacteriostatic agent;
- the food-grade plant-derived composite bacteriostatic agent includes 55 parts of cinnamaldehyde, 12 parts of eugenol, and 7 parts of trans-o-methoxycinnamaldehyde in parts by weight.
- Example 1 The performance test of the food-grade plant-derived composite bacteriostatic agent obtained in Example 1 is carried out.
- the specific test methods and test results are as follows:
- Example 2 It can be seen from Table 2 that the food-grade plant-derived composite bacteriostatic agent obtained in Example 1 has a light fragrance, the system is uniform and stable, the off-gas is very light, and the smell is coordinated.
- DPPH is widely used to quantitatively determine the antioxidant capacity of biological samples and foods.
- DPPH free radicals have a single electron and a strong absorption at 517nm.
- the alcohol solution is purple in color.
- a free radical scavenger is present, its absorption gradually disappears due to its single electron pairing, and the degree of discoloration is quantitatively related to the number of electrons it receives, so a spectrophotometer can be used for rapid quantitative analysis.
- the food-grade plant-derived compound bacteriostatic agent, rosemary oil, and BHT all have a certain ability to scavenge free radicals, while the food-grade plant-derived compound bacteriostatic agent has a much better free radical scavenging ability than BHT.
- rosemary oil indicating that it can replace both to become a new type of antioxidant used in cosmetics.
- test bacteria were: Staphylococcus aureus, Escherichia coli, Candida albicans, Pseudomonas aeruginosa, Aspergillus niger.
- the minimum bacteriostatic concentration MIC of the food-grade plant-derived composite bacteriostatic agent obtained in Example 1 was determined by the liquid medium dilution method. The specific method is as follows:
- Detection of minimum bacteriostatic concentration Take 0.1ml of mixed bacterial suspension and add to 10mL of nutrient broth culture medium containing bacteriostat at different concentrations, and mix evenly; set three parallel test groups, in which the observation of bacteria is placed in Incubate at 37°C for 24h, and observe the fungus at 28°C for 48h; after the cultivation, draw 1ml of the nutrient broth medium containing bacteriostat at different concentrations into the plate, pour the appropriate amount of medium, and observe the bacteria at 37 Incubate for 24 hours at °C, and observe the fungi at 28 °C for 48 hours; obtain the total number of plate colonies and take the average.
- the antimicrobial efficacy result data (MIC) is shown in Table 3:
- the minimum bacteriostatic concentration of the food-grade plant-derived compound bacteriostatic agent obtained in Example 1 is 0.05%.
- the amount of the food-grade plant-derived compound bacteriostatic agent obtained in Example 1 is not less than At 0.05%, the food-grade plant-derived composite bacteriostatic agent obtained in Example 1 can simultaneously treat five types of fungi including Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, Candida albicans and Aspergillus niger Play a restraining role.
- Example 4 It can be seen from Table 4 that the food-grade plant-derived composite bacteriostatic agent obtained in Example 1 has a good bacteriostatic effect in the pH range of 4-10.
- Example 1 It is known from Table 5 that the food-grade plant-derived composite bacteriostatic agent obtained in Example 1 has different stability under different temperature conditions, and the experimental results show that the food-grade plant-derived obtained in Example 1 has a temperature below 100°C The compound bacteriostatic agent can still maintain excellent bacteriostatic effect.
- the hair removal range is about 3cm ⁇ 3cm on the left and right of the back spine.
- the skin after hair removal then covered with two layers of gauze and cellophane on the skin surface, and then fixed with non-irritating tape and bandage, the other side of the skin as a control, using a closed test, the application time is 4h .
- the specific method for preparing a cream using a food-grade plant-derived compound bacteriostatic agent is:
- the food-grade plant-derived composite bacteriostatic agent includes 55 parts of cinnamaldehyde, 12 parts of eugenol, and 7 parts of trans-o-methoxycinnamaldehyde in parts by weight.
- the preparation method of cream is as follows:
- phase A weigh the feed liquid in phase A, add it in the order from top to top in Table 6, heat to 75°C and stir to disperse evenly, keep it warm for 20 minutes, and wait for use, which is recorded as phase A (that is, oil phase);
- phase B to phase A, homogenize and emulsify for 1.5 ⁇ 2.0min, then add phase C, homogenize and emulsify for 1min, take out, slowly stir and slowly cool to room temperature, and discharge.
- composition of the emulsion in this example is shown in Table 11,
- the food-grade plant-derived composite bacteriostatic agent includes 55 parts of cinnamaldehyde, 12 parts of eugenol, and 7 parts of trans-o-methoxycinnamaldehyde in parts by weight.
- the preparation method of the emulsion is as follows:
- phase A weigh the feed liquid in phase A, add in the order from top to bottom in Table 8, heat to 75°C and stir to disperse evenly, keep it warm for 20 minutes, and wait for use.
- the phase A is the oil phase;
- phase B to phase A, homogenize and emulsify for 1.5-2.0min, then add phase C, homogenize and emulsify for 1min, take out, slowly stir and slowly cool to room temperature, and discharge.
- the specific method for preparing the essence using the food-grade plant-derived compound bacteriostatic agent is:
- the food-grade plant-derived composite bacteriostatic agent includes 55 parts of cinnamaldehyde, 12 parts of eugenol, and 7 parts of trans-o-methoxycinnamaldehyde in parts by weight.
- the preparation method of essence is as follows:
- the specific method for preparing essence water using food-grade plant-derived compound bacteriostatic agent is:
- composition of the essence water in this embodiment is shown in Table 15,
- the food-grade plant-derived composite bacteriostatic agent includes 55 parts of cinnamaldehyde, 12 parts of eugenol, and 7 parts of trans-o-methoxycinnamaldehyde in parts by weight.
- the preparation method of essence water is as follows:
- aqueous solutions of 2 and 3 are heated and mixed evenly, added to 4 while stirring, and heated to stand until transparent.
- the specific method for preparing a facial cleanser using a food-grade plant-derived composite bacteriostatic agent is:
- the food-grade plant-derived composite bacteriostatic agent includes 55 parts of cinnamaldehyde, 12 parts of eugenol, and 7 parts of trans-o-methoxycinnamaldehyde in parts by weight.
- the preparation method of facial cleanser is as follows:
- phase A and phase B Weigh phase A and phase B according to the amount, heat and mix them separately, then add phase B to phase A and stir at low speed.
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Abstract
食品级植物源性复合抑菌剂在化妆品中的应用，所述食品级植物源性复合抑菌剂在化妆品中的添加量为0.04%~0.08%；该复合抑菌剂包括肉桂醛、丁香酚和反式邻甲氧基肉桂醛。该复合抑菌剂采用药食同源的植物进行提取，有很好的抑制微生物生长地效果，有效地延长化妆品的保存时间。与化学合成防腐剂相比，防腐效果相近的条件下，成分安全性更高，长时间使用不会给身体带来副作用。
Description
相关申请的交叉引用
本申请要求在2018年12月29日提交中国专利局、申请号为201811631165.3、申请名称为“食品级植物源性复合抑菌剂在化妆品中的应用”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
本申请涉及一种天然抑菌防腐材料的应用。
随着化妆品功能性多样化的增加，营养物质的添加会使微生物极易在产品中生长繁殖，例如在膏霜产品中含有大量营养丰富的物质，且保质期一般较长，在使用过程中反复接触微生物，尤其容易被微生物污染而导致变质。
添加防腐剂会抑制这些微生物的滋生，防止产品的腐败变质，减少因产品变质给皮肤带来的危害，能有效延长化妆品的货架期。而现有的化学防腐剂中，对羟基类抑菌剂被证实在脂肪组织中累积有致癌的可能性，还能够模拟某种雌激素增加女性乳腺癌的诱发几率。甲醛缓释类抑菌剂存在易挥发、热稳定性差、有刺激性气味的问题，而且普通消费者对甲醛有强烈的排斥心理。因此在化妆品中使用化学防腐剂会对人体产生较大的副作用。而且化学防腐剂成本过高，无法在工业上大规模应用。
发明内容
本申请是要解决现有的化妆品中的化学防腐剂对人体存在副作用且成本高、无法在工业上大规模应用的技术问题，而提供一种食品级植物源性复合抑菌剂在化妆品中的应用。
根据本申请的一个方面，本申请提供了食品级植物源性复合抑菌剂在化妆品中的应用，所述食品级植物源性复合抑菌剂作为防腐剂用于制备化妆品，所述食品级植物源性复合抑菌剂在化妆品中的添加量为0.04％～0.08％；所述食品级植物源性复合抑菌剂包括肉桂醛、丁香酚和反式邻甲氧基肉桂醛。
优选地，所述食品级植物源性复合抑菌剂按重量份数包括15份～85份的肉桂醛、3份～60份的丁香酚和3份～15份的反式邻甲氧基肉桂醛。
优选地，所述化妆品包括膏霜、乳液、精华液、精华水或洗面奶，还包括其它化妆品。
优选地，所述化妆品为膏霜，食品级植物源性复合抑菌剂在膏霜中的添加量为膏霜质量的0.05％。
优选地，所述化妆品为乳液，食品级植物源性复合抑菌剂在乳液中的添加量为乳液质量的0.06％。
优选地，所述化妆品为精华液，食品级植物源性复合抑菌剂在精华液中的添加量为精华液质量的0.05％。
优选地，所述化妆品为精华水，食品级植物源性复合抑菌剂在精华水中的添加量为精华液质量的0.04％～0.08％。
优选地，所述化妆品为洗面奶，食品级植物源性复合抑菌剂在洗面奶中的添加量为洗面奶质量的0.05％。
本申请的有益效果：
一、本申请的食品级植物源复合抑菌剂包含有香辛料、中草药、茶多酚、果胶酶解物、竹叶提取物等，它们属于天然植物的直接提取物，能阻止多种细菌、霉菌的生长，是理想的天然抑菌防腐材料，在其基础上本申请采用药食同源的植物进行提取肉桂醛和丁香酚，并加入反式邻甲氧基肉桂醛或石竹烯中的一种，制备食品级植物源性复合抑菌剂，该复合抑菌剂通过充分发挥组分之间的协同增效作用，大大提高其抑菌效果，抑菌谱广，且具有抗氧化的效果，防腐效果好，且制备工艺简单、生产成本低；
二、本申请在化妆品生产过程中添加了食品级植物源性复合抑菌剂，代替了传统的化学防腐剂，食品级植物源性复合抑菌剂采用药食同源的植物进行提取，成分源自天然，利用其制备出来的化妆品对人体更温和、安全、无刺激；且能够达到有效地延长化妆品的保存时间，与化学合成防腐剂相比，在保证化妆品货架期的时间范围内、防腐效果相近的条件下，成分安全性更高，长时间使用不会给身体带来副作用。
图1为实施例1食品级植物源性复合抑菌剂抗氧化曲线图；其中，A表示食品级植物源性复合抑菌剂的浓度-DPPH自由基清除率曲线图，图中B表示BHT的浓度-DPPH自由基清除率曲线图，图中C表示迷迭香油的浓度-DPPH自由基清除率曲线图。
实施例1：
食品级植物源性复合抑菌剂的制备方法：
(1)、制备含肉桂醛的植物提取物：水蒸气蒸馏法取60kg研细的肉桂树皮粉，放入烧瓶中，加水160L，装上冷凝管，加热回流10min。冷却后倒入蒸馏瓶中进行水蒸气蒸馏，收集馏出液80～100L；
将馏出液转移到分液漏斗中，用每份40L乙醚萃取两次。弃去水层，乙醚层移入小试管中，加入少量无水硫酸钠干燥，20min后，倒出萃取液，在通风橱内用水浴加热蒸去乙醚，即得含肉桂醛的植物提取物；
(2)、制备含丁香酚的植物提取物：称取丁香花蕾15kg，加水90L在蒸馏瓶浸泡后，直接加热进行水蒸汽蒸馏，收集馏液约30L；
将所得的馏液置于分液漏斗中，用乙酸乙酯萃取两次(每次20L)，合并上层乙酸乙酯萃取液(上层乙酸乙酯萃取液含丁香酚)，之后进行乙酸乙酯去除，即得含丁香酚的植物提取物。
(3)、将搅拌锅预加热至60℃，预热5分钟，将转速调至15r/min，打开搅拌锅，加入含肉桂醛的植物提取物、含丁香酚的植物提取物、反式邻甲氧基肉桂醛(购自上海甄准生物科技有限公司)共计100kg，将搅拌锅转速调至100r/min，搅拌50分钟，搅拌后分装，即得食品级植物源性复合抑菌剂；所述食品级植物源性复合抑菌剂按重量份数包括55份的肉桂醛、12份的丁香酚和7份的反式邻甲氧基肉桂醛。
对实施例1得到的食品级植物源性复合抑菌剂进行性能检测，具体检测方法和检测结果如下：
(一)对迷迭香油、BHT(2,6-二叔丁基-4-甲基苯酚)和食品级植物源性复合抑菌剂进行感官评价比较：
感官评价描述数据参照表1。
表1
迷迭香油、BHT(2,6-二叔丁基-4-甲基苯酚)和食品级植物源性复合抑菌剂的感官评价结果如表2所示。
表2
通过表2可知实施例1得到的食品级植物源性复合抑菌剂有淡淡的香气，体系均一稳定，杂气很淡，气味协调。
(二)将实施例1制备的食品级植物源性复合抑菌剂组合物、迷迭香油和BHT(2,6-二叔丁基-4-甲基苯酚)按照抗氧化实验方法，检测其抗氧化性能：
检测结果如图1所示，DPPH广泛用于定量测定生物试样和食品的抗氧化能力，DPPH自由基有单电子，在517nm处有一强吸收，其醇溶液呈紫色的特性。当有自由基清除剂存在时，由于与其单电子配对而使其吸收逐渐消失，其褪色程度与其接受的电子数量成定量关系，因而可用分光光度计进行快速的定量分析。从上图可以看出，食品级植物源性复合抑菌剂、迷迭香油、BHT都具有一定清除自由基能力，而食品级植物源性复合抑菌剂对自由基清除能力要远优于BHT和迷迭香油，说明其可以替代两者成为新型的抗氧化剂应用于化妆品中。
(三)抑菌效能实验方案
供试菌种为：金黄色葡萄球菌、大肠杆菌、白色念珠菌、铜绿假单胞杆菌、黑曲霉。
采用液体培养基稀释法测定实施例1得到的食品级植物源性复合抑菌剂的最低抑菌浓度MIC，具体方法如下：
(1)培养基的制备：营养肉汤培养基；
(2)菌悬液的制备：取活化后的金黄色葡萄球菌、活化后的大肠杆菌和活化后的铜绿假单胞杆菌于灭菌蒸馏水中分别制成1×10
8cfu/mL的菌悬液；取活化后的白假丝酵母菌和活化后的黑曲霉于灭菌蒸馏水中分别制成1×10
7cfu/mL的菌悬液；分别取上述细菌和真菌的菌悬液1mL于灭菌试管中混合均匀待用，得到混合菌悬液；
(3)含防腐剂组合物试管的制备：利用实施例1得到的食品级植物源性复合抑菌剂和营养肉汤培养基配置浓度分别为0.025％、0.05％、0.10％、0.20％、0.40％和0.80％的含抑菌剂的营养肉汤培养基；
(4)最低抑菌浓度检测：取混合菌悬液0.1ml分别加入10mL不同浓度含抑菌剂的营 养肉汤培养基中，并混合均匀；设置三组平行试验组，其中细菌的观察置于37℃培养24h，真菌的观察置于28℃培养48h；培养结束后分别在不同浓度含抑菌剂的营养肉汤培养基中吸取1ml于平板中，倒入适量培养基，细菌观察置于37℃培养24h，真菌的观察置于28℃培养48h；获取平板菌落总数，取平均值。
抑菌效能结果数据(MIC)如表3所示：
表3
注：“-”表示没有菌生长，“+”表示有极少菌，“++”表示有少数菌“++”表示有大量菌。
从表格3上可以看出，实施例1得到的食品级植物源性复合抑菌剂最小抑菌浓度为0.05％，当实施例1得到的食品级植物源性复合抑菌剂添加量不低于0.05％时，实施例1得到的食品级植物源性复合抑菌剂对金黄色葡萄球菌、铜绿假单胞菌、大肠埃希氏菌、白色假丝酵母和黑曲霉5种菌类都能同时起到抑制作用。
(四)不同pH条件下的抑菌效能实验方案
以不同pH条件下按照(三)抑菌效能实验方案的常规实验方法，检测其在不同pH条件下的抑菌效能，结果如表4所示：
表4
注：“-”表示没有菌生长，“+”表示有极少菌，“++”表示有少数菌“+++”表示有大量菌。
通过表4可知，实施例1得到的食品级植物源性复合抑菌剂在pH为4-10之间的酸碱范围内，都有良好的抑菌效能。
(五)高温稳定性实验
在高温条件下按照(三)抑菌效能实验方案的常规实验方法，检测其在不同高温条件下浓度为0.05％的含抑菌剂的营养肉汤培养基的抑菌效能，结果如表5所示：
表5
注：“-”表示没有菌生长，“+”表示有极少菌，“++”表示有少数菌“+++”表示有大量菌。
通过表5知，实施例1得到的食品级植物源性复合抑菌剂对不同的温度条件有不同的稳定性，实验结果表明，温度为100℃以下，实施例1得到的食品级植物源性复合抑菌剂仍可以保持优良的抑菌效果。
(六)皮肤刺激性/腐蚀性试验
参照《化妆品安全技术规范》(2015年版)中《皮肤刺激性/腐蚀性试验》，适用于化妆品原料安全性毒理学检测：
试验方法：
试验前约24h将兔子背部脊柱两侧毛剪掉，不可损伤表皮，去毛范围在背部脊柱左右各约3cm×3cm的范围内，取食品级植物源性复合抑菌剂0.5mL直接涂在背部脊柱其中一侧去毛后的皮肤上，然后用二层纱布及玻璃纸覆盖在皮肤表面，再用无刺激性胶布和绷带加以固定，另一侧皮肤作为对照，采用封闭试验，敷用时间为4h。
清除受试物后，分别在1h、24h、48h和72h观察涂布部位的皮肤反应，按表6进行皮肤反应评分，以兔子积分的平均值进行综合评价，根据1h、24h、48h和72h各观察时点最高积分均值，按表7判定皮肤刺激强度。
表6 皮肤刺激反应评分
| 皮肤反应 | 积分 |
| 红斑和焦痂形成 | |
| 无红斑 | 0 |
| 轻微红斑(勉强可见) | 1 |
| 明显红斑 | 2 |
| 中度—重度红斑 | 3 |
| 严重红斑(紫红色)至轻微焦痂形成 | 4 |
| 水肿形成 | |
| 无水肿 | 0 |
| 轻微水肿(勉强可见) | 1 |
| 轻度水肿(皮肤隆起轮廓清楚) | 2 |
| 中度水肿(皮肤隆起约1mm) | 3 |
| 重度水肿(皮肤隆起超过1mm，范围扩大) | 4 |
| 最高积分 | 8 |
表7 皮肤刺激强度分级
| 积分均值 | 强度 |
| 0-＜0.5 | 无刺激性 |
| 0.5-＜2.0 | 轻刺激性 |
| 2.0-＜6.0 | 中刺激性 |
| 6.0-＜8.0 | 强刺激性 |
试验结果见表8：
表8
由表8可看出，涂有食品级植物源性复合抑菌剂处的皮肤刺激强度积分均值为0.333＜0.5，所以为食品级植物源性复合抑菌剂对于皮肤没有刺激性。
实施例2：
使用食品级植物源性复合抑菌剂制备膏霜的具体方法为：
本实施例中膏霜的成分如表9所示，
表9
所述食品级植物源性复合抑菌剂按重量份数包括55份的肉桂醛、12份的丁香酚和7份的反式邻甲氧基肉桂醛。
膏霜的制备方法如下：
①将黄原胶加至甘油及1,3-丁二醇中预分散，加入去离子水搅拌均匀后，再加入EDTA-2Na，搅拌均匀并加热至75℃，保温20min，待用，记为B相；
②称量A相中料液，并按表6中从上至的次序添加，加热至75℃并搅拌分散均匀，保温20min，待用，记为A相(即为油相)；
③将B相加入A相中，均质乳化1.5～2.0min，然后再加入C相，均质乳化1min，取出，缓慢搅拌并慢降温至室温，出料。
对本实施例的膏霜进行28天的防腐测试，结果数据如表10：
表10
从表7可以看出，经过28天的防腐测试，该膏霜中大肠埃希氏菌、铜绿假单胞菌、金黄色葡萄球菌、白色假丝酵母和黑曲霉的从第7天到第28天的检测结果均为0。
实施例3：
使用食品级植物源性复合抑菌剂制备乳液的具体方法为：
本实施例中乳液的成分如表11所示，
表11
所述食品级植物源性复合抑菌剂按重量份数包括55份的肉桂醛、12份的丁香酚和7份的反式邻甲氧基肉桂醛。
乳液的制备方法如下：
①将黄原胶加至甘油中预分散，加入去离子水搅拌均匀后，再加入EDTA-2Na，搅拌均匀并加热至75℃，保温20min，再加入1,3-丙二醇和透明质酸钠，记为B相；
②称量A相中料液，并按表8中从上至下的次序添加，加热至75℃并搅拌分散均匀，保温20min，待用，记为A相即为油相；
③将B相加入A相中，均质乳化1.5-2.0min，然后再加入C相，均质乳化1min，取出，缓慢搅拌并慢降温至室温，出料。
对本实施例的乳液进行28天的防腐测试，结果数据如表12：
表12
从表9可以看出，经过28天的防腐测试，该乳液中大肠埃希氏菌、铜绿假单胞菌、金黄色葡萄球菌、白色假丝酵母和黑曲霉的从第7天到第28天的检测结果均为0。
实施例4：
使用食品级植物源性复合抑菌剂制备精华液的具体方法为：
本实施例中精华液的成分如表13所示，
表13
所述食品级植物源性复合抑菌剂按重量份数包括55份的肉桂醛、12份的丁香酚和7份的反式邻甲氧基肉桂醛。
精华液的制备方法如下：
①将黄原胶、尿囊素、HA加至甘油和1,3-丁二醇中预分散，加入去离子水搅拌均匀；
②加入甜菜碱，EDTA-2Na，D-泛醇，β-葡聚糖和乳酸钠，搅拌均匀并加热至70℃，保温20min后冷却至50℃，待用；
③将植物防腐剂加入PEG-60氢化蓖麻油中，加热至50℃，搅拌分散均匀；
④将①加入到②中混合均匀后再加入③中，搅拌分散均匀。
对本实施例的精华液进行28天的防腐测试，结果数据如表14：
表14
从表11可以看出，经过28天的防腐测试，该精华液中大肠埃希氏菌、铜绿假单胞菌、金黄色葡萄球菌、白色假丝酵母和黑曲霉的从第7天到第28天的检测结果均为0。
实施例5：
使用食品级植物源性复合抑菌剂制备精华水的具体方法为：
本实施例中精华水的成分如表15所示，
表15
所述食品级植物源性复合抑菌剂按重量份数包括55份的肉桂醛、12份的丁香酚和7份的反式邻甲氧基肉桂醛。
精华水的制备方法如下：
1.称取EDTA-二钠溶于水中，得到EDTA-二钠水溶液；
2.称取0.2g的卡波姆预溶于50mL的步骤1中EDTA-二钠水溶液中，预溶成透明凝胶状备用；
3.称取0.2g的黄原胶混溶于甘油、丁二醇、1，3-丙二醇、双丙甘醇中，分散均匀再与的步骤1中EDTA-二钠水溶液混合均匀；
4.称取氢化卵磷脂和植物源性防腐剂，水浴加热溶解，溶解后加入油醇聚醚-5，继续加热混合均匀；
将2和3的水溶液加热混合均匀，边搅拌边加入到4中，加热静置至透明即可。
对本实施例的精华水进行28天的防腐测试，结果数据如表16：
表16
从表13可以看出，经过28天的防腐测试，该精华水中大肠埃希氏菌、铜绿假单胞菌、金黄色葡萄球菌、白色假丝酵母和黑曲霉的从第7天到第28天的检测结果均为0。
实施例6：
使用食品级植物源性复合抑菌剂制备洗面奶的具体方法为：
本实施例中洗面奶的成分如表17所示，
表17
所述食品级植物源性复合抑菌剂按重量份数包括55份的肉桂醛、12份的丁香酚和7份的反式邻甲氧基肉桂醛。
洗面奶的制备方法如下：
将A相、B相按用量称取后分别加热混合均匀，然后将B相加入到A相中低速搅拌。
对本实施例的洗面奶进行28天的防腐测试，结果数据如表18：
表18
从表15可以看出，经过28天的防腐测试，该洗面奶中大肠埃希氏菌、铜绿假单胞菌、金黄色葡萄球菌、白色假丝酵母和黑曲霉的从第7天到第28天的检测结果均为0。
Claims (10)
- 食品级植物源性复合抑菌剂在化妆品中的应用，所述食品级植物源性复合抑菌剂包括肉桂醛、丁香酚和反式邻甲氧基肉桂醛。
- 根据权利要求1所述的食品级植物源性复合抑菌剂在化妆品中的应用，其特征在于所述食品级植物源性复合抑菌剂在化妆品中的添加量为化妆品质量的0.04％～0.08％。
- 根据权利要求1或2所述的食品级植物源性复合抑菌剂在化妆品中的应用，其特征在于所述食品级植物源性复合抑菌剂按重量份数包括15～85份肉桂醛、3～60份丁香酚和3～15份的反式邻甲氧基肉桂醛。
- 根据权利要求3所述的食品级植物源性复合抑菌剂在化妆品中的应用，其特征在于所述食品级植物源性复合抑菌剂按重量份数包括55份的肉桂醛、12份的丁香酚和7份的反式邻甲氧基肉桂醛。
- 根据权利要求1或2所述的食品级植物源性复合抑菌剂在化妆品中的应用，其特征在于所述化妆品包括膏霜、乳液、精华液、精华水或洗面奶。
- 根据权利要求5所述的食品级植物源性复合抑菌剂在化妆品中的应用，其特征在于所述食品级植物源性复合抑菌剂在膏霜中的添加量为膏霜质量的0.05％。
- 根据权利要求5所述的食品级植物源性复合抑菌剂在化妆品中的应用，其特征在于所述食品级植物源性复合抑菌剂在乳液中的添加量为乳液质量的0.05％。
- 根据权利要求5所述的食品级植物源性复合抑菌剂在化妆品中的应用，其特征在于所述食品级植物源性复合抑菌剂在精华液中的添加量为精华液质量的0.05％。
- 根据权利要求5所述的食品级植物源性复合抑菌剂在化妆品中的应用，其特征在于所述食品级植物源性复合抑菌剂在精华水中的添加量为精华水质量的0.04％～0.08％。
- 根据权利要求5所述的食品级植物源性复合抑菌剂在化妆品中的应用，其特征在于所述食品级植物源性复合抑菌剂在洗面奶中的添加量为洗面奶质量的0.05％。
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