CN113317431A - 一种水包油型香芹酚纳米乳剂及其制备方法 - Google Patents
一种水包油型香芹酚纳米乳剂及其制备方法 Download PDFInfo
- Publication number
- CN113317431A CN113317431A CN202110652418.0A CN202110652418A CN113317431A CN 113317431 A CN113317431 A CN 113317431A CN 202110652418 A CN202110652418 A CN 202110652418A CN 113317431 A CN113317431 A CN 113317431A
- Authority
- CN
- China
- Prior art keywords
- carvacrol
- oil
- water
- nanoemulsion
- polysorbate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- RECUKUPTGUEGMW-UHFFFAOYSA-N carvacrol Chemical compound CC(C)C1=CC=C(C)C(O)=C1 RECUKUPTGUEGMW-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 235000007746 carvacrol Nutrition 0.000 title claims abstract description 126
- HHTWOMMSBMNRKP-UHFFFAOYSA-N carvacrol Natural products CC(=C)C1=CC=C(C)C(O)=C1 HHTWOMMSBMNRKP-UHFFFAOYSA-N 0.000 title claims abstract description 126
- WYXXLXHHWYNKJF-UHFFFAOYSA-N isocarvacrol Natural products CC(C)C1=CC=C(O)C(C)=C1 WYXXLXHHWYNKJF-UHFFFAOYSA-N 0.000 title claims abstract description 126
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 239000007908 nanoemulsion Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229920000136 polysorbate Polymers 0.000 claims abstract description 27
- 239000004094 surface-active agent Substances 0.000 claims abstract description 22
- 229950008882 polysorbate Drugs 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 239000003755 preservative agent Substances 0.000 claims abstract description 14
- -1 polyoxyethylene Polymers 0.000 claims abstract description 13
- 230000002335 preservative effect Effects 0.000 claims abstract description 13
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 11
- 238000010008 shearing Methods 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- 239000004359 castor oil Substances 0.000 claims description 15
- 235000019438 castor oil Nutrition 0.000 claims description 15
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 15
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 15
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 15
- 239000000839 emulsion Substances 0.000 claims description 10
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 8
- 235000010234 sodium benzoate Nutrition 0.000 claims description 8
- 239000004299 sodium benzoate Substances 0.000 claims description 8
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 claims description 5
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 5
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 5
- 229920000053 polysorbate 80 Polymers 0.000 claims description 5
- 239000004302 potassium sorbate Substances 0.000 claims description 5
- 235000010241 potassium sorbate Nutrition 0.000 claims description 5
- 229940069338 potassium sorbate Drugs 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 239000003973 paint Substances 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 22
- 230000008901 benefit Effects 0.000 abstract description 7
- 230000005923 long-lasting effect Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 21
- 239000003814 drug Substances 0.000 description 16
- 229940079593 drug Drugs 0.000 description 16
- 239000000341 volatile oil Substances 0.000 description 11
- 239000007788 liquid Substances 0.000 description 10
- 230000008569 process Effects 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- 241000196324 Embryophyta Species 0.000 description 7
- 235000013305 food Nutrition 0.000 description 7
- 230000001580 bacterial effect Effects 0.000 description 6
- 241000191967 Staphylococcus aureus Species 0.000 description 5
- 230000005764 inhibitory process Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002502 liposome Substances 0.000 description 4
- 239000002609 medium Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 241000192125 Firmicutes Species 0.000 description 3
- 239000003995 emulsifying agent Substances 0.000 description 3
- 239000001963 growth medium Substances 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 2
- 229920000858 Cyclodextrin Polymers 0.000 description 2
- 239000001116 FEMA 4028 Substances 0.000 description 2
- 229920002774 Maltodextrin Polymers 0.000 description 2
- 239000005913 Maltodextrin Substances 0.000 description 2
- 244000061176 Nicotiana tabacum Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 description 2
- 235000011175 beta-cyclodextrine Nutrition 0.000 description 2
- 229960004853 betadex Drugs 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 229940035034 maltodextrin Drugs 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 239000003094 microcapsule Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 239000002504 physiological saline solution Substances 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 206010040872 skin infection Diseases 0.000 description 2
- 239000002047 solid lipid nanoparticle Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 231100000699 Bacterial toxin Toxicity 0.000 description 1
- 240000005250 Chrysanthemum indicum Species 0.000 description 1
- 235000018959 Chrysanthemum indicum Nutrition 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 239000012880 LB liquid culture medium Substances 0.000 description 1
- 235000013628 Lantana involucrata Nutrition 0.000 description 1
- 235000006677 Monarda citriodora ssp. austromontana Nutrition 0.000 description 1
- 240000007673 Origanum vulgare Species 0.000 description 1
- 241000233647 Phytophthora nicotianae var. parasitica Species 0.000 description 1
- 108010039918 Polylysine Proteins 0.000 description 1
- 241000235342 Saccharomycetes Species 0.000 description 1
- 241000191940 Staphylococcus Species 0.000 description 1
- 240000002657 Thymus vulgaris Species 0.000 description 1
- 235000007303 Thymus vulgaris Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000000688 bacterial toxin Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000007957 coemulsifier Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006353 environmental stress Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000009920 food preservation Methods 0.000 description 1
- 235000019249 food preservative Nutrition 0.000 description 1
- 239000005452 food preservative Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000013022 formulation composition Substances 0.000 description 1
- 229940075507 glyceryl monostearate Drugs 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 description 1
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229960004063 propylene glycol Drugs 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000001585 thymus vulgaris Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3481—Organic compounds containing oxygen
- A23L3/349—Organic compounds containing oxygen with singly-bound oxygen
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3481—Organic compounds containing oxygen
- A23L3/3508—Organic compounds containing oxygen containing carboxyl groups
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Medicinal Preparation (AREA)
Abstract
一种水包油型香芹酚纳米乳剂及其制备方法,属于纳米技术领域。水包油型香芹酚纳米乳剂的配方组成如下:香芹酚2.5~10%、聚山梨酯4~10%、聚氧乙烯型表面活性剂2%~5%、防腐剂0.05~0.2%和去离子水。本发明利用高速分散均质机制备水包油型香芹酚纳米乳剂,制备的水包油型香芹酚纳米乳剂粒径在50~100nm,具有分散性好,稳定性强,持效期长,生物安全性高,抗菌效果好,该制备方法简单、易操作,具有较高的经济效益。
Description
技术领域
本发明属于纳米技术领域,涉及一种水包油型香芹酚纳米乳剂的制备方法。
背景技术
植物精油是植物所特有的一种次生代谢产物,主要是含香味的挥发性有机化合物。植物精油的提取方法多样,主要有蒸馏、压缩、脂吸、压榨等方式。相对于植物中的其他物质,植物精油的安全性较高,因此广泛的应用于农业、食品、日化产品及制药工业中。例如在欧盟委员会(CEC)和美国食品药品监督管理局(FDA)认可的食品调味品材料清单中就包含着各种各样的精油成分。除上述用途外,部分精油还具有很强的抗菌活性,可以作为天然防腐剂来抑制微生物的生长,减缓食物变质的速度,延长食品的有效期。随着人们对“回归自然”追求的不断兴起,市场上对天然防腐剂的需求也不断增加,相关植物精油的市场份额也在不断扩大。
香芹酚是植物百里香和牛至挥发油的主要成分,呈淡黄色透明油状液体,有浓郁的香味,具有较强的挥发性。作为一种被食品行业广泛接受的抗菌剂和抗氧化剂,香芹酚不仅具有分子小、毒性低、极性低的特点,而且有着很强的抗菌和抗氧化作用。同时香芹酚的抗菌谱也较广,不仅对葡萄球菌属、大肠杆菌属等细菌均存在一定的抑制作用,而且对真菌、酵母菌等也有着很好的抑制性,具有较高的开发价值。
但香芹酚作为食品保鲜剂的应用受到以下因素的限制:(一)香芹酚在水相中的溶解度较低;(二)因其强烈的风味和香气而对食品的感官特性产生重大影响;(三)它们的抗菌活性因与复杂食品基质的物理或化学相互作用而降低。因此,香芹酚通常不是以原料的形式使用,而是制备成一定的剂型来发挥其相应的作用。
纳米乳剂是一种基于乳剂的递送系统,因其高负载能力、高效保护而特别适用于香芹酚。纳米乳剂具有许多其它制剂无可比拟的优点:(一)属于热力学稳定系统,经热压灭菌或离心也不能使之分层;(二)工艺简单,制备过程不需特殊设备,易操作;(三)可以提高药物的溶解度,形成对药物的保护作用并提高药物的生物利用度,因此纳米乳剂作为一种新型药物载体受到广泛的关注。将香芹酚制备成纳米乳剂可以缓解香芹酚的强烈气味,提高其在使用过程中的稳定性,更好地发挥出香芹酚的抗菌优势,使其在食品保鲜、卫生消杀等方面发挥更好的作用。
通过文献检索发现目前有关香芹酚制剂的专利主要分为以下方面:(一)将香芹酚制备成复方制剂。如中国专利CN110150332B“一种含有香芹酚的组合物、杀菌剂及其制备方法和应用”中将香芹酚和野菊精油复配成制剂来防治烟草青枯病和烟草黑胫病,这种方法难以说明香芹酚的作用;(二)将香芹酚制备成固体制剂。如中国专利CN109122684B“具有抑菌活性的香芹酚固体脂质纳米粒分散液及其制备方法和应用”中制备了香芹酚的固体脂质纳米粒,其配方组成中含有较多种类的表面活性剂,且制备过程中需要将香芹酚、单硬脂酸甘油酯和1,2-丙二醇酯熔融后混合,工艺较为复杂;中国专利CN108746663B“一种香芹酚微乳体系制备纳米银的方法”中抗菌能力主要是依靠稳定在香芹酚微乳液表面的纳米银来实现,虽然抗菌能力有所增强,但银离子会带来重金属污染等一系列环境问题;中国专利CN110742069A“一种香芹酚微胶囊及其制备方法”是以淀粉乳或麦芽糊精溶液为原料,加CGT酶液化制成淀粉或麦芽糊精糊化液,均质后采用喷雾干燥技术制备微胶囊,工艺复杂且质控困难;中国专利CN111466507A“一种香芹酚/β-环糊精蛋白脂质体及其制备方法和抗菌用途”中利用β-环糊精包埋香芹酚,再用脂质体包埋该包合物,最后通过ε-聚赖氨酸修饰该脂质体提升其抑菌活性,制备工艺复杂,质控困难且难以工业化;(三)将香芹酚制备成乳剂。如中国专利CN107197860A“含香芹酚的纳米乳及其制备方法”中香芹酚含量仅为0.5%~1%,使用过程中有着诸多的不便。
发明内容
本发明目的是提供一种水包油型香芹酚纳米乳剂。
本发明水包油型香芹酚纳米乳剂由按质量比由2.5~10%的香芹酚、4~10%的聚山梨酯、2%~5%的聚氧乙烯型表面活性剂、0.05~0.2%的防腐剂以及去离子水组成。
水包油型香芹酚纳米乳剂分散性好,稳定性强,生物安全性高,抗菌效果好。该水包油型香芹酚纳米乳剂,既降低了香芹酚的用量,又克服了香芹酚在使用过程中的易挥发、不稳定等缺点。
本发明的水包油型香芹酚纳米乳剂具有以下显著优点:
1、稳定性好,纳米乳剂属于热力学稳定体系,可长期放置不发生相分离;
2、不仅表现出与高浓度精油相似的抗菌效果,而且可以提高精油在使用过程中的稳定性,达到控释缓释效果;
3、选用水为主溶剂,减少了有机溶剂的使用,制备过程不造成污染,更加安全环保,在运输贮存过程中更加稳定;
4、将香芹酚制备成水包油型纳米乳剂,解决了香芹酚不溶于水的问题,减少了香芹酚的无用挥发,延长了香芹酚的持效期,提高了香芹酚的生物利用度。
进一步地,通过考察纳米乳剂的外观、平均粒径、Zeta电位以及抗菌效果,对水包油型香芹酚纳米乳剂的配方进行优化,从而得到更加稳定、更适合储存的水包油型香芹酚纳米乳剂配方。水包油型香芹酚纳米乳剂中各组分的质量比如下:香芹酚5%、聚山梨酯5%、聚氧乙烯型表面活性剂5%、防腐剂0.05%。
本发明所述的香芹酚为99.0%的香芹酚,水包油型香芹酚纳米乳剂的抗菌功效与香芹酚的纯度相关。纯度更高的香芹酚对金黄色葡萄球菌等革兰氏阳性菌的抑制作用更强。
本发明所述的聚山梨酯选自吐温40、吐温60、吐温80中的一种。吐温系列是一类亲水性非离子型表面活性剂,具有优良的乳化、分散、润湿等性能,无臭、无味,对人体安全无毒,是理想的乳化剂。
本发明所述的聚氧乙烯型表面活性剂选自蓖麻油聚氧乙烯醚40、蓖麻油聚氧乙烯醚60、蓖麻油聚氧乙烯醚80中的一种。这类表面活性剂稳定性较高,具有优异的表面性能,生物降解性和水溶性均较好,并且有良好的乳化、增溶性能,混合复配性能强。与吐温系列同用,发挥助乳化剂作用,可调节乳化剂的HLB值,形成更小的乳滴。
本发明所述的防腐剂选自山梨酸钾、苯甲酸钠中的一种。以水为溶剂的液体制剂,易被微生物污染而发霉变质,抗菌药液体制剂也能生长微生物,因为抗菌药物都有一定的抗菌谱。被微生物污染的液体制剂不仅发生理化性质的变化,影响制剂质量,而且会产生细菌毒素有害于人体,因此选择加入适量的防腐剂,防止污染。
本发明所述的水包油型香芹酚纳米乳剂的粒径为50~100 nm。极小的粒径使得香芹酚具有较大的比表面积,可降低香芹酚的用量,增加其溶解度和溶出度,提高其生物利用度。
本发明所述的水包油型香芹酚纳米乳剂为外用制剂,用于治疗各种细菌性皮肤感染,主用于革兰氏阳性球菌引起的皮肤感染。
本发明的另一目的为水包油型香芹酚纳米乳剂的制备方法,包括以下步骤:
将香芹酚、聚山梨酯和聚氧乙烯型表面活性剂混合搅拌,继续加去离子水,用高速分散均质机剪切处理后,加入防腐剂,得到水包油型香芹酚纳米乳剂;所述香芹酚、聚山梨酯、聚氧乙烯型表面活性剂和防腐剂的投料质量分别占总投料量的2.5~10%、4~10%、2%~5%和0.05~0.2%。
本工艺制备方法简单、易操作,具有较高的经济效益,产品具有分散性好,稳定性强,持效期长,生物安全性高,抗菌效果好的特点。
另外,本发明所述搅拌的设备是磁力搅拌器,搅拌的时间为15min,搅拌的转速为600 r/min。磁力搅拌器采用直流电机,噪音小,调速平稳,数显直观准确,适合搅拌低粘稠度的液体或固液混合物。搅拌时间和转速经过前期预实验选择。
所述剪切的时间为3~7 min,剪切的转速为8000~15000 r/min。选择适宜的剪切时间和转速能够获得粒径更小、分散更均匀、稳定性更高的纳米乳剂。
附图说明
图1是水包油型香芹酚纳米乳剂的平均粒径。
图2是水包油型香芹酚纳米乳剂的Zeta电位图。
图3是水包油型香芹酚纳米乳剂的热储、冷储、常温储存外观图。
图4是水包油型香芹酚纳米乳剂对于金黄色葡萄球菌的抑菌圈直径图。
具体实施方式
为了使本发明的目的和技术方案更加清楚,通过以下具体实施例予以详细的说明,但不限于这些具体的例子。
一、样品制备:
实施例1:
1)按量称取500 g香芹酚原药,400 g聚山梨酯吐温40,200 g蓖麻油聚氧乙烯醚40,混合,置于磁力搅拌器上600r/min搅拌15min,制得表面活性剂与香芹酚的混合物。
2)将称取好的8895 g去离子水加入以上混合物中,利用高速分散均质机以10000r/min剪切7 min;
3)剪切完成后,加入5 g的苯甲酸钠,混合均匀,即得水包油型香芹酚纳米乳剂。
实施例2:
1)按量称取500 g香芹酚原药,500 g聚山梨酯吐温60,500 g蓖麻油聚氧乙烯醚80,混合,置于磁力搅拌器上600r/min搅拌15min,制得表面活性剂与香芹酚的混合物;
2)将称取好的8495 g去离子水加入以上混合物中,利用高速分散均质机以12000r/min剪切5min;
3)剪切完成后,加入5 g的苯甲酸钠,混合均匀,即得水包油型香芹酚纳米乳剂。
实施例3:
1)按量称取500 g香芹酚原药,500 g聚山梨酯吐温80,500 g蓖麻油聚氧乙烯醚60,混合,置于磁力搅拌器上600r/min搅拌15min,制得表面活性剂与香芹酚的混合物;
2)将称取好的8495 g去离子水加入以上混合物中,利用高速分散均质机以12000r/min剪切5min;
3)剪切完成后,加入5 g的山梨酸钾,混合均匀,即得水包油型香芹酚纳米乳剂。
实施例4:
1)按量称取750 g香芹酚原药,400 g聚山梨酯吐温40,200 g蓖麻油聚氧乙烯醚40,混合,置于磁力搅拌器上600r/min搅拌15min,制得表面活性剂与香芹酚的混合物;
2)将称取好的8645 g余量的去离子水加入以上混合物中,利用高速分散均质机以10000 r/min剪切7min;
3)剪切完成后,加入5 g的苯甲酸钠,混合均匀,即得水包油型香芹酚纳米乳剂。
实施例5:
1)按量称取750 g香芹酚原药,500 g聚山梨酯吐温60,500 g蓖麻油聚氧乙烯醚80,混合,置于磁力搅拌器上600r/min搅拌15min,制得表面活性剂与香芹酚的混合物;
2)将称取好的8245 g去离子水加入以上混合物中,利用高速分散均质机以12000r/min剪切5min;
3)剪切完成后,加入5 g的苯甲酸钠,混合均匀,即得水包油型香芹酚纳米乳剂。
实施例6:
1)按量称取750 g香芹酚原药,500 g聚山梨酯吐温80,500 g蓖麻油聚氧乙烯醚60,混合,置于磁力搅拌器上600r/min搅拌15min,制得表面活性剂与香芹酚的混合物;
2)将称取好的8245 g去离子水加入以上混合物中,利用高速分散均质机以12000r/min剪切5min;
剪切完成后,加入5 g的山梨酸钾,混合均匀,即得水包油型香芹酚纳米乳剂。
实施例7:
1)按量称取1000 g香芹酚原药,400 g聚山梨酯吐温40,200 g蓖麻油聚氧乙烯醚40,混合,置于磁力搅拌器上600r/min搅拌15min,制得表面活性剂与香芹酚的混合物;
2)将称取好的8395 g余量的去离子水加入以上混合物中,利用高速分散均质机以10000 r/min剪切7min;
3)剪切完成后,加入5 g的苯甲酸钠,混合均匀,即得水包油型香芹酚纳米乳剂。
实施例8:
1)按量称取1000 g香芹酚原药,500 g聚山梨酯吐温60,500 g蓖麻油聚氧乙烯醚80,混合,置于磁力搅拌器上600r/min搅拌15min,制得表面活性剂与香芹酚的混合物;
2)将称取好的7995 g去离子水加入以上混合物中,利用高速分散均质机以12000r/min剪切5min;
3)剪切完成后,加入5 g的苯甲酸钠,混合均匀,即得水包油型香芹酚纳米乳剂。
实施例9:
1)按量称取1000 g香芹酚原药,500 g聚山梨酯吐温80,500 g蓖麻油聚氧乙烯醚60,混合,置于磁力搅拌器上600r/min搅拌15min,制得表面活性剂与香芹酚的混合物;
2)将称取好的7995 g余量的去离子水加入以上混合物中,利用高速分散均质机以12000 r/min剪切5min;
3)剪切完成后,加入5 g的山梨酸钾,混合均匀,即得水包油型香芹酚纳米乳剂。
二、性能测试:
对水包油型香芹酚纳米乳剂稳定性进行考察,主要研究抗菌乳剂在商业应用中可能遇到的一些环境应力因素对其稳定性的影响。
使用马尔文粒度仪在25℃条件下测定以上各例制备的纳米乳剂的平均粒径、Zeta电位。为了避免多重散射效应,在测量前,将各样品用去离子水稀释200倍。
在乳剂体系中,平均粒径是表明其物理稳定性的关键特征,描述了分散的油滴的平均尺寸。
从图1中可以看出,水包油型香芹酚纳米乳剂的粒径均低于100nm。
Zeta电位(ζ电位)是测量乳剂液滴表面净电荷的最常用参数,也是乳剂稳定性的指标。水包油型香芹酚纳米乳剂的ζ-电位值的降低有利于乳剂的长期稳定。
从图2中可以看出,水包油型香芹酚纳米乳剂的的ζ电位随着香芹酚含油量的增加而显著降低。
样品分别在低温(4±2℃)、高温(54±2℃)和常温(25±2℃)下储存,观察水包油型香芹酚纳米乳剂的外观,在高温下储存14天、在低温与常温下储存30天,从图3中可以看出,各水包油型香芹酚纳米乳剂均不出现相分离现象,外观均匀一致,无变化。图3中N1即实施例1对应的水包油型香芹酚纳米乳剂,其他类同。
三、应用:
采用纸片扩散法考察水包油型香芹酚纳米乳剂对革兰氏阳性菌(金黄色葡萄球菌)的抑制效果。
取出金黄色葡萄球菌(ATCC6538)的冻存菌株,在无菌条件下,37℃水浴解冻,移至新的15mL离心管中,加入5mL LB液体培养基,37℃,180rpm,振荡培养12 h。12 h后,再把菌种接种于LB固体培养基平板上,37℃培养,每次重复这个过程,直到有单个的菌落长出来,把单个的菌落再接种到LB液体培养基中,在37℃下,180rpm,振荡培养12 h。
将活化好的菌悬液离心后得到的菌泥用85%生理盐水洗涤两次(洗去死菌和LB培养基),用生理盐水将其稀释至OD600=0.5后,吸取100μL菌液至LB固体培养基平板表面,用涂布器涂布均匀,并在培养基中心垂直放置7mm空白药敏纸片,轻轻加压,使其与培养基接触无空隙,滴加20μL的水包油型香芹酚纳米乳剂,在37℃培养12h,观察并测量抑菌圈直径。将100 μL菌液均匀涂布的LB固体培养基作为对照。
采用纸片扩散法对革兰氏阳性菌(金黄色葡萄球菌)进行抗菌效果评估,如图4所示,结果显示以上实施例都能有效抑菌,并且纳米乳剂中香芹酚的含量越高,其抑菌圈越大。
Claims (10)
1.一种水包油型香芹酚纳米乳剂,其特征在于:按质量比由2.5~10%的香芹酚、4~10%的聚山梨酯、2%~5%的聚氧乙烯型表面活性剂、0.05~0.2%的防腐剂以及去离子水组成。
2.根据权利要求1所述的水包油型香芹酚纳米乳剂,其特征在于:该乳剂中各组分的质量比如下:香芹酚5%、聚山梨酯5%、聚氧乙烯型表面活性剂5%、防腐剂0.05%。
3.根据权利要求1或2所述的水包油型香芹酚纳米乳剂,其特征在于:所述香芹酚的纯度为99.0%。
4.根据权利要求1或2所述的水包油型香芹酚纳米乳剂,其特征在于:所述的聚山梨酯为吐温40、吐温60、吐温80中的一种。
5.根据权利要求1或2所述的水包油型香芹酚纳米乳剂,其特征在于:所述的聚氧乙烯型表面活性剂为蓖麻油聚氧乙烯醚40、蓖麻油聚氧乙烯醚60、蓖麻油聚氧乙烯醚80中的一种。
6.根据权利要求1或2所述的水包油型香芹酚纳米乳剂,其特征在于:所述防腐剂为山梨酸钾、苯甲酸钠中的一种。
7.根据权利要求1或2所述的水包油型香芹酚纳米乳剂,其特征在于:所述香芹酚纳米乳剂的粒径为50~100 nm;所述香芹酚纳米乳剂为外用制剂。
8.如权利要求1所述的水包油型香芹酚纳米乳剂的制备方法,其特征在于:取香芹酚、聚山梨酯、聚氧乙烯型表面活性剂混合搅拌,继续加去离子水,用高速分散均质机剪切处理后,加入防腐剂,得到水包油型香芹酚纳米乳剂;所述香芹酚、聚山梨酯、聚氧乙烯型表面活性剂和防腐剂的投料质量分别占总投料量的2.5~10%、4~10%、2%~5%和0.05~0.2%。
9.根据权利要求8所述的制备方法,其特征在于:所述搅拌为磁力搅拌,搅拌的时间为15 min,搅拌的转速为600 r/min。
10.根据权利要求8所述的制备方法,其特征在于:所述剪切的时间为3~7 min,剪切的转速为8000~15000 r/min。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110652418.0A CN113317431A (zh) | 2021-06-11 | 2021-06-11 | 一种水包油型香芹酚纳米乳剂及其制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110652418.0A CN113317431A (zh) | 2021-06-11 | 2021-06-11 | 一种水包油型香芹酚纳米乳剂及其制备方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN113317431A true CN113317431A (zh) | 2021-08-31 |
Family
ID=77420563
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110652418.0A Pending CN113317431A (zh) | 2021-06-11 | 2021-06-11 | 一种水包油型香芹酚纳米乳剂及其制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113317431A (zh) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114259004A (zh) * | 2021-12-16 | 2022-04-01 | 上海交通大学 | 一种抗菌透明微乳液水剂及其制备与应用 |
CN114288244A (zh) * | 2021-12-09 | 2022-04-08 | 扬州大学 | 一种花椒油纳米乳剂及其制备方法和应用 |
CN117379373A (zh) * | 2023-09-28 | 2024-01-12 | 石家庄正大鸿福牧业有限公司 | 一种均相稳定的大蒜油和香芹酚的复方水乳液及其制备方法 |
CN117379373B (zh) * | 2023-09-28 | 2024-06-11 | 石家庄正大鸿福牧业有限公司 | 一种均相稳定的大蒜油和香芹酚的复方水乳液及其制备方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102406721A (zh) * | 2011-11-24 | 2012-04-11 | 西北农林科技大学 | 一种水包油型复方苹果籽油纳米乳组合物及其制备方法 |
CN106343163A (zh) * | 2016-08-29 | 2017-01-25 | 厦门惠盈动物科技有限公司 | 一种乳化纳米牛至香酚和大蒜精添加剂及其制备方法 |
CN108143717A (zh) * | 2018-02-12 | 2018-06-12 | 周基清 | 一种薄荷脑纳米乳剂及其制备方法 |
CN112870162A (zh) * | 2021-04-14 | 2021-06-01 | 扬州大学 | 一种薄荷油纳米乳液的制备方法 |
-
2021
- 2021-06-11 CN CN202110652418.0A patent/CN113317431A/zh active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102406721A (zh) * | 2011-11-24 | 2012-04-11 | 西北农林科技大学 | 一种水包油型复方苹果籽油纳米乳组合物及其制备方法 |
CN106343163A (zh) * | 2016-08-29 | 2017-01-25 | 厦门惠盈动物科技有限公司 | 一种乳化纳米牛至香酚和大蒜精添加剂及其制备方法 |
CN108143717A (zh) * | 2018-02-12 | 2018-06-12 | 周基清 | 一种薄荷脑纳米乳剂及其制备方法 |
CN112870162A (zh) * | 2021-04-14 | 2021-06-01 | 扬州大学 | 一种薄荷油纳米乳液的制备方法 |
Non-Patent Citations (1)
Title |
---|
雷凯: "香芹酚纳米乳-羧甲基壳聚糖复合食品包装膜的制备与性能研究", 《硕士电子期刊》, no. 08, 15 August 2019 (2019-08-15), pages 1 - 58 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114288244A (zh) * | 2021-12-09 | 2022-04-08 | 扬州大学 | 一种花椒油纳米乳剂及其制备方法和应用 |
CN114259004A (zh) * | 2021-12-16 | 2022-04-01 | 上海交通大学 | 一种抗菌透明微乳液水剂及其制备与应用 |
CN114259004B (zh) * | 2021-12-16 | 2023-12-22 | 上海交通大学 | 一种抗菌透明微乳液水剂及其制备与应用 |
CN117379373A (zh) * | 2023-09-28 | 2024-01-12 | 石家庄正大鸿福牧业有限公司 | 一种均相稳定的大蒜油和香芹酚的复方水乳液及其制备方法 |
CN117379373B (zh) * | 2023-09-28 | 2024-06-11 | 石家庄正大鸿福牧业有限公司 | 一种均相稳定的大蒜油和香芹酚的复方水乳液及其制备方法 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Liew et al. | Physical, morphological and antibacterial properties of lime essential oil nanoemulsions prepared via spontaneous emulsification method | |
Talón et al. | Encapsulation of eugenol by spray-drying using whey protein isolate or lecithin: Release kinetics, antioxidant and antimicrobial properties | |
Guerra-Rosas et al. | Antimicrobial activity of nanoemulsions containing essential oils and high methoxyl pectin during long-term storage | |
Zahi et al. | Enhancing the antimicrobial activity of d-limonene nanoemulsion with the inclusion of ε-polylysine | |
Nirmal et al. | Formulation, characterisation and antibacterial activity of lemon myrtle and anise myrtle essential oil in water nanoemulsion | |
Prakash et al. | Nanoencapsulation: An efficient technology to boost the antimicrobial potential of plant essential oils in food system | |
Zahi et al. | Improving the antimicrobial activity of D-limonene using a novel organogel-based nanoemulsion | |
Jo et al. | Physical and antimicrobial properties of trans-cinnamaldehyde nanoemulsions in water melon juice | |
Liao et al. | Nanoencapsulation of essential oils as natural food antimicrobial agents: An overview | |
Li et al. | Thymol nanoemulsions formed via spontaneous emulsification: Physical and antimicrobial properties | |
Jiménez et al. | Elaboration and characterization of O/W cinnamon (Cinnamomum zeylanicum) and black pepper (Piper nigrum) emulsions | |
Cui et al. | Inhibition of Escherichia coli O157: H7 biofilm on vegetable surface by solid liposomes of clove oil | |
Letsididi et al. | Antimicrobial and antibiofilm effects of trans-cinnamic acid nanoemulsion and its potential application on lettuce | |
Roy et al. | Formulation and characterization of betel leaf (Piper betle L.) essential oil based nanoemulsion and its in vitro antibacterial efficacy against selected food pathogens | |
CN109601612A (zh) | 一种负载肉桂精油的皮克林乳液及其制备方法 | |
CN113317431A (zh) | 一种水包油型香芹酚纳米乳剂及其制备方法 | |
WO2019047004A1 (zh) | 一种天然替代的植物精油防腐剂及在化妆品中的应用 | |
Marcet et al. | Production and characterisation of biodegradable PLA nanoparticles loaded with thymol to improve its antimicrobial effect | |
Ren et al. | Effects of hydrosoluble calcium ions and organic acids on citrus oil emulsions stabilized with citrus pectin | |
Enayatifard et al. | Anti-microbial potential of nano-emulsion form of essential oil obtained from aerial parts of Origanum vulgare L. as food additive | |
Wang et al. | Nano-emulsification improves physical properties and bioactivities of litsea cubeba essential oil | |
Lima et al. | Cineole-containing nanoemulsion: Development, stability, and antibacterial activity | |
Polychniatou et al. | Evaluation of surface-active and antioxidant effect of olive oil endogenous compounds on the stabilization of water-in-olive-oil nanoemulsions | |
Lins et al. | On the formation, physicochemical properties and antibacterial activity of colloidal systems containing tea tree (Melaleuca alternifolia) oil | |
CN112870162A (zh) | 一种薄荷油纳米乳液的制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WD01 | Invention patent application deemed withdrawn after publication | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210831 |