CN114259004A - Antibacterial transparent microemulsion water aqua and preparation and application thereof - Google Patents
Antibacterial transparent microemulsion water aqua and preparation and application thereof Download PDFInfo
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- CN114259004A CN114259004A CN202111545491.4A CN202111545491A CN114259004A CN 114259004 A CN114259004 A CN 114259004A CN 202111545491 A CN202111545491 A CN 202111545491A CN 114259004 A CN114259004 A CN 114259004A
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- 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
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 is as follows: (1) mixing tween 80 and 1, 2-propylene glycol to obtain a mixed surfactant; (2) mixing the flavor essential oil and carvacrol (and annatto can also be added) 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 a 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 existing traditional bactericide, the water aqua is non-toxic and harmless; in addition, the antibacterial microemulsion aqua for dissolving 0.0-2.0% of bixin in mass fraction is stable, clear and transparent in the environment with pH of 3.0-6.9.
Description
Technical Field
The invention belongs to the technical field of microemulsion, and relates to an antibacterial transparent microemulsion water aqua, and preparation and application thereof.
Background
Microemulsions are characterized by isotropy, clarity, and thermodynamic stability. The microemulsion consists of oil body, surfactant, cosurfactant and water. Microemulsions are generally classified into W/O (water-in-oil) type, O/W (oil-in-water) type, O/W/O (oil-in-water-in-oil) type, W/O/W (water-in-oil-in-water) type, and bicontinuous type. The phase transition of the microemulsion is controlled by the volume ratio of the hydrophilic to hydrophobic portions of the surfactant, i.e.: hydrophilic-lipophilic balance (HLB). Whereas changes in the external environment can affect the HLB value, for example: temperature, ionic strength. Generally, a microemulsion system can be considered stable when the hydration diameter of the microemulsion is less than 100nm, the multiple dispersion phase index (PDI) is less than 0.3, and the microemulsion is clear (semi-) transparent.
The microemulsion is divided into two types of ionic microemulsion and non-ionic microemulsion, the microemulsion prepared by adopting lecithin as a surfactant belongs to the ionic microemulsion, the ionic microemulsion is usually not acid-resistant, and phase change occurs in an acidic environment to generate turbidity.
Annatto is a carotenoid isolated from the outer layer of the tropical shrub Bixa orellana l. (Bixaceae) seed. The main coloring components are dicarboxylic acid monomethyl ester carotene bixin (bixin) and dicarboxylic acid carotenoid norbixin (norbixin). The annatto is an edible pigment approved by national standard GB2760-2014 national food safety standard food additive national standard, and the maximum addition amount of the annatto is 0.01-0.6 g/kg. Annatto is also a safe Food colorant approved by the european union (E160b) and is "Generally accepted as safe" by the Food and Drug Administration (FDA) as a Food, Drug and cosmetic additive. And (6) authentication. In China, annatto has been widely used in beverages, pastries, sweets, dry (milk) cheese skins, casings, smoked products, dairy products and other foods. At present, domestic enterprises mostly use a method of adding maltodextrin to improve the stability of the bixin water, but the defect of unstable acid of the bixin is not overcome. So far, no commercial product related to non-ionic O/W antimicrobial microemulsions has emerged, nor has a technique developed to stabilize annatto in acidic aqueous phase.
Disclosure of Invention
The invention aims to provide an antibacterial transparent microemulsion water aqua and preparation and application thereof.
The purpose of the invention can be realized 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 the flavor essential 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-propylene glycol is (8-9.5): (0.5-2), which can be selected from 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 mint essential oil, lemon essential oil, clove essential oil, grapefruit essential oil, citrus 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 flavor essential oil to the carvacrol is 1: (10-1000), the mass ratio is 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 and the like.
Further, in the step (3), the process conditions of the self-emulsification method are specifically as follows: standing and degassing at the temperature of 1-40 ℃.
Further, in the step (3), the process conditions of the phase inversion temperature method are specifically as follows: heating at 50-95 ℃ for 3-30 min, and then cooling in water at 1-40 ℃.
Further, in the step (2), annatto is also added into the mixed essential oil.
The second technical scheme of the invention provides an antibacterial transparent microemulsion water aqua which is prepared by the preparation method.
The third technical scheme of the invention provides application of an antibacterial transparent microemulsion aqua, wherein the antibacterial transparent microemulsion is used for dissolving bixin with the mass fraction of 0.0-2.0% and is clear and transparent in the environment with the pH value of 3.0-6.9. When the addition amount of annatto is 0, it means that annatto is not added. Preferably, the mass fraction of annatto is different from 0. In a specific application herein, annatto is added during the preparation of the microemulsion aqua, specifically as a component of the mixed essential oil.
Tween 80 (also called Polysorbate-80, Tween 80), also known as polyoxyethylene sorbitan monooleate, and also known as Polysorbate, belong to the hydrophilic nonionic surfactants. The HLB value is about 15. 1, 2-propylene glycol 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 mixed surfactants for reducing the interfacial tension of oil-water two phases and stabilizing the structure of nanoparticles in a water phase, namely: the surfactant and the surfactant auxiliary agent are gathered at an 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 phenolic compound carvacrol is a broad-spectrum antibacterial plant essential oil, has no toxic or side effect, is a food additive which is allowed to be used and is regulated by the national standard GB2076-2014, and is approved as a GRAS-grade food additive by the FDA in the United states. The chemical structure of carvacrol includes a phenolic hydroxyl group capable of forming hydrogen bonds with water molecules, and has a hydrophobic benzene ring and an alkyl group. Therefore, the carvacrol used in the invention not only has broad-spectrum antibacterial property, but also has the function similar to that of 1, 2-propylene glycol as a surfactant auxiliary agent.
The microemulsion has a particle size of less than 100nm, and is classified into W/O (water-in-oil), O/W (oil-in-water), O/W/O, W/O/W, bicontinuous, and the like. The preparation method comprises the steps of uniformly mixing a surfactant and a surfactant auxiliary agent according to a certain proportion, uniformly mixing flavor essential oil and carvacrol containing or not containing annatto according to a certain proportion to prepare mixed essential oil, and fully and uniformly mixing the mixed surfactant, the mixed essential oil and water according to a certain proportion to prepare the microemulsion aqua.
Carvacrol and gourmet powder oil which contain or do not contain annatto are used as oil phases for sterilization, tween 80 and 1, 2-propylene glycol jointly form a compound surfactant with an HLB value of about 15, and the microemulsion 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 aqua which stably exists in an acidic water phase.
Compared with the prior art, the invention has the following advantages:
(1) the microemulsion is prepared in a self-emulsifying or temperature phase inversion mode, so that the energy consumption can be obviously reduced, and the aims of saving energy and reducing the production cost are fulfilled;
(2) the surfactant, the oil phase and the water raw materials for production are food-grade raw materials, so that the produced microemulsion product has edibility and biocompatibility;
(3) carvacrol is a food-grade natural antibacterial essential oil, and compared with the traditional antibacterial agent, the safety is better guaranteed;
(4) the invention has simple process flow, does not relate to complex equipment, has easy control of 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 and waste gas are discharged, the damage to the environment is avoided, and the method belongs to completely green production.
Drawings
FIG. 1 is a three-phase diagram of microemulsions with different formulations, wherein the three-phase diagram of the microemulsion prepared from Tween 80:1 and 2-propylene glycol in a mass ratio of 8:2 is shown from top to bottom; a three-phase diagram for preparing the microemulsion by using Tween 80:1, 2-propylene glycol in a mass ratio of 9: 1; a three-phase diagram of microemulsion preparation with the mass ratio of Tween 80:1 and 2-propylene glycol of 9.5: 0.5.
Fig. 2 shows the hydration diameter and PDI value of antibacterial microemulsion containing annatto (experimental 1, diluted 30-fold) and antibacterial microemulsion without annatto (control 1, diluted 30-fold) stored at pH 3-7 for different days.
FIG. 3-1 is the appearance of samples when irradiated with UVA (365nm), UVB (302nm), UVC (254nm) for 0, 1,2, 3, 4, 6 and 8h, an antimicrobial microemulsion containing annatto (Experimental 1, diluted 30 times), an antimicrobial microemulsion without annatto (control 1, diluted 30 times), a DMF solution of 0.0104mg/g annatto (blank 1).
In FIG. 3-2 (b) is the degradation kinetics of antibacterial microemulsion containing annatto (Experimental group 1, diluted 30 times) and DMF solution of 0.0104mg/g annatto (blank group 1) induced by different time of UVA, UVB and UVC; FIGS. 3-2(c), (d), (e) are the changes in hydration diameter and PDI induced by different time periods of UVA, UVB and UVC for antibacterial microemulsion containing bixin (Experimental group 1, diluted 30 times) and antibacterial microemulsion not containing bixin (control group 1, diluted 30 times), respectively.
FIG. 4-1 is a photograph of an antimicrobial microemulsion containing annatto (Experimental group 1, diluted 30 times) and an antimicrobial microemulsion not containing annatto (control group 1, diluted 30 times) heated from ambient temperature (. about.25 ℃) to 80 ℃ for 20min and then cooled to ambient temperature (. about.25 ℃).
FIG. 4-2 shows hydration diameter and PDI values of antibacterial microemulsion containing annatto (Experimental group 1, diluted 30 times) and antibacterial microemulsion not containing annatto (control group 1, diluted 30 times) after heating from ambient temperature (25 ℃) to 80 ℃ for 20min and then cooling to ambient temperature (25 ℃) under different pH conditions.
Fig. 5 is a graph of the viscosity of antibacterial microemulsion containing annatto (experimental 1, diluted 30 times) and antibacterial microemulsion not containing annatto (control 1, diluted 30 times) as a function of temperature using rheometer simulation.
Fig. 6 is a plate sterilization experiment of different gradient dilutions of antibacterial microemulsion without bixin.
Fig. 7 is a ninety-six well plate sterilization experiment of different gradient dilutions of antibacterial microemulsion without bixin.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In each of the following examples, tween 80 (greater than 98% pure) was purchased from shanghai taitan chemical limited (shanghai, china). 1, 2-propanediol (purity greater than 99%) was purchased from Shanghai Bide pharmaceutical technology, Inc. (Shanghai, China). Carvacrol (purity greater than 99%) was purchased from alatin reagent limited (shanghai, china). Citral (purity greater than 97%, which is one of the lemon essential oils) was purchased from alatin reagent limited (shanghai, china). Bixin (bixin, 89.24% pure, produced in peru) was purchased from Hebei Bless Joy Bio-Tech co, Ltd (Hebei youzala biotechnology limited, shijiazhuan, china).
Otherwise, unless otherwise specified, all the conventional commercial raw materials or conventional processing techniques are used in the art.
Example 1:
a method for preparing nonionic O/W type antibacterial microemulsion aqua with different flavors and using the aqua for stabilizing annatto in an acidic aqueous phase comprises the following specific steps:
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 the temperature of 80 ℃ for 10min, and cooling in the water at room temperature to prepare the clear, transparent and stable nonionic O/W type antibacterial microemulsion aqueous solution.
Mixing 72.2g of Tween 80 and 3.8g of 1, 2-propylene glycol, mixing 0.16g of citral, 7.84g of carvacrol and 3.9mg of annatto, finally, fully mixing the mixed surfactant, the mixed essential oil and 16g of water, heating in a water bath at the temperature of 80 ℃ for 10min, and cooling in the water at the room temperature to the normal temperature to prepare the clear, transparent and stable nonionic O/W type antibacterial microemulsion aqua containing the annatto.
The antibacterial microemulsion with or without annatto was diluted 10-fold and the hydrated diameter of the antibacterial microemulsion with annatto was determined to be about 17.67nm with a PDI value of 0.143, and the hydrated diameter of the antibacterial microemulsion without annatto was determined to be about 17.44nm with a PDI value of 0.135.
Acid stability studies of the antibacterial microemulsions with and without bixin showed no significant change in the hydrated diameter and PDI value of the microemulsion when stored for 35 days in a dark and atmospheric environment at pH 3-7. This indicates that the non-ionic microemulsion consisting of tween 80 and 1, 2-propanediol maintains good physical stability in an environment of pH 3-7 (fig. 1 and 2).
Different uv wavelengths were used, namely: 365nm (UVA), 302nm (UVB) and 254nm (UVC) ultraviolet lamps irradiate the antibacterial microemulsion with or without annatto. Setting the ultraviolet radiation power at 15W, the vertical distance between the lamp tube and the sample at 10cm, and the illumination time at 0-8 h. Ultraviolet stability studies (fig. 3-1 and 3-2) show that the hydrated diameter, PDI value of antibacterial microemulsions with and without bixin orange did not change significantly after UVA, UVB and UVC irradiation, demonstrating good photostability of bixin microemulsions.
A thermal stability study (figure 4-1 and figure 4-2) on the antibacterial microemulsion containing or not containing the annatto indicates that the turbidity of the antibacterial microemulsion is increased when the antibacterial microemulsion is heated at 80 ℃ for 5-20 min. However, upon cooling to ambient temperature (-25 ℃), the different microemulsions at pH 3-7 all returned to a clear and transparent state, and the hydrated diameter and PDI value of the microemulsions did not change significantly from the initial state.
The phase transition process of the bixin antibacterial microemulsion (i.e. experimental 1 sample) and the blank antibacterial microemulsion (i.e. control 1 sample) during the heat storage process was studied using rheometer simulation. Adding 13mL of freshly prepared bixin antibacterial microemulsion into a concentrical cylinder clamp, and setting the temperature program as follows: (1) keeping the temperature at 25 ℃ for 10 min; (2) the temperature is increased to 80 ℃ at the rate of 3 ℃/min; (3) keeping the temperature at 80 ℃ for 20 min; (4) the temperature is reduced to 25 ℃ at the cooling rate of 3 ℃/min; (5) keeping the temperature at 25 ℃ for 10 min. The constant shear rate was set at 100/s. The same procedure was repeated with 13ml of blank antimicrobial microemulsion. The variation of the viscosities of the bixin and blank antimicrobial microemulsions with temperature under the effect of constant shear rate was investigated. Rheological studies (fig. 5) on antibacterial microemulsions with and without bixin showed that as the temperature increased from 25 ℃ to 80 ℃, the viscosity of antibacterial microemulsions with and without bixin decreased significantly; the viscosity of the two materials is not changed obviously within 20min of heating at 80 ℃; the viscosity of the two materials gradually increases as the temperature decreases from 80 ℃ to 25 ℃, and finally reaches the value of the viscosity before heating.
TABLE 1
The antibacterial microemulsion without bixin was diluted 1000-fold, 500-fold and 100-fold with medium, respectively. To avoid marginal effects, 200 μ L of medium was added around the 96-well plate. mu.L of different sample media were added to each well of a 96-well plate, followed by mixing 20. mu.L of different gradient dilutions of E.coli suspension. After the addition, the plate was placed in a 37 ℃ incubator for culture. In combination with fig. 7, ninety-six pore plate sterilization experimental studies show that the antibacterial microemulsion has an obvious sterilization effect, and when the concentration of the microemulsion is fixed, the higher the concentration of the bacterial liquid, the better the sterilization effect; when the concentration of the bacterial liquid is higher, the sterilization effects of the microemulsions with different concentrations are greatly different; the micro-emulsion sterilization can achieve 100 percent of sterilization efficiency within a certain concentration range of bacterial liquid.
In conclusion, the preparation of the nonionic O/W type antibacterial microemulsion aqua with different flavors and the method for stabilizing the annatto in the acidic aqueous phase have simple equipment, and can meet the sterilization requirement in actual production and life; the antibacterial microemulsion has high water solubility and acid stability; the self-emulsifying process does not consume energy, so that the production efficiency is improved, and the cost is saved; the obtained antibacterial product has high quality and good safety. Therefore, the technology is suitable for large-scale industrial production.
Examples 2 to 11:
compared with the example 1, most of the essential oil is the same, except that in the example, the citral is respectively changed into equal-quality peppermint essential oil, clove essential oil, grapefruit essential oil, citrus essential oil, cinnamon essential oil, beef essential oil, chicken essential oil, lard essential oil, milk essential oil and bread baking essential oil.
Example 12:
most of them were 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 1: 200.
Example 13:
most of them were 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 1: 10.
Example 14:
compared with example 1, most of them are the same except that in this example, the mass ratio of the mixed surfactant, the mixed essential oil and the water is adjusted to 50: 2: 10, adjusting the rest specific components in equal proportion.
Example 15:
compared with example 1, most of them are the same except that in this example, the mass ratio of the mixed surfactant, the mixed essential oil and the water is adjusted to 80: 8: 30, adjusting the rest specific components in equal proportion.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, 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 embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The preparation method of the antibacterial transparent microemulsion aqua is characterized by comprising the following steps:
(1) mixing tween 80 and 1, 2-propylene glycol to obtain a mixed surfactant;
(2) mixing the flavor essential 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.
2. The preparation method of the antibacterial transparent microemulsion aqua according to claim 1, wherein in the step (1), the mass ratio of tween 80 to 1, 2-propylene glycol is (8-9.5): (0.5-2).
3. The method for preparing the antibacterial transparent microemulsion aqua according to claim 1, wherein in the step (2), the flavor essential oil is one or more of mint essential oil, lemon essential oil, clove essential oil, grapefruit essential oil, citrus essential oil, cinnamon essential oil, beef essential oil, chicken essential oil, lard essential oil, milk essential oil and bread baking essential oil.
4. The preparation method of the antibacterial transparent microemulsion aqua according to claim 1, wherein in the step (2), the mass ratio of the flavor essential oil to the carvacrol is 1: (10-1000).
5. The preparation method of the antibacterial transparent microemulsion aqua according to claim 1, wherein 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).
6. The preparation method of the antibacterial transparent microemulsion aqua according to claim 1, wherein in the step (3), the process conditions of the self-emulsifying method are as follows: standing and degassing at the temperature of 1-40 ℃.
7. The preparation method of the antibacterial transparent microemulsion aqua according to claim 1, wherein in the step (3), the process conditions of the phase inversion temperature method are as follows: heating at 50-95 ℃ for 3-30 min, and then cooling in water at 1-40 ℃.
8. The method for preparing the antibacterial transparent microemulsion aqua according to claim 1, wherein annatto is further added to the mixed essential oil in the step (2).
9. An antibacterial transparent microemulsion aqua prepared by the preparation method of any one of claims 1 to 8.
10. The use of the aqueous antibacterial transparent microemulsion according to claim 9, wherein the antibacterial transparent microemulsion is used for dissolving bixin with a mass fraction of 0.0-2.0% and is clear and transparent in an environment with a pH of 3.0-6.9.
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| 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 |
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| 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 |
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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 |
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