CN114259004B - Antibacterial transparent microemulsion aqua and preparation and application thereof - Google Patents
Antibacterial transparent microemulsion aqua and preparation and application thereof Download PDFInfo
- Publication number
- CN114259004B CN114259004B CN202111545491.4A CN202111545491A CN114259004B CN 114259004 B CN114259004 B CN 114259004B CN 202111545491 A CN202111545491 A CN 202111545491A CN 114259004 B CN114259004 B CN 114259004B
- Authority
- CN
- China
- Prior art keywords
- microemulsion
- annatto
- water
- antibacterial
- essential oil
- 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.)
- Active
Links
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 89
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 235000012665 annatto Nutrition 0.000 claims abstract description 58
- 244000017106 Bixa orellana Species 0.000 claims abstract description 52
- 239000010362 annatto Substances 0.000 claims abstract description 51
- 239000000341 volatile oil Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000004094 surface-active agent Substances 0.000 claims abstract description 23
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 20
- HHTWOMMSBMNRKP-UHFFFAOYSA-N carvacrol Natural products CC(=C)C1=CC=C(C)C(O)=C1 HHTWOMMSBMNRKP-UHFFFAOYSA-N 0.000 claims abstract description 19
- RECUKUPTGUEGMW-UHFFFAOYSA-N carvacrol Chemical compound CC(C)C1=CC=C(C)C(O)=C1 RECUKUPTGUEGMW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 235000007746 carvacrol Nutrition 0.000 claims abstract description 19
- WYXXLXHHWYNKJF-UHFFFAOYSA-N isocarvacrol Natural products CC(C)C1=CC=C(O)C(C)=C1 WYXXLXHHWYNKJF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims abstract description 17
- 229920000053 polysorbate 80 Polymers 0.000 claims abstract description 17
- 229960004063 propylene glycol Drugs 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims description 8
- WTEVQBCEXWBHNA-UHFFFAOYSA-N Citral Natural products CC(C)=CCCC(C)=CC=O WTEVQBCEXWBHNA-UHFFFAOYSA-N 0.000 claims description 7
- 229940043350 citral Drugs 0.000 claims description 7
- WTEVQBCEXWBHNA-JXMROGBWSA-N geranial Chemical compound CC(C)=CCC\C(C)=C\C=O WTEVQBCEXWBHNA-JXMROGBWSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 20
- 239000003921 oil Substances 0.000 abstract description 10
- 230000036571 hydration Effects 0.000 abstract description 6
- 238000006703 hydration reaction Methods 0.000 abstract description 6
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 abstract description 4
- 235000013923 monosodium glutamate Nutrition 0.000 abstract description 4
- 239000004223 monosodium glutamate Substances 0.000 abstract description 4
- 239000003899 bactericide agent Substances 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 244000000010 microbial pathogen Species 0.000 abstract 1
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 230000000845 anti-microbial effect Effects 0.000 description 31
- 238000010790 dilution Methods 0.000 description 15
- 239000012895 dilution Substances 0.000 description 15
- 239000012071 phase Substances 0.000 description 13
- 239000004599 antimicrobial Substances 0.000 description 11
- 230000001954 sterilising effect Effects 0.000 description 11
- 238000004659 sterilization and disinfection Methods 0.000 description 10
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 235000013772 propylene glycol Nutrition 0.000 description 8
- 239000001670 anatto Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- RAFGELQLHMBRHD-VFYVRILKSA-N Bixin Natural products COC(=O)C=CC(=C/C=C/C(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C(=O)O)/C)C RAFGELQLHMBRHD-VFYVRILKSA-N 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 5
- RAFGELQLHMBRHD-UHFFFAOYSA-N alpha-Fuc-(1-2)-beta-Gal-(1-3)-(beta-GlcNAc-(1-6))-GalNAc-ol Natural products COC(=O)C=CC(C)=CC=CC(C)=CC=CC=C(C)C=CC=C(C)C=CC(O)=O RAFGELQLHMBRHD-UHFFFAOYSA-N 0.000 description 5
- RAFGELQLHMBRHD-SLEZCNMESA-N bixin Chemical compound COC(=O)\C=C\C(\C)=C/C=C/C(/C)=C/C=C/C=C(\C)/C=C/C=C(\C)/C=C/C(O)=O RAFGELQLHMBRHD-SLEZCNMESA-N 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 4
- 230000001580 bacterial effect Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000001963 growth medium Substances 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 238000010587 phase diagram Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000002778 food additive Substances 0.000 description 3
- 235000013336 milk Nutrition 0.000 description 3
- 239000008267 milk Substances 0.000 description 3
- 210000004080 milk Anatomy 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- 244000223760 Cinnamomum zeylanicum Species 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 2
- 240000000560 Citrus x paradisi Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000287828 Gallus gallus Species 0.000 description 2
- 244000246386 Mentha pulegium Species 0.000 description 2
- 235000016257 Mentha pulegium Nutrition 0.000 description 2
- 235000004357 Mentha x piperita Nutrition 0.000 description 2
- 244000223014 Syzygium aromaticum Species 0.000 description 2
- 235000016639 Syzygium aromaticum Nutrition 0.000 description 2
- 235000015278 beef Nutrition 0.000 description 2
- 235000008429 bread Nutrition 0.000 description 2
- 235000021466 carotenoid Nutrition 0.000 description 2
- 235000017803 cinnamon Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
- 235000021474 generally recognized As safe (food) Nutrition 0.000 description 2
- 235000021473 generally recognized as safe (food ingredients) Nutrition 0.000 description 2
- 235000001050 hortel pimenta Nutrition 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
- 235000006010 Bixa orellana Nutrition 0.000 description 1
- 241000934828 Bixaceae Species 0.000 description 1
- LMKYZBGVKHTLTN-NKWVEPMBSA-N D-nopaline Chemical compound NC(=N)NCCC[C@@H](C(O)=O)N[C@@H](C(O)=O)CCC(O)=O LMKYZBGVKHTLTN-NKWVEPMBSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- UPYKUZBSLRQECL-UKMVMLAPSA-N Lycopene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1C(=C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=C)CCCC2(C)C UPYKUZBSLRQECL-UKMVMLAPSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 229920002774 Maltodextrin Polymers 0.000 description 1
- ZVKOASAVGLETCT-UOGKPENDSA-N Norbixin Chemical compound OC(=O)/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(\C)/C=C/C=C(\C)/C=C/C(O)=O ZVKOASAVGLETCT-UOGKPENDSA-N 0.000 description 1
- JERYLJRGLVHIEW-UENHKZIGSA-N Norbixin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C(=O)O)C=CC=CC=CC(=O)O JERYLJRGLVHIEW-UENHKZIGSA-N 0.000 description 1
- 244000086363 Pterocarpus indicus Species 0.000 description 1
- 235000009984 Pterocarpus indicus Nutrition 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- ZVKOASAVGLETCT-UOAMSCJGSA-N all-trans norbixin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C(=O)O)C=CC=C(/C)C=CC(=O)O ZVKOASAVGLETCT-UOAMSCJGSA-N 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 150000001746 carotenes Chemical class 0.000 description 1
- 235000005473 carotenes Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000006103 coloring component Substances 0.000 description 1
- 239000000490 cosmetic additive Substances 0.000 description 1
- 239000004064 cosurfactant Substances 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 235000011850 desserts Nutrition 0.000 description 1
- -1 dicarboxylic acid carotenoid Chemical class 0.000 description 1
- 235000021186 dishes Nutrition 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000576 food coloring agent Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000021472 generally recognized as safe Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 229940035034 maltodextrin Drugs 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229930003811 natural phenol Natural products 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000014594 pastries Nutrition 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 229950008882 polysorbate Drugs 0.000 description 1
- 229940068968 polysorbate 80 Drugs 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- NCYCYZXNIZJOKI-UHFFFAOYSA-N vitamin A aldehyde Natural products O=CC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C NCYCYZXNIZJOKI-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Medicinal Preparation (AREA)
Abstract
The invention relates to an antibacterial transparent microemulsion water aqua and preparation and application thereof, wherein the preparation process of the antibacterial transparent microemulsion water aqua specifically comprises the following steps: (1) Mixing Tween 80 and 1, 2-propylene glycol to obtain a mixed surfactant; (2) Mixing monosodium glutamate oil and carvacrol (optionally adding annatto) to obtain mixed essential oil; (3) And fully mixing the mixed surfactant, the mixed essential oil and water, and preparing the target product by a self-emulsifying method or a phase inversion temperature method. The oil-in-water antibacterial microemulsion has the hydration diameter of less than or equal to 20nm, is clear and transparent, and has broad-spectrum killing capability on food-borne pathogenic microorganisms. Compared with the traditional bactericide, the water aqua is nontoxic and harmless; in addition, the antibacterial microemulsion water aqua with the dissolution mass fraction of 0.0-2.0% of annatto is stable, clear and transparent in an environment with the pH value of 3.0-6.9.
Description
Technical Field
The invention belongs to the technical field of microemulsion, and relates to an antibacterial transparent microemulsion aqueous agent, and preparation and application thereof.
Background
Microemulsions have the characteristics of isotropy, clarity, transparency, and thermodynamic stability. The microemulsion consists of an oil body, a surfactant, a cosurfactant and water. Microemulsions are generally classified into a W/O (water-in-oil) type, an O/W (oil-in-water) type, an O/W/O (oil-in-water) type, a W/O/W (water-in-oil-in-water) type, and a bicontinuous type. The phase transition of the microemulsion is controlled by the volume ratio of hydrophilic to hydrophobic portions of the surfactant, namely: hydrophilic-lipophilic balance (HLB). Whereas changes in the external environment can affect the HLB value, for example: temperature, ionic strength. In general, a microemulsion can be considered a stable microemulsion system when the microemulsion has a hydrated diameter of less than 100nm, a polydisperse phase coefficient (PDI) of less than 0.3, and the microemulsion is clear (semi-) transparent.
The microemulsion is divided into two types, namely ionic microemulsion and nonionic microemulsion, and the microemulsion prepared by taking lecithin as a surfactant belongs to the ionic microemulsion, and the ionic microemulsion is generally not acid-proof and generates phase change in an acidic environment to generate turbidity.
Annatto (annatto) is a carotenoid isolated from the outer layer of the seeds of the tropical shrub Bixa orellana l. (Bixaceae). The main coloring components are hydrophobic dicarboxylic acid monomethyl ester carotene nopaline (bixin) and dicarboxylic acid carotenoid nornopaline (norbixin). The annatto is an edible pigment permitted by national standard GB2760-2014 national Standard for food safety, and the maximum addition amount is 0.01-0.6 g/kg. Annatto is also a safe food colorant licensed by the european union (E160 b) and is "recognized as safe" (Generally recognized as safe, GRAS) by the united states food and drug administration (Food and Drug Administration, FDA) as a food, drug and cosmetic additive. And (5) authentication. In China, annatto has been widely used in foods such as beverages, pastries, desserts, dried (milk) casein, casings, smoked products, dairy products, and the like. At present, domestic enterprises mostly use a method for adding maltodextrin to improve the stability of annatto water, but the defect of unstable acid of annatto water cannot be overcome. To date, no commercial products related to nonionic O/W antimicrobial microemulsions have emerged, nor have techniques been developed to stabilize annatto in an acidic aqueous phase.
Disclosure of Invention
The invention aims to provide an antibacterial transparent microemulsion aqua and preparation and application thereof.
The aim of the invention can be achieved by the following technical scheme:
one of the technical schemes of the invention provides a preparation method of an antibacterial transparent microemulsion water aqua, which comprises the following steps:
(1) Mixing Tween 80 and 1, 2-propylene glycol to obtain a mixed surfactant;
(2) Mixing monosodium glutamate oil and carvacrol to obtain mixed essential oil;
(3) And fully mixing the mixed surfactant, the mixed essential oil and water, and preparing the target product by a self-emulsifying method or a phase inversion temperature method.
Further, in the step (1), the mass ratio of tween 80 to 1, 2-propanediol is (8-9.5): (0.5-2), which may be 8:2,9:1,9.5:0.5, etc., preferably 9.5:0.5.
Further, in the step (2), the flavor essential oil is selected from one or more of peppermint essential oil, lemon essential oil, clove essential oil, grapefruit essential oil, orange essential oil, cinnamon essential oil, beef essential oil, chicken essential oil, lard essential oil, milk essential oil, and bread baking essential oil.
Further, in the step (2), the mass ratio of the monosodium glutamate oil to the carvacrol is 1: (10-1000), optionally with a mass ratio of 1:200-1:10, preferably 1:50.
Further, in the step (3), the mass ratio of the mixed surfactant to the mixed essential oil to the water is (50-80): (2-8): (10-30), optionally 76:8:16, etc.
Further, in the step (3), the process conditions of the self-emulsifying method are specifically as follows: standing and degassing at 1-40 ℃.
Further, in the step (3), the process conditions of the phase inversion temperature method are specifically: heating at 50-95 deg.c for 3-30 min and cooling in water at 1-40 deg.c.
In the step (2), annatto is further added to the mixed essential oil.
The second technical scheme of the invention provides an antibacterial transparent microemulsion aqueous agent, which is prepared by adopting the preparation method.
The third technical scheme of the invention provides application of an antibacterial transparent microemulsion water aqua, wherein the antibacterial transparent microemulsion is used for dissolving annatto with the mass fraction of 0.0% -2.0% and is clear and transparent in an environment with the pH value of 3.0-6.9. When the annatto addition was 0, it indicated that it was not added. Preferably, the mass fraction of annatto is not 0. In particular applications herein, annatto is added during the preparation of the aqueous microemulsion, in particular as a component of the mixed essential oil.
Tween 80 (also called Polysorbate-80, tween 80), an alias polyoxyethylene sorbitan monooleate, foreign name Polysorbate, belongs to a hydrophilic nonionic surfactant. The HLB value is about 15.1, 2-propanediol is colorless viscous liquid at normal temperature, and is a nonionic surfactant auxiliary agent. In the invention, tween 80 and 1, 2-propylene glycol are used as a mixed surfactant to reduce the interfacial tension of oil-water two phases and stabilize the structure of nano particles in the water phase, namely: the surfactant and the surfactant auxiliary agent are gathered at the oil-water interface, so that the Gibbs free energy of the interface is reduced, and the effect of stabilizing the interface is achieved.
The natural phenol compound carvacrol is a broad-spectrum antibacterial plant essential oil, has no toxic or side effect, is a food additive allowed to be used and specified by the national standard GB2076-2014, and is approved as GRAS grade food additive by the U.S. FDA. The chemical structure of carvacrol includes phenolic hydroxyl groups capable of forming hydrogen bonds with water molecules, and meanwhile, the carvacrol has a hydrophobic benzene ring and an alkyl group. Therefore, the carvacrol used by the invention not only has broad-spectrum antibacterial property, but also has the function similar to that of 1, 2-propanediol as a surfactant auxiliary agent.
The particle size of the microemulsion is less than 100nm, and is classified into W/O (water-in-oil), O/W (oil-in-water), O/W/O, W/O/W, bicontinuous, etc. The invention mixes surfactant and surfactant auxiliary agent uniformly in a certain proportion, then mixes wind monosodium glutamate oil and carvacrol containing or not containing annatto uniformly in a certain proportion to prepare mixed essential oil, and then fully and uniformly mixes the mixed surfactant, the mixed essential oil and water in a certain proportion to prepare the microemulsion aqua.
Carvacrol and gourmet powder oil with or without annatto are used as oil phases for sterilization, tween 80 and 1, 2-propanediol form a compound surfactant with an HLB value of about 15 together, and the microemulsion water aqua is prepared in a self-emulsifying or temperature phase inversion mode, so that the originally hydrophobic mixed essential oil is wrapped in hydrophilic microemulsion emulsion drops to form the microemulsion water aqua which stably exists in an acidic water phase.
Compared with the prior art, the invention has the following advantages:
(1) The microemulsion prepared by self-emulsifying or temperature phase inversion can obviously reduce energy consumption, and achieve the purposes of saving energy and reducing production cost;
(2) The surfactant for production, the oil phase and the water raw material are all food-grade raw materials, so that the produced microemulsion product has edibility and biocompatibility;
(3) The carvacrol is a food-grade natural antibacterial essential oil, and compared with the traditional antibacterial agent, the carvacrol has more ensured safety;
(4) The invention has simple process flow, does not involve complex equipment, has easily controlled working parameters, can realize full-automatic production and has high production efficiency;
(5) No chemical reagent is introduced in the process of preparing the microemulsion, the preparation process of each component is simple, no waste water or waste gas is discharged, the damage to the environment is avoided, and the microemulsion belongs to complete green production.
Drawings
FIG. 1 is a three-phase diagram of microemulsions of different formulations, wherein the three-phase diagram of the microemulsions is prepared by sequentially preparing tween 80:1, 2-propanediol in a mass ratio of 8:2 from top to bottom; preparing a three-phase diagram of the microemulsion by using tween 80 to 1, 2-propanediol with a mass ratio of 9 to 1; and preparing a three-phase diagram of the microemulsion by using the tween 80, the 1, 2-propanediol and the mass ratio of 9.5 to 0.5.
FIG. 2 shows the hydration diameters and PDI values for various days of storage of an antimicrobial microemulsion containing annatto (30-fold dilution of test group 1) and an antimicrobial microemulsion not containing annatto (30-fold dilution of control group 1) at pH 3-7.
FIG. 3-1 shows the appearance of samples of an antimicrobial microemulsion containing annatto (30-fold dilution in experimental group 1), an antimicrobial microemulsion not containing annatto (30-fold dilution in control group 1), and a DMF solution of 0.0104mg/g annatto (blank group 1) when irradiated with UVA (365 nm), UVB (302 nm), UVC (254 nm) for 0, 1,2, 3, 4, 6 and 8 hours.
FIG. 3-2 (b) is a graph of the degradation kinetics of an antimicrobial microemulsion containing annatto (experimental group 1, diluted 30-fold) and a DMF solution of 0.0104mg/g annatto (blank group 1) induced by different times UVA, UVB and UVC; FIGS. 3-2 (c), (d) and (e) are changes in hydration diameter and PDI values at UVA, UVB, UVC different time periods for an antimicrobial microemulsion containing annatto (experimental group 1, 30-fold dilution) and an antimicrobial microemulsion not containing annatto (control group 1, 30-fold dilution), respectively.
FIG. 4-1 is a photograph of an antimicrobial microemulsion containing annatto (30-fold dilution of experimental group 1) and an antimicrobial microemulsion not containing annatto (30-fold dilution of control group 1) heated from ambient temperature (25 ℃) to 80℃for 20 minutes, and then cooled to ambient temperature (25 ℃).
Fig. 4-2 shows the hydration diameter and PDI values after heating the antimicrobial microemulsion containing annatto (30-fold dilution of experimental group 1) and the antimicrobial microemulsion not containing annatto (30-fold dilution of control group 1) from ambient temperature (25 ℃) to 80 ℃ for 20 minutes at different pH conditions and then cooling to ambient temperature (25 ℃).
Fig. 5 is a graph of viscosity versus temperature using a rheometer simulation for antimicrobial microemulsions containing annatto (experimental group 1, 30-fold dilution) and not containing annatto (control group 1, 30-fold dilution).
FIG. 6 is a plate sterilization experiment of various gradient dilutions of an antimicrobial microemulsion without annatto.
Fig. 7 is a ninety-six well plate sterilization experiment of various gradient dilutions of an antimicrobial microemulsion without annatto.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
In the following examples, tween 80 (purity greater than 98%) was purchased from shanghai taitan chemical limited (shanghai, china). 1, 2-propanediol (purity greater than 99%) was purchased from Shanghai Pi De medical science and technology Co., ltd (Shanghai, china). Carvacrol (purity greater than 99%) was purchased from alas Ding Shiji limited (Shanghai, china). Citral (purity greater than 97%, which is one of the essential oils of lemon) was purchased from ala Ding Shiji limited (Shanghai, china). Bixin (rosewood, 89.24% pure, origin: peru) was purchased from Hebei Bless Joy Bio-Tech Co., ltd (Hebei Zaole Biotechnology Co., shijia, china).
The remainder, unless specifically stated, is indicative of a conventional commercially available feedstock or conventional processing technique in the art.
Example 1:
a method for preparing nonionic O/W type antibacterial microemulsion water agents with different flavors and stabilizing annatto in an acidic aqueous phase comprises the following specific processes:
mixing 72.2g of Tween 80 and 3.8g of 1, 2-propylene glycol, mixing 0.16g of citral and 7.84g of carvacrol, finally, fully mixing the mixed surfactant, the mixed essential oil and 16g of water, heating in a water bath at 80 ℃ for 10min, and cooling in water at room temperature to normal temperature to obtain a clear transparent stable nonionic O/W type antibacterial microemulsion aqua.
72.2g of Tween 80 and 3.8g of 1, 2-propylene glycol are mixed, 0.16g of citral, 7.84g of carvacrol and 3.9mg of annatto are mixed, finally, the mixed surfactant, the mixed essential oil and 16g of water are fully mixed, the mixture is heated in a water bath at 80 ℃ for 10min and then cooled to normal temperature in room temperature water, and the clear, transparent and stable nonionic O/W type antibacterial microemulsion aqua containing annatto is prepared.
The antimicrobial microemulsion with or without annatto was 10-fold diluted and the antimicrobial microemulsion with annatto had a hydrated diameter of about 17.67nm, a pdi value of 0.143, and the antimicrobial microemulsion without annatto had a hydrated diameter of about 17.44nm, a pdi value of 0.135.
Acid stability studies on antimicrobial microemulsions with or without annatto showed no significant change in the hydration diameter and PDI values of the microemulsions when stored for 35 days in a dark and normal pressure environment at pH 3-7. This shows that the nonionic microemulsion consisting of tween 80 and 1, 2-propanediol maintains good physical stability at pH 3-7 (fig. 1 and 2).
Different ultraviolet wavelengths are used, namely: ultraviolet light irradiation at 365nm (UVA), 302nm (UVB) and 254nm (UVC), with or without annatto. Setting the ultraviolet irradiation power to be 15W, setting the vertical distance between the lamp tube and the sample to be 10cm, and setting the illumination time to be 0-8h. The uv stability studies (fig. 3-1 and 3-2) show that the hydration diameter, PDI value of the antimicrobial microemulsion with or without annatto did not change significantly after UVA, UVB and UVC irradiation, demonstrating good light stability of the annatto microemulsion.
The heat stability studies of the antimicrobial microemulsion with or without annatto (FIGS. 4-1 and 4-2) show that heating at 80℃for 5-20 min causes an increase in the turbidity of the antimicrobial microemulsion. However, after cooling to ambient temperature (-25 ℃) the different microemulsions at pH 3-7 all return to a clear transparent state with no significant change in the hydrated diameter and PDI values of the microemulsions compared to the initial state.
The phase change process of the bixin antimicrobial microemulsion (i.e., test group 1 sample) and the blank antimicrobial microemulsion (i.e., control group 1 sample) during thermal storage was studied using a rheometer simulation. 13mL of freshly prepared bixin antimicrobial microemulsion was added to a concentric cylinder clamp and the temperature program was set as follows: (1) keeping the temperature at 25 ℃ for 10min; (2) raising the temperature to 80 ℃ at a heating rate of 3 ℃/min; (3) keeping the temperature at 80 ℃ for 20min; (4) the temperature is reduced to 25 ℃ at a cooling rate of 3 ℃/min; (5) constant temperature of 25 ℃ for 10min. The constant shear rate was set at 100/s. The same procedure was repeated with 13ml of the blank antimicrobial microemulsion. The viscosity of the bixin antimicrobial microemulsion and the blank antimicrobial microemulsion were studied as a function of temperature at a constant shear rate. Rheological studies of the antimicrobial microemulsion with or without annatto (fig. 5) show that the viscosity of the antimicrobial microemulsion with or without annatto decreases significantly as the temperature increases from 25 ℃ to 80 ℃; the viscosity of the two materials is not changed obviously within 20 minutes of heating at 80 ℃; as the temperature decreases from 80 ℃ to 25 ℃, the viscosity of both gradually increases, and finally reaches the viscosity value before heating.
Preparation of E.coli ATCC 25922 10 after activation and cultivation 4 ，10 3 ，10 2 ，10 1 CFU/mL bacterial liquid, the antibacterial microemulsion which is diluted by 500 times and does not contain annatto is added into the culture medium of the experimental group 2, the culture medium of the control group 2 is untreated, and the culture medium of the experimental group 2 and the culture medium of the control group 2 are both inAfter the biochemical incubator was left for 12 hours at 37 ℃, photographing and counting were performed, see fig. 6 and table 1. The experimental study of plate sterilization shows that the microemulsion diluted by 500 times is 10 to 4 ，10 3 ，10 2 ，10 1 Coli ATCC 25922, which had a significant inhibitory effect on CFU/mL, was found to be significantly inhibited in culture dishes 9cm in diameter, in the count range (10 4 ～10 1 ) The sterilization rate of more than 70 percent can be achieved.
TABLE 1
The antimicrobial microemulsion without annatto was diluted 1000-fold, 500-fold and 100-fold with medium, respectively. To avoid marginal effects, 200 μl of medium was added around the 96-well plate. 180. Mu.L of different sample media was added to each well of the 96-well plate, followed by mixing of 20. Mu.L of different gradient dilutions of E.coli suspension. After the addition, the cover plate is placed in a 37 ℃ incubator for culture. According to the figure 7, ninety-six pore plate sterilization experimental researches show that the antibacterial microemulsion has obvious sterilization effect, and when the concentration of the microemulsion is constant, the higher the concentration of concentrated bacterial liquid is, the better the sterilization effect is; when the concentration of the bacterial liquid is higher, the sterilizing effect of the microemulsions with different concentrations is greatly different; the sterilization efficiency of the microemulsion can reach 100% within a certain concentration range of the bacterial liquid.
In conclusion, the preparation of the nonionic O/W type antibacterial microemulsion water agent with different flavors and the method for stabilizing annatto in the acidic aqueous phase have simple equipment, and can meet the sterilization requirements in actual production and life; the antibacterial microemulsion has higher water solubility and acid stability; the self-emulsifying process does not consume energy, improves the production efficiency and saves the cost; the obtained antibacterial product has high quality and good safety. Therefore, the technology is suitable for large-scale industrial production.
Examples 2 to 11:
most of the same as in example 1 except that in this example, citral was changed to equal mass of peppermint essential oil, clove essential oil, grapefruit essential oil, orange essential oil, cinnamon essential oil, beef essential oil, chicken essential oil, lard essential oil, milk essential oil, and bread baking essential oil, respectively.
Example 12:
most of the same as in example 1, except that in this example, the mass of carvacrol was adjusted so that the mass ratio of citral to carvacrol was adjusted to be 1:200.
Example 13:
most of the same as in example 1, except that in this example, the mass of carvacrol was adjusted so that the mass ratio of citral to carvacrol was adjusted to be 1:10.
Example 14:
most of the same as in example 1 except that in this example, the mass ratio of the mixed surfactant, the mixed essential oil and water was adjusted to 50:2:10, the equal proportion of the rest specific components is adjusted.
Example 15:
most of the same as in example 1 except that in this example, the mass ratio of the mixed surfactant, the mixed essential oil and water was adjusted to 80:8:30, and the proportion of the rest specific components is adjusted.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (1)
1. The antibacterial transparent microemulsion is characterized by being prepared by the following steps:
mixing 72.2g Tween 80 and 3.8g of 1, 2-propylene glycol to obtain a mixed surfactant, mixing 0.16g citral, 7.84g carvacrol and 3.9mg annatto to obtain mixed essential oil, and finally, fully mixing the mixed surfactant, the mixed essential oil and 16g water, heating in a water bath at 80 ℃ for 10min, and cooling in water at room temperature to obtain a target product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111545491.4A CN114259004B (en) | 2021-12-16 | 2021-12-16 | Antibacterial transparent microemulsion aqua and preparation and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111545491.4A CN114259004B (en) | 2021-12-16 | 2021-12-16 | Antibacterial transparent microemulsion aqua and preparation and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114259004A CN114259004A (en) | 2022-04-01 |
| CN114259004B true CN114259004B (en) | 2023-12-22 |
Family
ID=80827562
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111545491.4A Active CN114259004B (en) | 2021-12-16 | 2021-12-16 | Antibacterial transparent microemulsion aqua and preparation and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114259004B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2952213A1 (en) * | 2014-05-26 | 2015-12-09 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Kit for colouring disinfected regions of a surface |
| CN107529792A (en) * | 2015-04-28 | 2018-01-02 | 科汉森天然色素有限责任公司 | Water dispersible coloured composition |
| CN111887264A (en) * | 2020-07-15 | 2020-11-06 | 上海驰纺材料科技有限公司 | Natural plant essential oil microemulsion antibacterial spray and preparation method thereof |
| CN112155146A (en) * | 2020-09-16 | 2021-01-01 | 上海交通大学 | Method for enabling bixin to stably exist in water phase |
| CN113317431A (en) * | 2021-06-11 | 2021-08-31 | 扬州大学 | Oil-in-water carvacrol nanoemulsion and preparation method thereof |
-
2021
- 2021-12-16 CN CN202111545491.4A patent/CN114259004B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2952213A1 (en) * | 2014-05-26 | 2015-12-09 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Kit for colouring disinfected regions of a surface |
| CN107529792A (en) * | 2015-04-28 | 2018-01-02 | 科汉森天然色素有限责任公司 | Water dispersible coloured composition |
| CN111887264A (en) * | 2020-07-15 | 2020-11-06 | 上海驰纺材料科技有限公司 | Natural plant essential oil microemulsion antibacterial spray and preparation method thereof |
| CN112155146A (en) * | 2020-09-16 | 2021-01-01 | 上海交通大学 | Method for enabling bixin to stably exist in water phase |
| CN113317431A (en) * | 2021-06-11 | 2021-08-31 | 扬州大学 | Oil-in-water carvacrol nanoemulsion and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114259004A (en) | 2022-04-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104397828B (en) | Preparation method of modified zein composite slow-release antibacterial liquid membrane | |
| Zahi et al. | Improving the antimicrobial activity of D-limonene using a novel organogel-based nanoemulsion | |
| EP0660676A1 (en) | Novel compositions. | |
| DE102005031464A1 (en) | Emulsifier system, emulsion and their use | |
| JP2014082993A (en) | Gallate-type catechin-containing functional drink | |
| CN109329702B (en) | Compound bactericide of plant extract and preparation method thereof | |
| Mahmoudi et al. | Ultrasonication and encapsulation of Butcher broom (Ruscus Hyrcanus L.) extract and its bioactive effects on qualitative properties, oxidative stability and shelf life of cake | |
| CN104782796A (en) | Vegetable oil-containing antibacterial type edible oil gel and preparation method thereof | |
| CN111067009A (en) | Method for improving thermal stability of beet red pigment | |
| Tripathi et al. | Antioxidant, antibacterial analysis of pectin isolated from banana peel and its application in edible coating of freshly made mozzarella cheese | |
| KR101205680B1 (en) | The manufacturing method of an antioxidizing composition for maintenance of freshness for food and it's composition | |
| FI104093B (en) | Process for the preparation of plant rubber product and its use | |
| CN114259004B (en) | Antibacterial transparent microemulsion aqua and preparation and application thereof | |
| Kavakebi et al. | Green biosynthesized Satureja rechingeri Jamzad-Ag/poly vinyl alcohol film: quality improvement of Oncorhynchus mykiss fillet during refrigerated storage | |
| CN112155146B (en) | Method for enabling bixin to stably exist in water phase | |
| Gao et al. | Application of seed mucilage as functional biopolymer in meat product processing and preservation | |
| CN112220824A (en) | Antibacterial nano microemulsion system, preparation method, application and application method | |
| DE68909011T2 (en) | Liquid egg product. | |
| KR100449209B1 (en) | Denatured Spirulina and manufacturing method thereof | |
| CN110075339A (en) | A kind of natural air scavenging solution and preparation method thereof | |
| KR101761605B1 (en) | Method for manufacturing colored potatoes extract using acid solvents and ultrasonication and method for sterilizing the same | |
| KR980008061A (en) | Decolorized and deodorized purified fish sauce | |
| KR101643298B1 (en) | Method for reducing the bacillus cereus spore contained traditional korean fermented sauces and traditional korean fermented sauces prepared therefrom | |
| CN108840300B (en) | Aseptic filling pretreatment device and process for sauce | |
| WO2014196619A1 (en) | Method for producing sterile konjak glucomannan powder and sterile konjak glucomannan powder obtained thereby |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |