CN117224481A - Food-grade O/W quercetin microemulsion, and preparation method and application thereof - Google Patents
Food-grade O/W quercetin microemulsion, and preparation method and application thereof Download PDFInfo
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- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 title claims abstract description 224
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 title claims abstract description 111
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 title claims abstract description 111
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229960001285 quercetin Drugs 0.000 title claims abstract description 111
- 235000005875 quercetin Nutrition 0.000 title claims abstract description 111
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000593 microemulsion method Methods 0.000 title description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- HIQIXEFWDLTDED-UHFFFAOYSA-N 4-hydroxy-1-piperidin-4-ylpyrrolidin-2-one Chemical compound O=C1CC(O)CN1C1CCNCC1 HIQIXEFWDLTDED-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000004094 surface-active agent Substances 0.000 claims abstract description 15
- 235000013305 food Nutrition 0.000 claims abstract description 9
- 239000003921 oil Substances 0.000 claims description 49
- 235000019198 oils Nutrition 0.000 claims description 48
- 239000012071 phase Substances 0.000 claims description 42
- 239000002245 particle Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 14
- 239000003814 drug Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000004064 cosurfactant Substances 0.000 claims description 9
- 239000003995 emulsifying agent Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 229940079593 drug Drugs 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 5
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 claims description 3
- 235000019483 Peanut oil Nutrition 0.000 claims description 3
- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 claims description 3
- 239000000312 peanut oil Substances 0.000 claims description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 3
- 229920000053 polysorbate 80 Polymers 0.000 claims description 3
- 239000008346 aqueous phase Substances 0.000 claims description 2
- YYZUSRORWSJGET-UHFFFAOYSA-N ethyl octanoate Chemical compound CCCCCCCC(=O)OCC YYZUSRORWSJGET-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 9
- 239000013543 active substance Substances 0.000 abstract 3
- 239000000825 pharmaceutical preparation Substances 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 11
- 239000002994 raw material Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
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- -1 flavonoid compound Chemical class 0.000 description 4
- 238000005063 solubilization Methods 0.000 description 4
- 230000007928 solubilization Effects 0.000 description 4
- 230000000975 bioactive effect Effects 0.000 description 3
- 239000002537 cosmetic Substances 0.000 description 3
- 238000000502 dialysis Methods 0.000 description 3
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- 238000002474 experimental method Methods 0.000 description 3
- 229930003935 flavonoid Natural products 0.000 description 3
- 235000017173 flavonoids Nutrition 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000693 micelle Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229920002494 Zein Polymers 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000004071 biological effect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000012377 drug delivery Methods 0.000 description 2
- 238000000338 in vitro Methods 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000013268 sustained release Methods 0.000 description 2
- 239000012730 sustained-release form Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000005019 zein Substances 0.000 description 2
- 229940093612 zein Drugs 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
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- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
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Abstract
The application discloses a food-grade O/W quercetin microemulsion, a preparation method and application thereof, wherein the food-grade O/W quercetin microemulsion comprises the following components in percentage by weight based on the weight: 10% -42% of surfactant, 2% -32% of oil phase solution and the balance of water phase; the oil phase solution consists of isopropyl myristate and ethanol, wherein the weight ratio of the isopropyl myristate to the ethanol=1:1-4. The O/W microemulsion has simple preparation method, is an excellent carrier of active substances or functional substances with poor stability and water solubility represented by quercetin, thereby improving the stability of the active substances or functional substances in food and pharmaceutical preparations and improving the slow release behavior of the active substances or functional substances.
Description
Technical Field
The application belongs to the field of pharmaceutics, and particularly relates to food-grade O/W quercetin microemulsion, and a preparation method and application thereof.
Background
A microemulsion is a dispersion of two immiscible liquids, one of which is dispersed in the other in the form of tiny droplets. Microemulsions have many advantages such as high bioavailability, high solubility, high stability, low toxicity, etc., and thus have wide application in the fields of pharmaceuticals, cosmetics, foods, etc.
The oil-in-water (O/W) microemulsion is a microemulsion which takes oil as a disperse phase and water as a continuous phase, can effectively wrap bioactive substances, protect the bioactive substances from the influence of external environment, and prolong the action time of the bioactive substances. Oil-in-water microemulsions generally require the addition of hydrophilic emulsifiers to reduce the surface tension of the water-oil interface, promoting the formation and stabilization of the microemulsion.
Quercetin is a naturally occurring flavonoid compound and has various biological activities such as antioxidation, anti-inflammatory, antibacterial, anti-tumor and the like. Quercetin has low solubility in water, and its application in pharmaceuticals and cosmetics is limited. Therefore, the use of oil-in-water microemulsions to support quercetin is an effective method to increase the solubility and bioavailability of quercetin.
At present, the quercetin is mainly modified or encapsulated by a preparation carrier at home and abroad to solve the problems that the quercetin Pi Suyi is oxidized and insoluble in water and the like. For example, in patent CN105534897a, flos Sophorae Immaturus is used as a raw material to prepare quercetin, the quercetin is modified, and then the quercetin microemulsion is mixed with the prepared blank microemulsion and subjected to ultrasonic vibration to obtain the high water-solubility quercetin microemulsion. Ma Juanjuan and the like are based on the interaction between zein and polysaccharide, phospholipid and polyphenol to prepare quercetin composite colloidal particles and stabilize Pickering emulsion delivery systems. The solubility and photo-thermal stability of the quercetin are obviously improved. (Ma Juanjuan; research on the biological Activity and bioavailability of quercetin delivery vehicles constructed based on zein, doctor's laboratory paper, university of North China, 2021, 4:1-179.). However, these methods have complicated preparation processes and high cost.
Disclosure of Invention
The application aims to: aiming at the defects of the prior art, the technical problem to be solved by the application is to provide the oil-in-water quercetin microemulsion and the preparation method thereof, and the problem of low solubility and poor bioavailability of the quercetin is solved by using the microemulsion technology to prepare the oil-in-water quercetin microemulsion, so that the stability and the drug effect of the quercetin are improved. The emulsion has good stability and sustained release performance, and can effectively improve the solubility and bioavailability of quercetin.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows:
a food-grade O/W quercetin microemulsion comprises a blank microemulsion composed of a surfactant, an oil phase solution and an aqueous phase, and the blank microemulsion is a carrier encapsulated quercetin microemulsion; the oil phase solution comprises oil and cosurfactant;
the quercetin microemulsion has the following characteristics:
(1) Appearance: transparent or translucent, colorless or pale yellow liquid;
(2) Average particle diameter: 200-300 nm;
(3) pH value: 6.0 to 8.0;
(4) Drug content: 0.4 mg/g-1.51 mg/g;
(5) Drug release: the accumulated release rate of the quercetin microemulsion is 25-47% within 24 hours.
Specifically, the quercetin is a flavonoid compound, and the chemical name of the quercetin is 3,3',4',5, 7-pentahydroxy flavonoid.
Specifically, the surfactant is any one of an emulsifier EL-35, tween-80 and an emulsifier OP, and the emulsifier EL-35 is preferred. EL-35 is a nonionic surfactant, has the chemical name of polyoxyethylene-35 stearyl alcohol ether, has the characteristics of low toxicity, low irritation, low conductivity and the like, can effectively reduce the surface tension of the microemulsion and the repulsive force between micelles, and improves the stability and the solubilization capacity of the microemulsion.
Specifically, the oil is selected from any one of peanut oil, isopropyl myristate, ethyl butyrate and ethyl n-octoate, preferably isopropyl myristate, and the chemical name of the oil is isopropyl myristate. Isopropyl myristate is a non-volatile or low-volatile oil, has good biocompatibility and safety, and can effectively avoid loss and deterioration of the drug caused by volatilization or oxidation of the oil during storage and use.
Further, the oil phase solution also contains cosurfactant, and the cosurfactant is any one of absolute ethyl alcohol, polyethylene glycol 400, ethylene glycol and isopropanol, preferably absolute ethyl alcohol. The absolute ethyl alcohol is used for reducing interfacial tension, adjusting the polarity of water and oil and adjusting the HLB value. Absolute ethyl alcohol is a common solubilizer and solubilizer, and can increase the solubility of quercetin in an oil phase and the content of the oil phase in the microemulsion, so that the drug loading and release efficiency are improved.
Preferably, the components and weight percentages are as follows: 10% -42% of surfactant, 2% -32% of oil phase solution and the balance of water phase; the oil phase solution consists of isopropyl myristate and ethanol, wherein the weight ratio of the isopropyl myristate to the ethanol=1:1-4.
In the blank microemulsion, the optimal microemulsion comprises the following formula: the components and weight percentages are as follows: 30% of surfactant, 20% of oil phase solution and the balance of water phase.
Preferably, the oil phase consists of isopropyl myristate and ethanol in a weight ratio of isopropyl myristate (IPM): ethanol=1:2.
Furthermore, the application also provides a preparation method of the food-grade O/W microemulsion, which specifically comprises the following steps:
under the condition of continuous stirring, adding the surfactant into a mixing kettle according to the weight percentage, then adding the oil phase solution, and finally adding the water phase until the liquid is clear and transparent.
Preferably, the stirring speed is 100 rpm-500 rpm; the temperature is 50-60 ℃, preferably 55 ℃; the pH is controlled to be 6 to 8, preferably 7.4.
Furthermore, the application also provides application of the food-grade O/W quercetin microemulsion as a carrier in food and pharmacy.
The beneficial effects are that:
(1) The quercetin microemulsion prepared by the application has good stability and sustained-release effect, and can be used in foods or medicines to increase the solubility and bioavailability of quercetin. The accumulated release rate of the quercetin in 24 hours is 25% -47%, which indicates that the microemulsion has good slow release effect, and can prolong the action time of the medicine in vivo and improve the bioavailability of the medicine.
(2) Compared with the prior art, the quercetin microemulsion prepared by the application has the following advantages:
high solubility and stability: quercetin has low solubility in water, which limits its bioavailability and efficacy. However, the microemulsion can significantly improve the solubility of quercetin in water, so that the quercetin can be absorbed and utilized by human body more easily.
The preparation method of the O/W microemulsion is simple and easy to implement, and only the components are added according to the proportion and mixed uniformly.
The particles of the O/W microemulsion have small particle size (< 300 nm) and uniform distribution, and the microemulsion system has good stability.
In conclusion, the synthesized quercetin oil-in-water microemulsion has great potential in various application fields such as drug delivery, functional food and cosmetic industries and the like.
Drawings
The foregoing and/or other advantages of the application will become more apparent from the following detailed description of the application when taken in conjunction with the accompanying drawings and detailed description.
FIG. 1 is a linear relationship between quercetin concentration and ultraviolet absorption.
Figure 2 is the solubility of different surfactant micelle solutions to quercetin.
Figure 3 is the solubility of different oils for quercetin.
FIG. 4 content of quercetin in microemulsion at different temperatures.
FIG. 5 content of quercetin in microemulsions at different pH values.
FIG. 6 is a plot of quercetin release rate versus time for different samples.
Detailed Description
The application is described below with reference to specific examples. It will be appreciated by those skilled in the art that these examples are for illustration of the application only and are not intended to limit the scope of the application in any way.
The experimental methods in the following examples are conventional methods unless otherwise specified. The raw materials and reagent materials used in the examples below are all commercially available products unless otherwise specified.
The experimental steps are as follows:
9.8mg of quercetin samples were accurately weighed and dissolved in absolute ethanol to prepare absolute ethanol solutions with concentrations of 1.96, 3.92, 5.88, 7.84, 9.80 and 11.76 ug/mL. The UV absorption of each solution was measured at 370nm, respectively, and the results are shown in FIG. 1.
1. Selection of surfactants
The absorbance values of the sample solutions of EL-35, tween-80 and emulsifier OP dissolved with quercetin were measured at 370nm, and the solubility of quercetin was calculated, and the results are shown in FIG. 2. As can be seen from FIG. 2, the solubility of quercetin in emulsion micelle solution EL-35 is highest, and the emulsifier EL-35 is selected as surfactant because EL-35 has high edible safety, wide application range and strong emulsifying capacity.
2. Selection of oil phase
The solubility of quercetin in peanut oil, ethyl butyrate, isopropyl myristate, ethyl n-octoate sample solutions was measured at 370nm and the results are shown in figure 3. As can be seen from fig. 3, the solubility of quercetin in the above common oils is not great, and the solvent alone cannot meet the drug delivery requirements, and isopropyl myristate is primarily selected.
3. Cosurfactant selection
The cosurfactant has the functions of reducing interfacial tension, increasing interfacial fluidity and regulating HLB value. The experiment is carried out on absolute ethyl alcohol, polyethylene glycol 400, ethylene glycol and isopropanol respectively, wherein the isopropanol is toxic and has strong hydrophilicity, and oil-in-water microemulsion is easy to form. The co-surfactant carbon chain is too long and the molecular volume is large, which results in increased resistance to intercalation into the membrane. The solubility of the cosurfactant and the oil is determined by testing the solubility of the cosurfactant and the oil in different proportions in consideration of factors such as short chain, non-toxic safety, micro emulsion area size and the like. The ratio of absolute ethanol to oil is 1:2. 1: 1. 2:1, the solubility is 17.4mg/g, 23.5mg/g and 32.75mg/g respectively; the proportions of polyethylene glycol 400 and oil are 1:2. 1: 1. 2:1, the solubility is 2.25mg/g, 6.7mg/g and 10.7mg/g respectively; as available, in the maximum solubilization experiments, the ratio of absolute ethanol, polyethylene glycol 400, and oil was all 2:1. From the analysis, it was determined that the ratio of isopropyl myristate to absolute ethanol in the EL-35/ethanol/isopropyl myristate/water system was 1:2.
4. Temperature selection
The prepared O/W microemulsion is added with excessive quercetin, and is placed in water baths with the temperature of 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60 and 65 ℃ for one hour, and after magnetic stirring, the microemulsion is obtained by centrifugation and filtration, and the influence of the microemulsion on the solubilization capacity of the quercetin at different temperatures is examined by adopting an ultraviolet spectrophotometry for quantitative analysis. FIG. 4 shows that the solubility of quercetin increases from 0.4mg/g to 0.8mg/g as the temperature increases from 10℃to 25 ℃; when the temperature is raised to 55 ℃, the solubility of quercetin is increased to 0.151mg/g; the temperature continues to rise and the solubility of quercetin tends to decrease. From this, it was found that the solubility of quercetin was maximized when the temperature was 55 ℃, and therefore the treatment temperature was selected to be the optimum temperature of 55 ℃.
Selection of pH
The O/W microemulsion was formulated with phosphate buffer, and at 55deg.C, excess quercetin was added to observe the effect of different pH on the solubilization capacity of quercetin.
It can be seen from FIG. 5 that below pH 7.4, the solubility of quercetin increases from 0.4mg/g to 1.51mg/g as the pH increases from 4 to 7.4; as the pH was increased from 7.4 to 10, the solubility of quercetin was reduced from 1.51mg/g to 0.87mg/g. Thus, the solubility of quercetin was maximized at pH 7, so pH 7.4 was selected as the optimal pH.
Example 1O/W microemulsion
The formula of the raw materials comprises: (Unit: g)
The preparation method comprises the following steps:
firstly, mixing ethanol and isopropyl myristate to obtain an oil phase solution; under the condition that a magnetic stirrer is continuously stirred, the rotating speed is 250rpm, adding EL-35 into a mixing kettle, then adding the oil phase solution, and finally adding water until the mixing system is clear and transparent, thus obtaining the microemulsion with the average particle diameter of 215 nm.
Example 2 an O/W microemulsion
The formula of the raw materials comprises: (Unit: kg)
The preparation method comprises the following steps:
firstly, mixing ethanol and isopropyl myristate to obtain an oil phase solution; under the condition that a magnetic stirrer is continuously stirred, the rotating speed is 100rpm, adding EL-35 into a mixing kettle, then adding the oil phase solution, and finally adding water until the mixing system is clear and transparent, thus obtaining the microemulsion with the average particle diameter of 227 nm.
Example 3 an O/W microemulsion
The formula of the raw materials comprises: (Unit: g)
The preparation method comprises the following steps:
firstly, mixing ethanol and isopropyl myristate to obtain an oil phase solution; under the condition that a magnetic stirrer is continuously stirred, the rotating speed is 500rpm, adding EL-35 into a mixing kettle, then adding the oil phase solution, and finally adding water until the mixing system is clear and transparent, thus obtaining the microemulsion with the average particle diameter of 263 nm.
EXAMPLE 4A quercetin O/W microemulsion
The formula of the raw materials comprises: (Unit: g)
The preparation method comprises the following steps:
ethanol and isopropyl myristate are mixed to obtain an oil phase solution. Under the condition of uninterrupted stirring by a magnetic stirrer, the rotating speed is 250rpm, adding EL-35 into a mixing kettle placed in a water bath at 55 ℃, then adding the oil phase solution, adding water, adjusting the pH of the solution to 7.4, then adding excessive quercetin, stirring to dissolve, and centrifugally filtering to obtain clear and transparent liquid.
The obtained quercetin microemulsion has the following characteristics:
(1) Appearance: transparent or translucent, colorless or pale yellow liquid;
(2) Average particle diameter: 232nm;
(3) Drug release: as shown in fig. 6, the accumulated release rate of the quercetin microemulsion in 24 hours is 47%, which indicates that the quercetin microemulsion has a better slow release effect.
Example 5A quercetin O/W microemulsion
The formula of the raw materials comprises: (Unit: g)
The preparation method comprises the following steps:
ethanol and isopropyl myristate are mixed to obtain an oil phase solution. Under the condition of uninterrupted stirring by a magnetic stirrer, the rotating speed is 100rpm, adding EL-35 into a mixing kettle placed in a water bath at 10 ℃, then adding the oil phase solution, adding water, adjusting the pH value of the solution to be 4, then adding excessive quercetin, stirring to dissolve, and then centrifugally filtering to obtain clear and transparent liquid.
The average particle size of the obtained quercetin microemulsion is 270nm, and the accumulated release rate of the quercetin microemulsion within 24 hours is 25%.
EXAMPLE 6A quercetin O/W microemulsion
The formula of the raw materials comprises: (Unit: g)
The preparation method comprises the following steps:
ethanol and isopropyl myristate are mixed to obtain an oil phase solution. Under the condition of uninterrupted stirring by a magnetic stirrer, the rotating speed is 250rpm, adding EL-35 into a mixing kettle placed in a water bath at 65 ℃, then adding the oil phase solution, adding water, adjusting the pH of the solution to 11, then adding excessive quercetin, stirring to dissolve, and centrifugally filtering to obtain clear and transparent liquid, wherein the average particle size of the obtained quercetin microemulsion is 294nm. The accumulated release rate of the quercetin microemulsion is 32% within 24 hours, which shows that the quercetin microemulsion has a good slow release effect.
Test example 1 investigation of microemulsion Performance
1. Measurement of microemulsion particle size
The particle size of the microemulsion samples prepared in examples 1-6 was measured at 25℃using a Nano-Zs90 Markov laser scatterometer, and the average particle size of the microemulsion was calculated. The results are shown in Table 1.
TABLE 1 measurement results of microemulsion particle size
The results in Table 1 show that the O/W microemulsions prepared in examples 1-6 all have particle sizes of less than 300nm. And compared with the corresponding blank microemulsion (the microemulsion prepared in the examples 1-3), the particle size of the quercetin O/W microemulsion is slightly increased, and the dispersion degree is not significantly different.
Test example 2 Release test of quercetin O/W microemulsion according to the application
The test method comprises the following steps: simulating in-vitro release by using a dialysis bag, and examining the in-vitro release effect of a quercetin microemulsion system.
The reference was quercetin 1.51mg/g oil phase solution. 5mL of the quercetin microemulsion prepared in examples 4-6 and quercetin 1.51mg/g oil phase solution were taken in dialysis bags, respectively, and the dialysis bags were placed in triangular flasks containing 50mL of PBS and magnetically stirred at room temperature. 5mL of dialysate was taken from the flask at different times and made up with the same volume of PBS. Measuring quercetin content by ultraviolet spectrophotometry.
The results of example 4 are shown in FIG. 6.
By calculating the accumulated release rate, the quercetin oil phase solution is found to have release rates of 72.35% and 100% at 3h and 24h respectively, and complete release at 24 h. Whereas the quercetin O/W microemulsion prepared in example 4 had release rates of only 35.6% and 47% at 3h and 24h, respectively; the release rate is later and more slow, reaching 58% at 60 h. From this, the above-mentioned O/W microemulsion has a remarkable effect of releasing quercetin.
Test example 3 light stability test of quercetin O/W micro emulsion of the present application
The test method comprises the following steps:
the quercetin O/W microemulsions prepared in examples 4-6 and the quercetin Pi Suyou phase solutions were placed in colorless open glass containers, respectively, at 25deg.C, and placed in the open air for 110 days, respectively, at days 1, 2, 3 and 110, and the content of quercetin was determined by the above method. The relative percentage of quercetin at each of the other measurement points was calculated with the quercetin content at day 0 being 100%, and the results are shown in table 2.
TABLE 2 results of stability investigation of quercetin O/W microemulsion
From Table 2, it can be seen that the quercetin O/W microemulsion of the application can significantly improve the stability of quercetin. In addition, the relative content of quercetin in the quercetin O/W microemulsion prepared in example 4 was always higher than that in the quercetin O/W microemulsions prepared in examples 5 and 6; the O/W microemulsion of example 4 showed better encapsulation of quercetin.
The application provides a food-grade O/W quercetin microemulsion, a preparation method and an application thought and method thereof, and a method for realizing the technical scheme is a plurality of methods and approaches, the above is only a preferred embodiment of the application, and it should be pointed out that a plurality of improvements and modifications can be made by one of ordinary skill in the art without departing from the principle of the application, and the improvements and modifications are also considered as the protection scope of the application. The components not explicitly described in this embodiment can be implemented by using the prior art.
Claims (10)
1. The food-grade O/W quercetin microemulsion is characterized by comprising a blank microemulsion composed of a surfactant, an oil phase solution and an aqueous phase, and quercetin encapsulated by the blank microemulsion as a carrier; the oil phase solution comprises oil and cosurfactant;
the quercetin microemulsion has the following characteristics:
(1) Appearance: transparent or translucent, colorless or pale yellow liquid;
(2) Average particle diameter: 200-300 nm;
(3) pH value: 6.0 to 8.0;
(4) Drug content: 0.4-1.51 mg/g;
(5) Drug release: the accumulated release rate of the quercetin microemulsion is 25-47% within 24 hours.
2. Food grade O/W quercetin microemulsion according to claim 1, wherein the surfactant is any of emulsifier EL-35, tween-80 and emulsifier OP, preferably emulsifier EL-35.
3. Food grade O/W quercetin microemulsion according to claim 1 wherein the oil is selected from any of peanut oil, isopropyl myristate, ethyl butyrate, ethyl n-octanoate, preferably isopropyl myristate.
4. Food grade O/W quercetin microemulsion according to claim 1, wherein the cosurfactant is any of absolute ethanol, polyethylene glycol 400, ethylene glycol, isopropanol, preferably absolute ethanol.
5. The method for preparing the food-grade O/W quercetin microemulsion according to claim 1, wherein the food-grade O/W quercetin microemulsion comprises the following components in percentage by weight: 10% -42% of surfactant, 2% -32% of oil phase solution and the balance of water phase; the oil phase solution consists of isopropyl myristate and ethanol, wherein the weight ratio of the isopropyl myristate to the ethanol=1:1-4.
6. The food-grade O/W quercetin microemulsion according to claim 5, wherein the blank microemulsion comprises the following components in percentage by weight: 30% of surfactant, 20% of oil phase solution and the balance of water phase.
7. The food grade O/W quercetin microemulsion according to claim 5, wherein the oil phase solution is composed of isopropyl myristate and ethanol in a weight ratio of isopropyl myristate to ethanol=1:2.
8. A process for the preparation of food-grade O/W microemulsions according to any of claims 1 to 6, characterized in that it comprises in particular:
under the condition of continuous stirring, adding the surfactant into a mixing kettle according to the weight percentage, then adding the oil phase solution, and finally adding the water phase until the liquid is clear and transparent.
9. The method for producing an O/W microemulsion according to claim 8, wherein the stirring speed is 100rpm to 500rpm, the temperature is 50 to 60℃and the pH is controlled to 6 to 8.
10. Use of the food-grade O/W quercetin microemulsion according to claim 1 as a carrier in food and pharmaceutical applications.
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