WO2021143060A1 - 一种厚朴植物防腐抑菌组合物及其制备工艺与应用 - Google Patents
一种厚朴植物防腐抑菌组合物及其制备工艺与应用 Download PDFInfo
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- WO2021143060A1 WO2021143060A1 PCT/CN2020/099129 CN2020099129W WO2021143060A1 WO 2021143060 A1 WO2021143060 A1 WO 2021143060A1 CN 2020099129 W CN2020099129 W CN 2020099129W WO 2021143060 A1 WO2021143060 A1 WO 2021143060A1
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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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/52—Stabilizers
- A61K2800/524—Preservatives
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- the invention relates to a magnolia officinalis plant antiseptic and bacteriostatic composition and its preparation process and application.
- Microbial contamination will cause a series of changes in cosmetics such as discoloration, precipitation, and taste change, which will not only greatly affect the quality of cosmetics, but also affect the user experience.
- the addition of chemical preservatives is mainly used to avoid the spoilage of cosmetics.
- the addition of pure chemical preservatives often has certain safety or irritation problems.
- Magnolia Bark extract has a wide range of antibacterial activities, of which the inhibitory effect on Staphylococcus aureus is the strongest.
- the invention intends to effectively reduce the proportion of pure chemical preservatives in cosmetics through the antiseptic effect of Magnolia Bark extract, thereby avoiding potential safety risks as much as possible.
- the purpose of the present invention is to overcome the defects of the prior art and provide a magnolia officinalis plant antiseptic and antibacterial composition, which contains natural plant extracts, is milder and has less potential risk than traditional pure chemical preservatives, and can be safely applied In the cosmetics industry.
- Another object of the present invention is to provide a preparation process and application of the antiseptic and antibacterial composition of Magnolia officinalis plant.
- a technical solution for achieving the above-mentioned objective is: a magnolia officinalis plant antiseptic and bacteriostatic composition, which is composed of the following components by weight percentage:
- magnolia plant antiseptic and antibacterial composition wherein the solvent is selected from one or more of 1,2-propanediol, 1,3-butanediol, 1,2-pentanediol and glycerin.
- magnolia plant antiseptic and antibacterial composition wherein, in the magnolia bark extract, the mass percentage of magnolol is not less than 3.5%, and the mass percentage of magnolol is not less than 6.5 %.
- the invention also provides a preparation process of the Magnolia officinalis plant antiseptic and antibacterial composition according to claim 1, comprising the following steps:
- Magnolia officinalis extract preparation steps Weigh an appropriate amount of Magnolia officinalis dry medicinal material, add it to the ethanol aqueous solution with a volume fraction of 70% after crushing, the material-to-liquid ratio of Magnolia officinalis dry medicinal material to the ethanol aqueous solution is 1:8g/L, at 75 Reflux and extract twice at °C, combine the two extracts for filtration and enrichment to obtain the Magnolia officinalis crude extract; centrifuge the Magnolia officinalis crude extract to remove the insoluble matter, and use the activated carbon decolorization process to obtain the decolorized Magnolia officinalis extract , The ethanol is removed by concentration under reduced pressure and then freeze-dried to obtain Magnolia Bark Extract;
- step S2 dissolving the magnolia bark extract prepared in step S1 in a solvent, and sonicating until it is completely mixed uniformly, to obtain the magnolia bark plant antiseptic and antibacterial composition.
- the activated carbon decolorization process is: adding 3 to 5% volume concentration of activated carbon to the crude extract of Magnolia officinalis by centrifugation to remove insoluble matter, and heating at 50°C Decolorization for 1h under water bath conditions.
- the mass percentage of magnolol is not less than 3.5%, and the mass percentage of magnolol is not less than 6.5% .
- the present invention also provides an application of the Magnolia officinalis plant antiseptic and bacteriostatic composition according to claim 1.
- the Magnolia officinalis plant antiseptic and bacteriostatic composition is used in cosmetics, and the Magnolia officinalis plant antiseptic and bacteriostatic composition is used in cosmetics.
- the quality of the cosmetics is 3 to 5% of the total quality of the cosmetics.
- the cosmetics are creams or lotions.
- Magnolia officinalis plant antiseptic and antibacterial composition Using the Magnolia officinalis plant antiseptic and antibacterial composition and its preparation process and application technical solutions, the Magnolia officinalis plant antiseptic and antibacterial composition, added to creams and lotions, can also pass the regulations of the United States Pharmacopoeia. Anti-corrosion challenge test, with broad-spectrum sterilization effect, has a good market application prospect and market for cosmetics.
- Figure 1 is a calibration diagram of the content of magnolol and honokiol in Magnolia officinalis extract.
- a preparation process of Magnolia officinalis plant antiseptic and antibacterial composition includes the following steps:
- Magnolia officinalis extract preparation steps Weigh an appropriate amount of Magnolia officinalis dry medicinal material, add it to the ethanol aqueous solution with a volume fraction of 70% after crushing, the material-to-liquid ratio of Magnolia officinalis dry medicinal material to the ethanol aqueous solution is 1:8g/L, at 75 Reflux and extract twice at °C, combine the two extracts for filtration and enrichment to obtain the Magnolia officinalis crude extract; centrifuge the Magnolia officinalis crude extract to remove insoluble matter, and use the activated carbon decolorization process.
- the activated carbon decolorization process is: removal by centrifugation
- the crude extract of Magnolia officinalis was added with 3 to 5% volume concentration of activated carbon.
- the decolorized extract of Magnolia officinalis was obtained by filtration, which was concentrated under reduced pressure to remove the ethanol and then freeze-dried. , That is, Magnolia Bark Extract; In the Magnolia Bark Extract, the mass percentage of honokiol is not less than 3.5%, and the mass percentage of magnolol is not less than 6.5%;
- magnolia bark extract prepared in step S1 dissolving the magnolia bark extract prepared in step S1 in a solvent, and sonicating until it is completely mixed uniformly, to obtain the magnolia bark plant antiseptic and antibacterial composition.
- the solvent is selected from one or more of 1,2-propylene glycol, 1,3-butanediol, 1,2-pentanediol and glycerin.
- the mass percentage of magnolol is not less than 3.5%, and the mass percentage of magnolol is not less than 6.5%.
- Escherichia coli, Pseudomonas aeruginosa, and Staphylococcus aureus are all 1-6 ⁇ 107CFU/mL, while Candida albicans, Aspergillus niger is 1-6 ⁇ 107CFU/mL, and the bacterial suspension after configuration is stored at 4°C for later use.
- Magnolia Bark Extract is prepared into a specific concentration of Magnolia Bark Extract by a doubling and a half dilution method. 3mL Magnolia Bark Extract and 3mL Trypticase Soy Broth (TSB) are added to each test tube, and 0.3mL bacterial suspension is added , Ensure that the concentration of bacteria in each tube is 1-6 ⁇ 106CFU/mL, and the concentration of fungi is 1-6 ⁇ 105CFU/mL, set up positive and negative control groups, and culture at 30°C for 24h (bacteria) and 48h (fungi) , Through the comparison of turbidity, the lowest concentration of Magnolia Bark extract under the condition of adding Magnolia Bark extract for clarification is the antibacterial MIC of Magnolia Bark extract. The method is also applicable when the Magnolia Bark extract is replaced with 1,2-pentanediol, p-hydroxyacetophenone, honokiol and magnolol.
- a magnolia officinalis plant antiseptic and bacteriostatic composition is composed of the following components in percentage by weight: Magnolia officinalis extract 20% and 1,2-pentanediol 80%.
- a preparation process of a Magnolia officinalis plant antiseptic and antibacterial composition comprising the following steps: adding 2g of Magnolia officinalis extract to 8g of 1,2-pentanediol, and ultrasonicating for 5 minutes until it is completely mixed uniformly to obtain Magnolia officinalis plant Antiseptic and antibacterial composition for use.
- a magnolia officinalis plant antiseptic and bacteriostatic composition is composed of the following components in percentage by weight: magnolia bark extract 25% and 1,2-pentanediol 75%.
- a preparation process of Magnolia officinalis plant antiseptic and bacteriostatic composition comprising the following steps: add 2.5g of Magnolia officinalis extract to 7.5g of 1,2-pentanediol, and sonicate it for 5 minutes until it is completely mixed and uniform.
- the antiseptic and bacteriostatic composition of Pak plant is reserved for use.
- a magnolia officinalis plant antiseptic and antibacterial composition is composed of the following components by weight percentage: Magnolia Bark extract 30% and 1,2-pentanediol 70%.
- a preparation process of Magnolia officinalis plant antiseptic and bacteriostatic composition comprising the following steps: adding 3g of Magnolia officinalis extract to 7g of 1,2-pentanediol, and sonicating it for 5 minutes until it is completely mixed uniformly to obtain Magnolia officinalis plant
- the antiseptic and antibacterial composition is reserved for future use.
- magnolia plant antiseptic and antibacterial composition obtained in Examples 1-3 has excellent broad-spectrum antibacterial effects, and the antibacterial MIC is lower than 1,2-pentanediol, honokiol, The antibacterial MIC of Magnolia Bark Extract itself is even close to the level of pure chemical preservative p-hydroxyacetophenone.
- magnolia plant antiseptic and antibacterial composition obtained from Examples 1-3 is added to cream cosmetics
- magnolia plant antiseptic and antibacterial composition obtained from Examples 1-3 is added to cream cosmetics
- the specific application examples are as follows:
- application examples 1 to 4 were prepared, and the cream cosmetics of application examples 1 to 4 were subjected to anti-corrosion tests.
- the specific anti-corrosion challenge methods and evaluation criteria are as follows:
- the method was carried out according to the United States Pharmacopoeia (USP), 3 sample bottles assembled with 50g samples were inoculated with Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Candida albicans and Aspergillus niger To make the final bacterial content of each gram of sample 1-6 ⁇ 106CFU/g, mold yeast content 1-6 ⁇ 105CFU/g, mix well, and place them at 30 ⁇ 1°C and 25 ⁇ Cultivate in a 1°C constant temperature incubator, and then test the number of survivors of each bacteria on the 0th, 7th, 14th, and 28th days.
- USP United States Pharmacopoeia
- the effectiveness criterion is: the concentration of live bacteria should be less than 0.1% of the initial concentration after 14 days of culture, and no longer increase; the fungal concentration of 14 days of culture should be maintained or lower than the initial concentration, and no longer increase.
- magnolia plant antiseptic and antibacterial composition obtained in Examples 1-3 can pass the antiseptic challenge excellently when added to moisturizing lotion cosmetics, and its antiseptic ability is basically equivalent to that of pure chemical preservatives, and has very good performance. Application prospects and development value.
- Magnolia officinalis plant antiseptic and antibacterial composition in moisturizing lotion cosmetics.
- the Magnolia officinalis plant antiseptic and antibacterial composition obtained from Examples 1-3 is added to it, and the application example formula of pure chemical preservative is compared, and the specific application is Examples are as follows:
- the Magnolia officinalis plant antiseptic and antibacterial composition provided by the present invention has a broad-spectrum bactericidal effect when no chemical preservative: p-hydroxyacetophenone is used and the addition amount is 3 to 5%.
- the antiseptic ability is basically equivalent to the combination of pure chemical preservatives, and it has a good application prospect and market in the cosmetics market.
- the Magnolia officinalis plant antiseptic and antibacterial composition has a broad-spectrum bactericidal effect when no chemical preservative, that is, p-hydroxyacetophenone, is added in an amount of 3 to 5%, and the antiseptic ability is basically the same as that of pure chemical antiseptic.
- the combination of agents is equivalent, and it has a good application prospect and market in the cosmetics market.
- Magnolia officinalis plant antiseptic and antimicrobial composition and its preparation process and application of the present invention.
- the Magnolia officinalis plant antiseptic and antimicrobial composition is added to creams and lotions, and can also pass the US Pharmacopoeia regulations.
- Anti-corrosion challenge test has a broad-spectrum sterilization effect, and has a good market application prospect and market for cosmetics.
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Abstract
一种厚朴植物防腐抑菌组合物，由以下重量百分比含量的组分组成:厚朴提取物20～30％；溶剂70～80％。含有天然植物提取物，相比传统的纯化学防腐剂更加温和且潜在风险更小，可安全应用于化妆品行业中。还公开了一种厚朴植物防腐抑菌组合物的制备工艺与应用，厚朴植物防腐抑菌组合物添加于膏霜和润肤水中，也能很好的通过美国药典规定的防腐挑战测试，具有广谱杀菌效果，具有良好的化妆品市场应用前景和市场。
Description
本发明涉及一种厚朴植物防腐抑菌组合物及其制备工艺与应用。
微生物污染会使得化妆品出现变色、沉淀、变味等一系列变化，不仅会极大的影响化妆品品质，更会影响用户体验。目前主要通过化学防腐剂的添加来避免化妆品的腐败变质，然而纯化学防腐剂的添加往往都存在一定的安全或者刺激性问题。
全国中西医结合皮肤性病学术会议论文汇编.2012上发表了赵暕等的《甲醛与乌洛托品溶液致变应性接触性皮炎1例》，研究表明乌洛托品会导致甲醛释放，从而导致接触性皮炎。
航天护理年会.2007上发表了顾敏等的《皮炎湿疹类患者接触性致敏原分析》，研究表明布罗波尔是导致皮炎湿疹的十大过敏源之一。
许多天然植物具有很好的抗菌效果，添加天然植物作为部分的防腐替代直至完全使用天然植物进行化妆品防腐具有良好的市场前景。例如：
中药材，2009(05):147-150上发表了刘莹的《厚朴抑菌活性成分提取方法研究》，研究表明厚朴提取物对五味子根腐病菌具有很好的抑制作用。
中国美容医学，2010(11):108-109上发表了张建国的《厚朴超临界提出物中厚朴酚与和厚朴酚抑菌性研究》，研究表明实验表明厚朴提取物中厚朴酚、和厚朴酚均具有出色的抗菌能力。
辽宁师范大学，2010上发表了李慧的《厚朴中有效成分活性检测及结构鉴定》，研究表明厚朴提取物具有广泛的抗菌活性，其中对金黄色葡萄球菌的抑制作用最强。
本发明拟在通过厚朴提取物防腐功效，有效降低化妆品中纯化学防腐剂的用量占比从而尽可能的规避潜在安全风险。调研其他研究工作者的相关报道，均未见将厚朴提取物和厚朴酚及戊二醇复配的相关报道。
发明内容
本发明的目的是克服现有技术的缺陷，提供一种厚朴植物防腐抑菌组合物，含有天然植物提取物，相比传统的纯化学防腐剂更加温和且潜在风险更小，可安全应用于化妆品行业中。
本发明的另外一个目的是提供一种厚朴植物防腐抑菌组合物的制备工艺与应用。
实现上述目的一种技术方案是：一种厚朴植物防腐抑菌组合物，由以下重量百分比含量的组分组成：
厚朴提取物 20～30％；
溶剂 70～80％。
上述的一种厚朴植物防腐抑菌组合物，其中，所述溶剂选用1，2－丙二醇、1，3－丁二醇、1，2－戊二醇和甘油中的一种或多种。
上述的一种厚朴植物防腐抑菌组合物，其中，所述厚朴提取物中，和厚朴酚的质量百分含量不低于3.5％，厚朴酚的质量百分含量不低于6.5％。
本发明还提供了一种如权利要求1所述的厚朴植物防腐抑菌组合物的制备工艺，包括以下步骤：
S1，厚朴提取物制备步骤：称取适量厚朴干药材，粉碎后加入体积分数为70％的乙醇水溶液中，厚朴干药材与乙醇水溶液的料液比为1：8g/L，在75℃条件下回流提取2次，合并两次提取液进行过滤富集，即得厚朴粗提取液；将厚朴粗提取液离心去除不溶物，通过活性炭脱色工艺，得脱色后的厚朴提取液，经减压浓缩去除乙醇后经冷冻干燥，即得厚朴提取物；
S2，将步骤S1制得的厚朴提取物溶解于溶剂中，超声至完全混合均匀，即可得到厚朴植物防腐抑菌组合物。
上述的厚朴植物防腐抑菌组合物的制备工艺，步骤S1中，所述活性炭脱色工艺为：在离心去除不溶物的厚朴粗提取液中加入3～5％体积浓度的活性炭，在50℃水浴条件下脱色1h。
上述的厚朴植物防腐抑菌组合物的制备工艺，所述厚朴提取物中，和厚朴酚的质量百分含量不低于3.5％，厚朴酚的质量百分含量不低于6.5％。
本发明还提供了一种如权利要求1所述的厚朴植物防腐抑菌组合物的应用，所述厚朴植物防腐抑菌组合物应用在化妆品中，所述厚朴植物防腐抑菌组合物的质量为所述化妆品总质量的3～5％。
上述的厚朴植物防腐抑菌组合物的应用，所述化妆品为膏霜或润肤水。
采用本发明的厚朴植物防腐抑菌组合物及其制备工艺与应用的技术方案，厚朴植物防腐抑菌组合物，添加于膏霜和润肤水中，也能很好的通过美国药典规定的防腐挑战测试，具有广谱杀菌效果，具有良好的化妆品市场应用前景和市场。
图1为厚朴提取物中厚朴酚以及和厚朴酚的含量的标定图。
为了使本技术领域的技术人员能更好地理解本发明的技术方案，下面结合附图对其具体实施方式进行详细地说明：
一种厚朴植物防腐抑菌组合物的制备工艺，包括以下步骤：
S1，厚朴提取物制备步骤：称取适量厚朴干药材，粉碎后加入体积分数为70％的乙醇水溶液中，厚朴干药材与乙醇水溶液的料液比为1：8g/L，在75℃条件下回流提取2次，合并两次提取液进行过滤富集，即得厚朴粗提取液；将厚朴粗提取液离心去除不溶物，通过活性炭脱色工艺，活性炭脱色工艺为：在离心去除不溶物的厚朴粗提取液中加入3～5％体积浓度的活性炭，在50℃水浴条件下脱色1h后，经过滤得脱色后的厚朴提取液，经减压浓缩去除乙醇后经冷冻干燥，即得厚朴提取物；厚朴提取物中，和厚朴酚的质量百分含量不低于3.5％，厚朴酚的质量百分含量不低于6.5％；
S2，将步骤S1制得的厚朴提取物溶解于溶剂中，超声至完全混合均匀，即可得到厚朴植物防腐抑菌组合物。溶剂选用1，2－丙二醇、1，3－丁二醇、1，2－戊二醇和甘油中的一种或多种。
请参阅图1，厚朴提取物中厚朴酚以及和厚朴酚的含量进行标定，具体结果如下：
HPLC条件，液相柱：Agilent Zorbax C18(4.6*250mm，5μm)，波长：294nm， 柱温：35℃，流动相：0-25min，30％甲醇，70％水。
依据上述HPLC条件，以厚朴酚浓度(C)为横坐标，峰面积(S)为纵坐标，得厚朴酚线性方程：S＝14252C+34.956，R2＝0.9994,在使用浓度范围(0.01-1.43mg·mL-1)内具有很好的线性关系；以和厚朴酚浓度(C)为横坐标，峰面积(S)为纵坐标，得和厚朴酚线性方程：S＝14631C+10.872，R2＝0.999,在使用浓度范围(0.01-1.01mg·mL-1)内具有很好的线性关系；厚朴提取物中厚朴酚、和厚朴酚含量测定，保证浓度在上述范围内平行测定三次代入对应厚朴酚、和厚朴酚线性方程即得。
经重复实验测得所述厚朴提取物中，和厚朴酚质量百分含量不低于3.5％、厚朴酚质量百分含量不低于6.5％。
为使得后续可将厚朴提取物与现有化学防腐剂进行复配，需对1,2-戊二醇、对羟基苯乙酮、和厚朴酚、厚朴酚及厚朴提取物的抑菌MIC进行测定，具体实验方法如下：
选取复苏最新版美国药典(USP)关于化妆品微生物限定的五种菌，即大肠埃希氏菌(ATCC 11229)、铜绿假单胞菌(ATCC 9027)、金黄色葡萄球菌(ATCC 6538)、白假丝酵母菌(ATCC 10231)、黑曲霉(ATCC 16404)。
通过菌落复苏、计数等操作，配置特定浓度的菌悬液，即大肠埃希氏菌、铜绿假单胞菌、金黄色葡萄球菌均为1-6×107CFU/mL，而白假丝酵母菌、黑曲霉均为1-6×107CFU/mL，配置完成后的菌悬液置于4℃贮存备用。
厚朴提取物通过倍半稀释方法配置成特定浓度的厚朴提取液，每一试管中加入3mL厚朴提取液及3mL胰酪胨大豆肉汤培养基(TSB)，并加入0.3mL菌悬液，确保每一管中细菌浓度在1-6×106CFU/mL，真菌浓度在1-6×105CFU/mL，设立阳性及阴性对照组，在30℃条件下培养24h(细菌)、48h(真菌)，通过浊度对比，在加入厚朴提取液为澄清条件下的厚朴提取液最低浓度即为厚朴提取物的抑菌MIC。将厚朴提取物换成1,2-戊二醇、对羟基苯乙酮、和厚朴酚、厚朴酚，该方法同样适用。
厚朴提取物及1,2-戊二醇、对羟基苯乙酮、和厚朴酚、厚朴酚的抑菌MIC进行测定，具体实验结果如表1所示：
| MIC(g/L) | 大肠埃希氏菌 | 金黄色葡萄球菌 | 铜绿假单胞菌 | 白假丝酵母菌 | 黑曲霉 |
| 厚朴提取物 | 60 | 60 | 30 | 60 | 30 |
| 1,2-戊二醇 | 30 | 30 | 30 | 30 | 60 |
| 对羟基苯乙酮 | 5 | 5 | 2.5 | 2.5 | 5 |
| 和厚朴酚 | 8 | 8 | 8 | 8 | 4 |
| 厚朴酚 | 8 | 8 | 8 | 8 | 8 |
表1
针对上述抑菌MIC数据，选定厚朴提取物、1,2-戊二醇进行复配，发现此组合抑菌能力可以得到极好的提升，为更好地阐述其复配结果，下面结合具体实施例进行进一步说明。
实施例1：
一种厚朴植物防腐抑菌组合物，由以下重量百分比含量的组分组成：厚朴提取物20％、1,2-戊二醇80％。
一种厚朴植物防腐抑菌组合物的制备工艺，包含以下步骤：将2g厚朴提取物、加至8g的1,2-戊二醇中，经5min超声至完全混合均匀，得厚朴植物防腐抑菌组合物，备用。
实施例2：
一种厚朴植物防腐抑菌组合物，由以下重量百分比含量的组分组成：厚朴提取物25％、1,2-戊二醇75％。
一种厚朴植物防腐抑菌组合物的制备工艺，包含以下步骤：将2.5g厚朴提取物、加至7.5g的1,2-戊二醇中，经5min超声至完全混合均匀，得厚朴植物防腐抑菌组合物，备用。
实施例3：
一种厚朴植物防腐抑菌组合物，由以下重量百分比含量的组分组成：厚朴提取物30％、1,2-戊二醇70％。
一种厚朴植物防腐抑菌组合物的制备工艺，包含以下步骤：将3g厚朴提取物、 加至7g的1,2-戊二醇中，经5min超声至完全混合均匀，得厚朴植物防腐抑菌组合物，备用。
抑菌MIC试验：
为更好地验证实施例1－3所得厚朴植物防腐抑菌组合物的防腐效果，首先依据抑菌MIC方式进行测定实施例1－3所得厚朴植物防腐抑菌组合物抑菌MIC，具体结果如表2所示：
| MIC(g/L) | 大肠埃希氏菌 | 金黄色葡萄球菌 | 铜绿假单胞菌 | 白假丝酵母菌 | 黑曲霉 |
| 实施例1 | 2.5 | 2 | 2.5 | 2 | 2 |
| 实施例2 | 2.5 | 2 | 2.5 | 2 | 2 |
| 实施例3 | 1 | 1.5 | 1.5 | 1 | 1 |
表2
根据表2数据，可以得出实施例1－3所得厚朴植物防腐抑菌组合物的广谱抑菌效果优异，且抑菌MIC均低于1，2－戊二醇、和厚朴酚、厚朴提取物本身的抑菌MIC，甚至接近纯化学防腐剂对羟基苯乙酮的水平。
防腐验证试验：
为更好体现所得厚朴植物防腐抑菌组合物的防腐效果，将其应用于实际膏霜类化妆品中，由实施例1－3所得的厚朴植物防腐抑菌组合物加入膏霜类化妆品中，并对比纯化学防腐剂的应用实例配方，具体应用实例如下：
| 原料名称 | 应用实例1 | 应用实例2 | 应用实例3 | 应用实例4 |
| 丙烯酸(脂)类 | 0.30％ | 0.30％ | 0.30％ | 0.30％ |
| 聚二甲基硅氧烷 | 1.00％ | 1.00％ | 1.00％ | 1.00％ |
| 黄原胶 | 0.15％ | 0.15％ | 0.15％ | 0.15％ |
| 透明质酸钠 | 0.20％ | 0.20％ | 0.20％ | 0.20％ |
| 透明质酸 | 0.20％ | 0.20％ | 0.20％ | 0.20％ |
| 十三烷醇偏苯三酸酯 | 2.00％ | 2.00％ | 2.00％ | 2.00％ |
| 牛油果树果脂 | 2.00％ | 2.00％ | 2.00％ | 2.00％ |
| 青刺果油 | 0.10％ | 0.10％ | 0.10％ | 0.10％ |
| 甘油硬脂酸酯 | 1.00％ | 1.00％ | 1.00％ | 1.00％ |
| 马齿苋提取物 | 3.00％ | 3.00％ | 3.00％ | 3.00％ |
| 氨甲基丙醇 | 0.10％ | 0.10％ | 0.10％ | 0.10％ |
| 实施例1制得组合物 | 3.00％ | － | － | － |
| 实施例2制得组合物 | － | 4.00％ | － | － |
| 实施例3制得组合物 | － | － | 5.00％ | － |
| 对羟基苯乙酮 | － | － | － | 0.25％ |
| 戊二醇 | － | － | － | 3.00％ |
| 水 | 86.95％ | 85.95％ | 84.95％ | 86.70％ |
表3
按照表3的配方制得应用实例1～4，将应用实例1～4的膏霜类化妆品进行防腐试验，具体防腐挑战方法及评价标准如下：
方法依据美国药典(USP)进行，3组装有50g样品的样品瓶中接种金黄色葡萄球菌、大肠埃希氏菌、铜绿假单胞菌、金黄色葡萄球菌、白假丝酵母菌和黑曲霉菌的混合菌悬液，使每克样品最终含细菌量为1－6×106CFU/g，霉菌酵母菌量为1－6×105CFU/g，充分混匀，分别置于30±1℃和25±1℃恒温培养箱中培养，然后在第0、7、14、28天分别检验每种菌的存活数量，存活数量越少，其防腐剂抗菌效果越好。有效性标准为：培养14天时活的细菌浓度应小于起始浓度的0.1％，并不再增加；培养14天真菌浓度应保持或低于起始浓度，并不再增加。
应用实例1～4的防腐挑战结果如表4所示：
根据表4数据，表明实施例1－3所得厚朴植物防腐抑菌组合物在加入润肤水类化妆品，可以优异的通过防腐挑战，其防腐能力基本与纯化学防腐剂相当，具有很好的应用前景和开发价值。
厚朴植物防腐抑菌组合物在润肤水类化妆品中的应用，由实施例1-3所得的厚朴植物防腐抑菌组合物加入其中，并对比纯化学防腐剂的应用实例配方，具体应用实例如下：
| 原料名称 | 应用实例5 | 应用实例6 | 应用实例7 | 应用实8 |
| 甘油 | 3.00％ | 3.00％ | 3.00％ | 3.00％ |
| 甘油聚醚－26 | 3.00％ | 3.00％ | 3.00％ | 3.00％ |
| 羟乙基纤维素 | 0.05％ | 0.05％ | 0.05％ | 0.05％ |
| 透明质酸钠 | 0.02％ | 0.02％ | 0.02％ | 0.02％ |
| 透明质酸 | 0.02％ | 0.02％ | 0.02％ | 0.02％ |
| β－葡萄糖 | 3.00％ | 3.00％ | 3.00％ | 3.00％ |
| 马齿苋提取物 | 3.00％ | 3.00％ | 3.00％ | 3.00％ |
| 实施例1制得组合物 | 3.00％ | － | － | － |
| 实施例2制得组合物 | － | 4.00％ | － | － |
| 实施例3制得组合物 | － | － | 5.00％ | － |
| 对羟基苯乙酮 | － | － | － | 0.25％ |
| 戊二醇 | － | － | － | 3.00％ |
| 水 | 84.91％ | 83.91％ | 82.91％ | 84.60％ |
表5
厚朴植物防腐抑菌组合物在润肤水类化妆品中的应用，上述应用实例的防腐挑战结果如下：
按照表3的配方制得应用实例5～8，将应用实例5～8的润肤水类化妆品进行防腐试验，防腐挑战结果如表6所示：
表6
根据表6数据，表明实施例1－3所得厚朴植物防腐抑菌组合物在加入润肤水类化妆品中可以优异的通过防腐挑战，其防腐能力基本与纯化学防腐剂相当，具有很好的应用前景和开发价值。
综上所述，本发明提供的一种厚朴植物防腐抑菌组合物在不使用化学防腐剂：对羟基苯乙酮情况下，添加量为3－5％时，具有广谱杀菌效果，且防腐能力基本与纯化学防腐剂的组合相当，具有良好的化妆品市场应用前景和市场。
本发明的厚朴植物防腐抑菌组合物，在不使用化学防腐剂即对羟基苯乙酮情况下，添加量为3－5％时，具有广谱杀菌效果，且防腐能力基本与纯化学防腐剂的组合相当，具有良好的化妆品市场应用前景和市场。
综上所述，本发明的厚朴植物防腐抑菌组合物及其制备工艺与应用，厚朴植物防腐抑菌组合物添加于膏霜和润肤水中，也能很好的通过美国药典规定的防腐挑战测试，具有广谱杀菌效果，具有良好的化妆品市场应用前景和市场。
本技术领域中的普通技术人员应当认识到，以上的实施例仅是用来说明本发 明，而并非用作为对本发明的限定，只要在本发明的实质精神范围内，对以上所述实施例的变化、变型都将落在本发明的权利要求书范围内。
Claims (8)
- 一种厚朴植物防腐抑菌组合物，其特征在于，由以下重量百分比含量的组分组成：厚朴提取物 20～30％；溶剂 70～80％。
- 如权利要求1所述的一种厚朴植物防腐抑菌组合物，其特征在于，所述溶剂选用1，2－丙二醇、1，3－丁二醇、1，2－戊二醇和甘油中的一种或多种。
- 如权利要求1所述的一种厚朴植物防腐抑菌组合物，其特征在于，所述厚朴提取物中，和厚朴酚的质量百分含量不低于3.5％，厚朴酚的质量百分含量不低于6.5％。
- 一种如权利要求1所述的厚朴植物防腐抑菌组合物的制备工艺，其特征在于，包括以下步骤：S1，厚朴提取物制备步骤：称取适量厚朴干药材，粉碎后加入体积分数为70％的乙醇水溶液中，厚朴干药材与乙醇水溶液的料液比为1：8g/L，在75℃条件下回流提取2次，合并两次提取液进行过滤富集，即得厚朴粗提取液；将厚朴粗提取液离心去除不溶物，通过活性炭脱色工艺，得脱色后的厚朴提取液，经减压浓缩去除乙醇后经冷冻干燥，即得厚朴提取物；S2，将步骤S1制得的厚朴提取物溶解于溶剂中，超声至完全混合均匀，即可得到厚朴植物防腐抑菌组合物。
- 如权利要求4所述的厚朴植物防腐抑菌组合物的制备工艺，其特征在于，步骤S1中，所述活性炭脱色工艺为：在离心去除不溶物的厚朴粗提取液中加入3～5％体积浓度的活性炭，在50℃水浴条件下脱色1h。
- 如权利要求4所述的厚朴植物防腐抑菌组合物的制备工艺，其特征在于，所述厚朴提取物中，和厚朴酚的质量百分含量不低于3.5％，厚朴酚的质量百分含量不低于6.5％。
- 一种如权利要求1所述的厚朴植物防腐抑菌组合物的应用，其特征在于，所述厚朴植物防腐抑菌组合物应用在化妆品中，所述厚朴植物防腐抑菌组合物的质量 为所述化妆品总质量的3～5％。
- 一种如权利要求1所述的厚朴植物防腐抑菌组合物的应用，其特征在于，所述化妆品为膏霜或润肤水。
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