WO2021139194A1 - 一种用于洗手液的纳米植物抗菌剂及制备方法 - Google Patents

一种用于洗手液的纳米植物抗菌剂及制备方法 Download PDF

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WO2021139194A1
WO2021139194A1 PCT/CN2020/113984 CN2020113984W WO2021139194A1 WO 2021139194 A1 WO2021139194 A1 WO 2021139194A1 CN 2020113984 W CN2020113984 W CN 2020113984W WO 2021139194 A1 WO2021139194 A1 WO 2021139194A1
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nano
antibacterial agent
hand sanitizer
plant antibacterial
plant
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PCT/CN2020/113984
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English (en)
French (fr)
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应光辉
应宗效
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浙江神英科技股份有限公司
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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]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005—Antimicrobial preparations
    • 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
    • A61Q19/10—Washing or bathing preparations
    • 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
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/413—Nanosized, i.e. having sizes below 100 nm

Definitions

  • the invention relates to the field of daily chemicals, in particular to a nano plant antibacterial agent for hand sanitizer and a preparation method.
  • Antibacterial hand sanitizer is accepted by more and more consumers as a daily cleaning product. It is used in hospitals, schools and other public places, and has a good instant sterilization effect. Initially, restricted by living conditions and the market, people usually wash their hands with soap, soap, and washing powder. Although they can achieve a certain cleaning effect, they have a stimulating effect on the skin and have poor antibacterial effects.
  • antibacterial agents various antibacterial agents are used in hand sanitizers.
  • many antibacterial agents have side effects.
  • triclocarban and triclosan are the most widely used antibacterial agents, but studies have shown that they are harmful to the reproduction and development of animals. Continued use may cause drug resistance problems. Short-term exposure to low-dose triclosan may also be possible Causes allergies and dermatitis.
  • parachloro-m-xylenol entering the human body through the esophagus will cause necrosis of gastrointestinal mucosal cells, imbalance of intestinal flora and other adverse effects, and it is harmful to fish and is not environmentally friendly.
  • the amount of antibacterial agents added is gradually increasing, and the side effects are getting bigger and bigger.
  • Tea tree essential oil is a pure plant antibacterial agent with broad-spectrum antibacterial activity, and has a good killing or inhibitory effect on many bacteria and fungi.
  • tea tree oil has been developed into many types of products, such as preservatives, antibacterial agents and fragrances, and is mainly used in many fields such as cosmetics, medicines, food fragrances and beauty industries.
  • tea tree oil has also been used in advanced skin care products, personal care products, plant feeds, and furniture cleaning and sterilization products. Because of its safety, environmental protection, and strong antibacterial properties, tea tree oil is in great demand in domestic and foreign markets. And has broad development and utilization value.
  • Litsea cubeba It not only has broad-spectrum antibacterial properties, but also contains ⁇ -pinene with a special pine aroma; it contains camphene and is used in lavender oil cosmetics, soaps, deodorants and fruits.
  • plant antibacterial is a manifestation of the whole plant.
  • antibacterial plants contain alkaloids, polysaccharides, saponins, organic acids, etc.
  • the simple purification may cause the extract to be inactivated.
  • antibacterial plants In order to use antibacterial plants for antibacterial, it reflects the comprehensive antibacterial effect.
  • the antibacterial nanometerization of plants is a better direction.
  • the present invention proposes a nano plant antibacterial agent for hand sanitizer, which imparts certain activity to the plant antibacterial agent through nanometerization without leaching and purification. Treatment, comprehensive utilization of the antibacterial function of antibacterial plants. Further, the present invention proposes a preparation method of the nano plant antibacterial agent.
  • a method for preparing nano-plant antibacterial agent for hand sanitizer its key feature is: the specific preparation method is as follows:
  • step (1) Disperse the coarsely pulverized materials in step (1) with sodium chloride, magnesium nitrate, and polylysine evenly, and then through jet milling, they are micronized to nanometer level under the protection of nitrogen to obtain nanopowder;
  • step (3) The nano powder obtained in step (2) is added to the sodium alginate solution, ultrasonically dispersed, and then spray-dried under high pressure to obtain a nano plant antibacterial agent for hand sanitizer.
  • a mixture of fruits, flowers, and leaves of Litsea cubeba is selected for the purpose of comprehensively utilizing the antibacterial properties of Litsea cubeba. More preferably, the collected fruits, flowers, and leaves of Litsea cubeba are mixed in a mass ratio of 1:0.1:10. Litsea cubeba, pungent in nature, slightly bitter, aromatic, non-toxic. It has good antibacterial properties and is often used as a natural antifungal agent in feed.
  • Litsea cubeba such as ⁇ -pinene: with special pine aroma; camphene is used in lavender oil cosmetics, soaps, deodorants and fruit-based food flavors; ⁇ -Myrcene has a balsamic scent, can be used in citrus cologne and deodorant, and can be used to synthesize linalool, geraniol, citronellol, ionone and other precious fragrances.
  • ⁇ -pinene with special pine aroma
  • camphene is used in lavender oil cosmetics, soaps, deodorants and fruit-based food flavors
  • ⁇ -Myrcene has a balsamic scent, can be used in citrus cologne and deodorant, and can be used to synthesize linalool, geraniol, citronellol, ionone and other precious fragrances.
  • antibacterial materials for hand sanitizers if they are refined, they will increase the cost and the volatilization and inactivation of the refined
  • the fruits, leaves and leaves of Litsea cubeba have excellent antibacterial function, which is a comprehensive effect of various activities. For this reason, the present invention ensures the antibacterial activity on the one hand by nano-forming the fruits, leaves and leaves of Litsea cubeba, on the other hand, avoids the complicated purification process, and can also give the hand sanitizer a fragrance effect when used in the absorbing liquid.
  • the pressure of the freeze-drying treatment environment in step (1) is 40-50 Pa
  • the temperature of the cold trap is -40°C to -45°C
  • the treatment time is 1-2 hours.
  • the coarse pulverization in step (1) refers to the use of a conventional pulverizer to pulverize the dried product to pass a 50-mesh sieve.
  • the coarsely pulverized material in step (2) is prepared with sodium chloride, magnesium nitrate, and polylysine in a mass ratio of 100:5-10:3-5:1-3; sodium chloride and magnesium nitrate are: Inorganic salt, on the one hand, as a salt can assist the later grinding to grind coarsely pulverized materials to nanometer level, on the other hand, sodium chloride and magnesium nitrate can penetrate the coarsely pulverized material to promote the refinement of the coarsely pulverized material; in addition, sodium chloride, Magnesium nitrate is a commonly used regulator in hand sanitizer, and will not affect the overall effect of hand sanitizer after use.
  • polylysine can not only penetrate the coarsely pulverized material to promote refinement, but also has a good antibacterial effect on gram-positive bacteria, gram-negative bacteria, yeasts and molds; it has good antibacterial effects on E. coli and Salmonella The antibacterial effect is very good.
  • the jet mill in step (2) adopts a supersonic jet mill, and more preferably a JSM-Q-3 jet mill.
  • the compressed air is frozen, filtered, and dried, it forms a supersonic jet into the pulverizing chamber through a nozzle.
  • the material is fluidized, and the accelerated material merges at the intersection of the jet airflows of several nozzles, causing violent collision, friction, and shearing to achieve ultra-fine pulverization of particles.
  • the pulverized material is transported to the impeller classification area by the rising airflow. Under the action of the centrifugal force of the grading wheel and the suction force of the fan, the coarse and fine powder are separated.
  • the coarse powder returns to the crushing chamber according to its own gravity and continues to be crushed.
  • the airflow enters the cyclone collector, the fine dust is collected by the bag filter, and the purified gas is discharged by the induced draft fan.
  • the adopted classification speed is 1800rpm-2000rpm, and nanometer-level powder is
  • the nano powder and the sodium alginate solution are dispersed in a mass ratio of 1:5, and the mass concentration of the sodium alginate solution is 2.5%;
  • the ultrasonic dispersion treatment adopts a power of 2000W, a frequency of 20KHZ, and a treatment of 35- 60min;
  • ultrasonic dispersion can disperse the agglomerated nanoparticles, so that the surface of the nanoparticles are in contact with sodium alginate; so that the sodium alginate can be evenly coated on the surface of the nanoparticles during spray drying.
  • high-pressure spray drying is used in step (3), the pressure of the atomizing gun is controlled at 1.5-2.0 MPa, the gun caliber is controlled at less than 0.5 mm, and the drying temperature is controlled at 80-90°C.
  • the sodium alginate is coated on the surface of the nano powder to obtain a nano plant antibacterial agent for hand sanitizer. On the one hand, it prevents the nanoparticles from agglomerating during storage, and on the other hand, it is added to the basic hand sanitizer It is easy to disperse and suspend evenly in the hand sanitizer, which is more convenient to use.
  • the invention also provides a nano plant antibacterial agent for hand sanitizer prepared by the above method.
  • the collected fruits, flowers, and leaves of Litsea cubeba are mixed and freeze-dried, then coarsely crushed, and ground with sodium chloride, magnesium nitrate, and polylysine to nano-powder by jet milling; and sodium alginate is coated on the surface; With the comprehensive antibacterial properties of Litsea cubeba, no purification, leaching and other treatments are required.
  • the obtained nano antibacterial agent is easy to disperse in the hand sanitizer and has excellent antibacterial activity. It has a two-child inhibitory effect on Escherichia coli, Salmonella, Aspergillus niger, etc. .
  • a nano plant antibacterial agent for hand sanitizer and its preparation method compared with the prior art, has the following
  • the present invention comprehensively utilizes plant antibacterial agents through nano-treatment, and at the same time prevents the active ingredients of the plant antibacterial active agents from being inactivated, without the need for complicated treatments such as purification and leaching.
  • the nano antibacterial agent of the present invention is evenly dispersed in the basic hand sanitizer, is suitable for addition to various hand sanitizers, and has wide adaptability.
  • the nano antibacterial agent of the present invention is more healthy and environmentally friendly than chemically synthesized antibacterial agents.
  • the preparation process of the nano antibacterial agent of the present invention is easy to control, the preparation method is environmentally friendly and pollution-free, has better practicability, has significant progress compared with the existing technology, and has a wide range of large-scale production value.
  • Figure 1 shows the antibacterial effect of the nano-plant antibacterial agent obtained in Example 1.
  • Figure 2 shows the antibacterial effect of no nano-plant antibacterial agent.
  • step (2) Prepare the coarsely pulverized materials in step (1) with sodium chloride, magnesium nitrate, and polylysine at a mass ratio of 100:5:3:1, and disperse them evenly, and then pass the JSM-Q-3 jet mill pulverizer After the compressed air is frozen, filtered and dried, it will form a supersonic airflow through the nozzles and be injected into the crushing chamber to fluidize the materials. The accelerated materials merge at the intersection of the jet airflows of several nozzles, causing violent collisions and frictions. , Shear to achieve ultra-fine pulverization of particles, using a classification speed of 1800 rpm, through high-speed classification, to obtain nano powder;
  • step (3) Disperse the nano powder obtained in step (2) with the sodium alginate solution at a mass ratio of 1:5, and the mass concentration of the sodium alginate solution is 2.5%; in an ultrasonic processor, the power is 2000W, the frequency is 20KHZ, and the treatment is 35min; Then use high-pressure spray drying, the pressure of the atomizing gun is controlled at 1.5MPa, the gun caliber is controlled at less than 0.5mm, and the drying temperature is controlled at 80°C. Through high-pressure spray drying, the sodium alginate is coated on the surface of the nano powder, thereby obtaining a nano plant antibacterial agent for hand sanitizer.
  • step (2) Prepare the coarsely pulverized materials in step (1) with sodium chloride, magnesium nitrate, and polylysine at a mass ratio of 100:8:5:1, and disperse them evenly, and then pass the JSM-Q-3 jet mill pulverizer After the compressed air is frozen, filtered and dried, it will form a supersonic airflow through the nozzles and be injected into the crushing chamber to fluidize the materials. The accelerated materials merge at the intersection of the jet airflows of several nozzles, causing violent collisions and frictions. , Shear to achieve ultra-fine pulverization of particles, using a classification speed of 2000 rpm, through high-speed classification, to obtain nano powder;
  • step (3) Disperse the nano powder obtained in step (2) with the sodium alginate solution at a mass ratio of 1:5, and the mass concentration of the sodium alginate solution is 2.5%; in an ultrasonic processor, the power is 2000W, the frequency is 20KHZ, and the treatment is performed for 50 minutes; Then use high-pressure spray drying, the pressure of the atomizing gun is controlled at 1.5MPa, the gun caliber is controlled at less than 0.5mm, and the drying temperature is controlled at 90°C. Through high-pressure spray drying, the sodium alginate is coated on the surface of the nano powder, thereby obtaining a nano plant antibacterial agent for hand sanitizer.
  • step (2) Prepare the coarsely pulverized materials in step (1) with sodium chloride, magnesium nitrate, and polylysine in a mass ratio of 100:10:5:2, and disperse them evenly, and pass the JSM-Q-3 jet mill pulverizer
  • the compressed air is frozen, filtered and dried, it will form a supersonic airflow through the nozzles and be injected into the crushing chamber to fluidize the materials.
  • the accelerated materials merge at the intersection of the jet airflows of several nozzles, causing violent collisions and frictions.
  • Shear to achieve ultra-fine pulverization of particles using a classification speed of 1800rpm-2000rpm, through high-speed classification, to obtain nano-powder;
  • step (3) Disperse the nano powder obtained in step (2) with the sodium alginate solution at a mass ratio of 1:5, and the mass concentration of the sodium alginate solution is 2.5%; in an ultrasonic processor, the power is 2000W, the frequency is 20KHZ, and the treatment is 60min; Then use high-pressure spray drying, the pressure of the atomizing gun is controlled at 2.0MPa, the gun caliber is controlled at less than 0.5mm, and the drying temperature is controlled at 90°C. Through high-pressure spray drying, the sodium alginate is coated on the surface of the nano powder, thereby obtaining a nano plant antibacterial agent for hand sanitizer.
  • Comparative Example 1 did not reach the nanometer level, the plant antibacterial particles were larger and the activity performance was slightly worse, so the antibacterial effect was reduced.
  • step (1) The coarsely pulverized material in step (1) is pulverized by a conventional vortex jet mill, and the classification speed is 600 rpm to obtain micron-sized powder;
  • step (3) Disperse the micron-sized powder obtained in step (2) with the sodium alginate solution at a mass ratio of 1:5, and the mass concentration of the sodium alginate solution is 2.5%; in the ultrasonic processor, the power is 2000W, the frequency is 20KHZ, and the treatment is 35min. ; Then use high-pressure spray drying, the pressure of the atomizing gun is controlled at 1.5MPa, the gun caliber is controlled at less than 0.5mm, and the drying temperature is controlled at 80°C. Through high-pressure spray drying, the sodium alginate is coated on the surface of the micron powder, thereby obtaining a plant antibacterial agent for hand sanitizer.
  • Litsea cubeba essential oil is commercially available as an antibacterial agent.
  • Comparative Example 2 is a directly refined essential oil. Although it exerts better activity, it is also easily inactivated in a complicated hand sanitizer environment, which reduces the antibacterial and antibacterial effect.
  • Example 1 The plant antibacterial agents obtained in Example 1, Comparative Example 1, and Comparative Example 2 were uniformly dispersed with the basic hand sanitizer at a mass ratio of 3:50 (the mass percentage formula of the basic hand sanitizer was 25% cocamidopropyl betaine, 10 % Sodium laureth sulfate, 1% sodium chloride, 2.5% citric acid, 0.5% octyl hydroxystearate, 2% EDTA-2Na, 1.5% hydroxypropyl cellulose, 0.5% benzyl alcohol, 1 % Polyquaternium-7, 56% deionized water) to obtain an antibacterial hand sanitizer.
  • the mass percentage formula of the basic hand sanitizer was 25% cocamidopropyl betaine, 10 % Sodium laureth sulfate, 1% sodium chloride, 2.5% citric acid, 0.5% octyl hydroxystearate, 2% EDTA-2Na, 1.5% hydroxypropyl cellulose, 0.5%
  • dissolution resistance (antibacterial) product antibacterial performance test method prepare Aspergillus niger into a suspension of 106cfu/mL; mix the antibacterial hand sanitizer and Aspergillus niger suspension at a volume ratio of 50:1 to obtain the result.
  • the mixed solution placed for 20 minutes, add PBS phosphate buffer (0.01mol/L), the volume of PBS phosphate buffer is the same as that of the mixed solution; then draw 50 ⁇ L and culture on LB/PDA medium at 37°C for 48h, and determine the colony count Make b.
  • Blank reference sample Mix the basic hand sanitizer (without nano plant antibacterial agent) and Aspergillus niger suspension at a volume ratio of 50:1 to obtain a mixed solution. After placing it for 20 minutes, add PBS phosphate buffer (0.01mol/L), The volume of PBS phosphate buffer added is the same as that of the mixed solution; then 50 ⁇ L of LB/PDA medium is cultured at 37°C for 48h, and the number of colonies is determined and counted as a.
  • Y (a-b)/a ⁇ %; where Y is the antibacterial efficiency; a is the number of colonies in the blank control sample; b is the number of colonies in the test sample.
  • the antibacterial rate is shown in Table 1.
  • Aspergillus niger is a pathogenic microorganism, that is, a microorganism that does not cause human or animal diseases under normal circumstances. However, due to the rapid growth, it is easy to diffuse through the air to pollute the environment, so pay attention to protection when using it in the laboratory.
  • the nano-plant antibacterial agent of the present invention has good activity through nano-treatment, and its antibacterial performance is excellent; Comparative Example 1 does not reach the nanometer level, the plant antibacterial grade particles are larger, and the activity performance is slightly poor, so it is antibacterial The effect is reduced; Comparative Example 2 is an extract of antibacterial plants. Although the activity is better after leaching, it is also easy to be inactivated in a complicated hand sanitizer environment after leaching, which reduces the antibacterial and antibacterial effect.
  • Example 1 Disperse the nanometer plant antibacterial agent, deionized water, and starch ether obtained in Example 1 at a mass ratio of 1:10:0.1, and smear it on a 10 ⁇ 10 cm glass plate as template A; Disperse with a mass ratio of 10:0.1, smear it on a 10 ⁇ 10cm glass plate as template B; then drop 100 ⁇ L of Pseudomonas aeruginosa suspension with a concentration of 10 6 cfu/mL on the glass plates of sample A and B Place it for 4 hours and observe through a high-power microscope:
  • Figure 1 shows sample A, which shows that there is no obvious breeding colony, indicating that the nano-plant antibacterial agent of the present invention has good antibacterial properties;
  • Figure 2 shows sample B, where the colony of Pseudomonas aeruginosa grows rapidly.

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Abstract

一种用于洗手液的纳米植物抗菌剂及制备方法。将收集的山苍子果实、花、叶混合冷冻干燥后粗粉碎；与氯化钠、硝酸镁、聚赖氨酸分散均匀，经气流磨，在氮气保护下微细化至纳米级别，得到纳米粉；将纳米粉加入海藻酸钠液，超声分散处理，然后高压喷雾干燥，得到一种用于洗手液的纳米植物抗菌剂。通过纳米化处理，综合利用植物抗菌剂，同时防止植物抗菌活性剂的活性成分失活，无需进行提纯、浸出等繁杂的处理。适合添加于各类洗手液，适应性较宽。相比于化学合成抗菌剂更为健康和环保。

Description

一种用于洗手液的纳米植物抗菌剂及制备方法 技术领域
本发明涉及日化领域，特别涉及一种用于洗手液的纳米植物抗菌剂及制备方法。
背景技术
抗菌洗手液作为一种日常用洗涤用品被越来越多的消费者所接受，应用于医院、学校等公共场合，起到了良好的即时性杀菌效果。最初，受生活条件和市场的制约，人们洗手通常用的是香皂、肥皂和洗衣粉等，虽然它们能达到一定的清洁洗效果，但对皮肤有刺激作用、抗菌效果差。
随着抗菌剂的发展，各类抗菌剂被用于洗手液。然而很多抗菌剂存在副作用。其中三氯卡班、三氯生是应用最广泛的抗菌剂，但有研究表明它们对动物的生殖和发育有危害，持续使用可能导致耐药性问题，低剂量的三氯生短期接触也可能导致过敏和皮炎。除此之外，对氯间二甲苯酚通过食管进入人体会造成胃肠黏膜细胞坏死、肠菌群失调等不良影响，而且对鱼群有害不环保。为了实现抗菌效果，抗菌剂的添加量逐步增大，同时副作用也越来越大。
因此，研发新型的、低毒天然的抗菌剂成为热点。如各类植物精油，萃取自天然植物，具有光谱的抗菌活性，安全且环保。常用的抗菌植物有苦参、广藿香、丁香、生姜等均具有抑菌性能。红花、紫草、艾纳香、刺天茄等药用植物制成的乙醇提取液，其成分复杂，抗菌作用广谱。
茶树精油是一种纯植物抗菌剂，具有广谱的抗菌活性，对许多细菌和真菌具有较好的杀灭或抑制作用。在国外，茶树油已被研发成多种类型的产品，如作为防腐剂、抗菌剂和芳香剂，主要应用于化妆品、药品、食品香料及美容行业等诸多领域。在中国茶树油也已用在高级护肤品、个人护理用品、植物型饲 料、家具清洁杀菌用品中，茶树油因其安全、环保、抗菌性强等特点，在国内外市场具有极大的需求量并具有广阔的开发利用价值。
山苍子中可提炼各种有价值的资源，其不但具有广谱的抗菌性，而且含有α-蒎烯具特殊松木香气；含有莰烯用于薰衣草油化妆品、香皂、除臭剂中及水果型食品香精中；含有的β-月桂烯具清谈香脂香气，可用于柑桔型的古龙香水和除臭剂中，可用于合成芳樟醇、香叶醇、香茅醇、紫罗兰酮等名贵香料。
目前，大部分是将具有抗菌功能的植物进行提纯，单纯获得抗菌剂的成分。然而植物抗菌是植物整体的体现，如抗菌植物含有生物碱、多糖、皂苷、有机酸等，单纯的提纯可能造成提取物失活。为了将抗菌植物用于抗菌，体现综合的抗菌效果。将植物抗菌纳米化是一个较佳的方向。
发明内容
为了综合利用植物抗菌剂，同时防止植物抗菌活性剂的活性成分失活，本发明提出一种用于洗手液的纳米植物抗菌剂，其通过纳米化赋予植物抗菌剂一定的活性，同时无需浸出提纯处理，综合利用了抗菌植物的抗菌功能。进一步，本发明提出该纳米植物抗菌剂的制备方法。
为了实现上述技术目的，采用如下的技术方案：
一种用于洗手液的纳米植物抗菌剂的制备方法，其关键的特征是：具体制备方法如下：
(1)将收集的山苍子果实、花、叶混合冷冻干燥后粗粉碎；
(2)将步骤(1)粗粉碎的物料与氯化钠、硝酸镁、聚赖氨酸分散均匀，经气流磨，在氮气保护下微细化至纳米级别，得到纳米粉；
(3)将步骤(2)得到的纳米粉加入海藻酸钠液，超声分散处理，然后高压喷雾干燥，得到一种用于洗手液的纳米植物抗菌剂。
优选的，步骤(1)选用山苍子果实、花、叶混合，目的是综合利用山苍子的抗菌性。进一步优选的，采集的山苍子果实、花、叶以质量比1∶0.1∶10混合。山苍子，性味辛、微苦，有香气，无毒。其具有良好的抗菌性，在饲料中常用作天然防霉剂。在山苍子中可提炼各种有价值的资源，如含有α-蒎烯：具特殊松木香气；含有莰烯用于薰衣草油化妆品、香皂、除臭剂中及水果型食品香精中；含有的β-月桂烯具清谈香脂香气，可用于柑桔型的古龙香水和除臭剂中，可用于合成芳樟醇、香叶醇、香茅醇、紫罗兰酮等名贵香料。在用于洗手液抗菌原料时，如果进行提炼会造成成本上升以及提炼物的挥发和失活。山苍子的果实、化、叶具有优异的抗菌功能，是一种综合各种活性作用的效果。为此本发明通过将山苍子的果实、化、叶纳米化，一方面保证了抗菌活性，另一方面看避免了提纯的繁杂工艺，用于吸收液还可以赋予洗手液清香效果。
优选的，步骤(1)所述冷冻干燥的处理环境的压力为40-50Pa，冷阱温度采用-40℃～-45℃，处理的时间为1-2小时。
优选的，步骤(1)所述粗粉碎是指采用常规粉碎机将干燥物粉碎至过50目筛。
优选的，步骤(2)所述粗粉碎的物料与氯化钠、硝酸镁、聚赖氨酸以质量比100∶5-10∶3-5∶1-3配制；氯化钠、硝酸镁为无机盐，一方面作为盐可以辅助后期研磨使粗粉碎物料研磨至纳米级，另一方面，氯化钠、硝酸镁可以渗透粗粉碎物，促进粗粉碎物细化；再者，氯化钠、硝酸镁是洗手液中的常用调节剂，使用后不会影响洗手液整体效果。使用聚赖氨酸不但可以渗透粗粉碎物促进细化，而且聚赖氨酸对革兰氏阳性菌、革兰氏阴性菌、酵母菌、霉菌均有良好的抑菌效果；对大肠杆菌、沙门氏菌抑菌效果非常好。
优选的，步骤(2)所述气流磨采用超音速气流磨，进一步优选JSM-Q-3型气流磨，压缩空气经过冷冻、过滤、干燥后，经喷嘴形成超音速气流射入粉碎室，使物料呈流态化，被加速的物料在数个喷嘴的喷射气流交汇点汇合，产生剧烈的碰撞、磨擦、剪切而达到颗粒的超细粉碎。粉碎后的物料被上升的气流输送至叶轮分级区内，在分级轮离心力和风机抽力的作用下，实现粗细粉的分离，粗粉根据自身的重力返回粉碎室继续粉碎，合格的细粉随气流进入旋风收集器，微细粉尘由袋式除尘器收集，净化的气体由引风机排出。采用的分级转速为1800rpm-2000rpm，通过高速分级，得到纳米级粉末。
优选的，步骤(3)所述纳米粉与海藻酸钠液以质量比1∶5分散，海藻酸钠液的质量浓度为2.5％；所述超声分散处理采用功率2000W、频率20KHZ，处理35-60min；不同于常规的搅拌分散，超声分散可以使团聚的纳米粒子分散开，从而使纳米粒子表面均接触海藻酸钠；以便在喷雾干燥时使海藻酸钠均匀包覆在纳米粒子的表面。
优选的，步骤(3)中采用高压喷雾干燥，雾化枪的压力控制在1.5-2.0MPa，枪口径控制在小于0.5mm，干燥温度控制在80-90℃。通过高压喷雾干燥，使海藻酸钠包覆在纳米粉的表面，从而得到一种用于洗手液的纳米植物抗菌剂，一方面防止纳米粒在存储时团聚，另一方面，其加入基础洗手液后容易分散开，并在洗手液中均匀悬浮，使用更为方便。
本发明还提供由上述方法制备得到的一种用于洗手液的纳米植物抗菌剂。通过将收集的山苍子果实、花、叶混合冷冻干燥后粗粉碎，与氯化钠、硝酸镁、聚赖氨酸经气流磨研磨至纳米粉；并在表面包覆海藻酸钠；其综合了山苍子的综合抗菌性，不需要进行提纯、浸出等处理，得到的纳米抗菌剂易于在洗手液 中分散，抗菌活性优异，对大肠杆菌、沙门氏菌、黑曲霉菌等具有两孩的抑制作用。
一种用于洗手液的纳米植物抗菌剂及制备方法，与现有技术相比具有如下
有益效果：
(1)本发明通过纳米化处理，综合利用植物抗菌剂，同时防止植物抗菌活性剂的活性成分失活，无需进行提纯、浸出等繁杂的处理。
(2)本发明纳米抗菌剂在基础洗手液分散均匀，适合添加于各类洗手液，适应性较宽。
(3)本发明纳米抗菌剂相比于化学合成抗菌剂更为健康和环保。
(4)本发明纳米抗菌剂制备工艺易控，制备方法是环保无污染，具有较佳的实用性，较现有的技术具有显著的进步，并具有广泛的规模化推广生产价值。
附图说明
图1是实施例1得到的纳米植物抗菌剂的抑菌效果。
图2是未加纳米植物抗菌剂的抑菌效果。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述。显然，所描述的实施例是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
(1)将采集的山苍子果实、花、叶以质量比1∶0.1∶10混合，在压力为40Pa，冷阱温度采用-40℃℃，冷冻干燥处理1小时，冷冻干燥后粗粉碎过50目筛；
(2)将步骤(1)粗粉碎的物料与氯化钠、硝酸镁、聚赖氨酸以质量比100∶5∶3∶1配制，分散均匀，经JSM-Q-3型气流磨粉碎机，压缩空气经过冷冻、过滤、干燥后，经喷嘴形成超音速气流射入粉碎室，使物料呈流态化，被加速的物料在数个喷嘴的喷射气流交汇点汇合，产生剧烈的碰撞、磨擦、剪切而达到颗粒的超细粉碎，采用的分级转速为1800rpm，通过高速分级，得到纳米粉；
(3)将步骤(2)得到的纳米粉与海藻酸钠液以质量比1∶5分散，海藻酸钠液的质量浓度为2.5％；在超声处理机中功率2000W、频率20KHZ，处理35min；然后采用高压喷雾干燥，雾化枪的压力控制在1.5MPa，枪口径控制在小于0.5mm，干燥温度控制在80℃。通过高压喷雾干燥，使海藻酸钠包覆在纳米粉的表面，从而得到一种用于洗手液的纳米植物抗菌剂。
实施例2
(1)将采集的山苍子果实、花、叶以质量比1∶0.1∶10混合，压力为40Pa，冷阱温度采用-40℃，冷冻干燥处理2小时，冷冻干燥后粗粉碎过50目筛；
(2)将步骤(1)粗粉碎的物料与氯化钠、硝酸镁、聚赖氨酸以质量比100∶8∶5∶1配制，分散均匀，经JSM-Q-3型气流磨粉碎机，压缩空气经过冷冻、过滤、干燥后，经喷嘴形成超音速气流射入粉碎室，使物料呈流态化，被加速的物料在数个喷嘴的喷射气流交汇点汇合，产生剧烈的碰撞、磨擦、剪切而达到颗粒的超细粉碎，采用的分级转速为2000rpm，通过高速分级，得到纳米粉；
(3)将步骤(2)得到的纳米粉与海藻酸钠液以质量比1∶5分散，海藻酸钠液的质量浓度为2.5％；在超声处理机中功率2000W、频率20KHZ，处理50min；然后采用高压喷雾干燥，雾化枪的压力控制在1.5MPa，枪口径控制在小于0.5mm，干燥温度控制在90℃。通过高压喷雾干燥，使海藻酸钠包覆在纳米粉的表面，从而得到一种用于洗手液的纳米植物抗菌剂。
实施例3
(1)将采集的山苍子果实、花、叶以质量比1∶0.1∶10混合，压力为40Pa，冷阱温度采用-40℃℃，冷冻干燥处理2小时，冷冻干燥后粗粉碎过50目筛；
(2)将步骤(1)粗粉碎的物料与氯化钠、硝酸镁、聚赖氨酸以质量比100∶10∶5∶2配制，分散均匀，经JSM-Q-3型气流磨粉碎机，压缩空气经过冷冻、过滤、干燥后，经喷嘴形成超音速气流射入粉碎室，使物料呈流态化，被加速的物料在数个喷嘴的喷射气流交汇点汇合，产生剧烈的碰撞、磨擦、剪切而达到颗粒的超细粉碎，采用的分级转速为1800rpm-2000rpm，通过高速分级，得到纳米粉；
(3)将步骤(2)得到的纳米粉与海藻酸钠液以质量比1∶5分散，海藻酸钠液的质量浓度为2.5％；在超声处理机中功率2000W、频率20KHZ，处理60min；然后采用高压喷雾干燥，雾化枪的压力控制在2.0MPa，枪口径控制在小于0.5mm，干燥温度控制在90℃。通过高压喷雾干燥，使海藻酸钠包覆在纳米粉的表面，从而得到一种用于洗手液的纳米植物抗菌剂。
对比例1没有达到纳米级，植物抗菌级颗粒较大，活性表现稍差，因此抑菌效果有所降低。
对比例1
(1)将采集的山苍子果实、花、叶以质量比1∶0.1∶10混合，在压力为40Pa，冷阱温度采用-40℃℃，冷冻干燥处理1小时，冷冻干燥后粗粉碎过50目筛；
(2)将步骤(1)粗粉碎的物料采用常规涡旋气流粉碎机粉碎，分级转速为600rpm，得到微米级粉；
(3)将步骤(2)得到的微米级粉与海藻酸钠液以质量比1∶5分散，海藻酸钠液的质量浓度为2.5％；在超声处理机中功率2000W、频率20KHZ，处理35min； 然后采用高压喷雾干燥，雾化枪的压力控制在1.5MPa，枪口径控制在小于0.5mm，干燥温度控制在80℃。通过高压喷雾干燥，使海藻酸钠包覆在微米粉的表面，从而得到一种用于洗手液的植物抗菌剂。
对比例2
市售山苍子精油作为抗菌剂。
对比例2为直接精炼的精油，尽管活性发挥较好，但也容易在复杂的洗手液环境中失活，使得抗菌抑菌效果降低。
抗菌效果的测试：
1、抑菌性能测试
将实施例1、对比例1、对比例2得到的植物抗菌剂分别与基础洗手液以质量比3∶50分散均匀(基础洗手液的质量百分比配方为25％椰油酰胺丙基甜菜碱、10％月桂醇聚醚硫酸酯钠、1％氯化钠、2.5％柠檬酸、0.5％辛基羟基硬脂酸酯、2％EDTA-2Na、1.5％羟丙基纤维素、0.5％苯甲醇、1％聚季铵盐-7、56％份去离子水)得到抗菌洗手液。
参考GB15979-2002溶出性抗(抑)菌产品抑菌性能试验方法，将黑曲霉菌配制为106cfu/mL的悬浮液；将抗菌洗手液与黑曲霉菌悬浮液以体积比50∶1混合均匀得到混合液，放置20min后加入PBS磷酸缓冲液(0.01mol/L)，PBS磷酸缓冲液加入体积与混合液相同；然后吸取50μL在LB/PDA培养基上在37℃培养48h，测定其菌落数计作b。
空白参比样：将基础洗手液(未加纳米植物抗菌剂)与黑曲霉菌悬浮液以体积比50∶1混合均匀得到混合液，放置20min后加入PBS磷酸缓冲液(0.01mol/L)，PBS磷酸缓冲液加入体积与混合液相同；然后吸取50μL在LB/PDA培养基上在37℃培养48h，测定其菌落数计作a。
计算抑菌效率：Y＝(a-b)/a×％；其中Y为抑菌效率；a为空白对照样菌落数；b为测试样菌落数。抑菌率如表1所示。
注意：黑曲霉是病原微生物，即在通常情况下不会引起人类或者动物疾病的微生物。但由于生长快速，极易通过空气扩散污染环境，在实验室使用时注意防护。
表1：
测试项目 实施例1 对比例1 对比例2
抑菌率(％) 92 64 51
通过上述测试，本发明纳米植物抗菌剂通过纳米化处理，具有良好的活性，其抑菌性能表现优异；对比例1没有达到纳米级，植物抗菌级颗粒较大，活性表现稍差，因此抑菌效果有所降低；对比例2为抗菌植物的浸出物，尽管浸出后活性发挥较好，但浸出后也容易在复杂的洗手液环境中失活，使得抗菌抑菌效果降低。
2、杀菌性能测试
将实施例1得到的纳米在植物抗菌剂与去离子水、淀粉醚以质量比1∶10∶0.1分散，涂抹在10×10cm的玻璃板上，作为样板A；将去离子水、淀粉醚以质量比10∶0.1分散，涂抹在10×10cm的玻璃板上，作为样板B；然后分将取100μL浓度为10 6cfu/mL的铜绿假单胞菌悬浮液滴在样板A、B玻璃板上放置4h，通过高倍显微镜观察：图1为样板A，没有明显的繁殖菌落，说明本发明纳米植物抗菌剂具有较好的抑菌性；图2为样板B，铜绿假单胞菌菌落急剧生长。

Claims (10)

  1. 一种用于洗手液的纳米植物抗菌剂的制备方法，其特征是：具体制备方法如下：
    (1)将收集的山苍子果实、花、叶混合冷冻干燥后粗粉碎；
    (2)将步骤(1)粗粉碎的物料与氯化钠、硝酸镁、聚赖氨酸分散均匀，经气流磨，在氮气保护下微细化至纳米级别，得到纳米粉；
    (3)将步骤(2)得到的纳米粉加入海藻酸钠液，超声分散处理，然后高压喷雾干燥，得到一种用于洗手液的纳米植物抗菌剂。
  2. 根据权利要求1所述一种用于洗手液的纳米植物抗菌剂的制备方法，其特征是：步骤(1)选用采集的山苍子果实、花、叶以质量比1∶0.1∶10混合。
  3. 根据权利要求1所述一种用于洗手液的纳米植物抗菌剂的制备方法，其特征是：步骤(1)所述冷冻干燥的处理环境的压力为40-50Pa，冷阱温度采用-40℃～-45℃，处理的时间为1-2小时。
  4. 根据权利要求1所述一种用于洗手液的纳米植物抗菌剂的制备方法，其特征是：步骤(1)所述粗粉碎是指采用常规粉碎机将干燥物粉碎至过50目筛。
  5. 根据权利要求1所述一种用于洗手液的纳米植物抗菌剂的制备方法，其特征是：步骤(2)所述粗粉碎的物料与氯化钠、硝酸镁、聚赖氨酸以质量比100∶5-10∶3-5∶1-3配制。
  6. 根据权利要求1所述一种用于洗手液的纳米植物抗菌剂的制备方法，其特征是：步骤(2)所述气流磨采用超音速气流磨，采用的分级转速为1800rpm-2000rpm。
  7. 根据权利要求1所述一种用于洗手液的纳米植物抗菌剂的制备方法，其特征是：步骤(3)所述纳米粉与海藻酸钠液以质量比1∶5分散，海藻酸钠液的 质量浓度为2.5％。
  8. 根据权利要求1所述一种用于洗手液的纳米植物抗菌剂的制备方法，其特征是：步骤(3)所述超声分散处理采用功率2000W、频率20KHZ，处理35-60min。
  9. 根据权利要求1所述一种用于洗手液的纳米植物抗菌剂的制备方法，其特征是：步骤(3)中采用高压喷雾干燥，雾化枪的压力控制在1.5-2.0MPa，枪口径控制在小于0.5mm，干燥温度控制在80-90℃。
  10. 由权利要求1-9任一项所述的方法制备得到的一种用于洗手液的纳米植物抗菌剂。
PCT/CN2020/113984 2020-01-06 2020-09-08 一种用于洗手液的纳米植物抗菌剂及制备方法 WO2021139194A1 (zh)

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