CN112056558A - Oil-in-water carotene microemulsion and preparation method thereof - Google Patents

Oil-in-water carotene microemulsion and preparation method thereof Download PDF

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CN112056558A
CN112056558A CN202010992781.2A CN202010992781A CN112056558A CN 112056558 A CN112056558 A CN 112056558A CN 202010992781 A CN202010992781 A CN 202010992781A CN 112056558 A CN112056558 A CN 112056558A
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emulsifier
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water
microemulsion
carotenoid
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赵月春
刘嘉英
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South China Agricultural University
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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Abstract

The invention discloses an oil-in-water carotene microemulsion and a preparation method thereof, wherein the microemulsion comprises 0.5-5% of carotenoid, 3-20% of grease, 0.1-4% of antioxidant, 12-60% of compound emulsifier, 0-0.3% of preservative and the balance of deionized water. The invention replaces the commonly used short-chain alcohol co-emulsifier in the traditional microemulsion preparation by emulsifier compounding, converts fat-soluble carotenoid into a water-soluble preparation through emulsification processing, improves the solubility limit of the carotenoid, prolongs the storage time of functional components in the product, ensures that the prepared carotenoid microemulsion is clear and transparent, has small particle size and concentrated distribution, has good properties, does not delaminate after centrifugation and long-time storage, has stable microemulsion system, can further improve the bioavailability, greatly broadens the application range and meets different production requirements.

Description

Oil-in-water carotene microemulsion and preparation method thereof
[ technical field ] A method for producing a semiconductor device
The invention relates to an oil-in-water carotene microemulsion and a preparation method thereof, belonging to the technical field of food processing.
[ background of the invention ]
Carotenoids are a class of natural pigments that are classified by structural division into hydrocarbons (carotenes) and oxygenated derivatives (xanthophylls). More than 20 carotenoids, such as alpha-carotene, beta-carotene, lycopene, lutein, zeaxanthin, and the like, exist in human blood and tissues. Carotenoids are an important source of dietary vitamin a, mainly found in vegetables such as spinach, carrots, and orange or yellow fruits such as mango and papaya. Because the color of the plant extract is bright and has a wide existing range and a stable and uniform coloring function, a plurality of carotenoids such as beta-carotene, lycopene and the like are internationally recognized excellent natural pigments, almost all carotenoids show the characteristic of eliminating excessive free radicals generated in the life cycle of cells, and the strong antioxidation characteristic enables the carotenoids to show a plurality of functional characteristics in human health, such as antioxidation, body immunity enhancement, cancer incidence reduction, degenerative disease related diseases and the like. Carotenoids are therefore of great interest in many fields such as food, medicine, cosmetics.
Carotenoids have a common chemical structural feature of a polyene chain consisting of 8 isoprene basic units, and constitute a class of compounds or derivatives thereof through conjugated double bonds. The most important part of the carotenoid molecule is the conjugated double bond system that determines biological function and color, but also because of the structural uniqueness, carotenoids are sensitive to light, heat, oxygen, and acid and are susceptible to degradation or isomerization. And carotenoids are generally insoluble in water and soluble in part of the organic agent. The instability and fat-soluble nature of carotenoids has limited their use in water-soluble systems. Therefore, the embedding treatment of the carotenoid to prepare the carotenoid preparation with good water solubility and uniform and stable state is beneficial to wider application.
The carotenoid preparations on the market at present mainly comprise capsules, powder and the like, and the carotenoid preparations are prepared by coating the carotenoid into micro particles by using a film forming material (wall material). Wall materials commonly used in the food industry are proteins, vegetable gums, alginates and chitosan. However, the particle size of the product is usually large, the particle size of many carotenoid microencapsulated preparations is between 0.7 and 5 μm, the requirements of biological utilization are difficult to achieve, the light transmittance of the carotenoid microencapsulated preparations dissolved in water is poor, the carotenoid microencapsulated preparations are formed by external forces such as a homogenizer or ultrasound during preparation, equipment is complex, and the requirements of strong light transmittance, strong coloring power and the like in some fields cannot be met.
Microemulsions are transparent, homogeneous, thermodynamically stable liquid systems composed of water, oil, and an emulsifier. Compared with the common emulsion, the microemulsion has transparent and uniform appearance, can spontaneously form a thermodynamic stable system without acquiring energy from the outside, has the droplet size within 100nm, and has the advantages of uniform and transparent appearance, smaller particle size, greatly improved bioavailability, simple operation and the like compared with other carotenoid preparations.
Common microemulsions are usually prepared from water, oil, emulsifiers, and co-emulsifiers. Coemulsifiers for preparing O/W microemulsions are usually short-chain alcohols such as ethanol, glycerol, etc. According to the national standard of food additives, short-chain alcohol which can be added into food is less in alcohol, glycerol and the like, but the addition of the substances can influence the mouthfeel of the microemulsion, applicable people of the food and the preparation temperature.
[ summary of the invention ]
The invention aims to improve the water-soluble characteristic of the carotenoid, and provides a preparation method of an oil-in-water carotenoid microemulsion which is transparent and uniform in microemulsion system, can be stably dissolved in water, has small particle size and is concentrated.
It is another object of the present invention to provide a process for the preparation of the microemulsion.
The purpose of the invention is realized by the following technical scheme:
an oil-in-water carotenoid microemulsion is characterized by comprising the following components in percentage by mass:
Figure BDA0002691341980000031
the compound emulsifier in the invention is preferably a Tween-Span system emulsifier.
The compound emulsifier in the invention is composed of Span emulsifier and Tween emulsifier, when Tween-Span system emulsifier is mixed for use, a 'compound' is adsorbed on the interface to lead the interface to be arranged tightly and have higher strength, thus achieving the effects of preventing coalescence and increasing the stability of emulsion. When the emulsifiers with similar structures are mixed for use, the synergistic effect is obvious, particularly when one emulsifier is a derivative of another emulsifier, the compound synergistic effect is obvious, and the emulsifying effect of the compounded emulsifier is good.
In the invention, the HLB value range of the Span emulsifier is 1-9, and the HLB value range of the Tween emulsifier is 10-18.
In the invention, the Span emulsifier accounts for 1-15% of the total weight of the microemulsion, and preferably the Span emulsifier accounts for 1-7% of the total weight of the microemulsion; the HLB value of the Span emulsifier is preferably 3-8.
Preferably, the Span-based emulsifier is at least one of sorbitan oleic acid triester (Span85), sorbitol tristearate (Span65), sorbitan oleic acid ester (Span80), sorbitan stearate (Span60), sorbitan monopalmitate (Span40), and sorbitan lauric acid monoester (Span 20).
Further preferably, the Span-based emulsifier is at least one selected from sorbitan oleate (Span80), sorbitan stearate (Span60), sorbitan monopalmitate (Span40), and sorbitan monolaurate (Span 20).
In the invention, the mass ratio of the Span emulsifier with the HLB value of 3-5 to the Span emulsifier with the HLB value of 6-8 in the oil phase is 1: 0.1-10, preferably 1: 0.1-5.
Preferably, the Tween-based emulsifier is at least one of polyoxyethylene sorbitan tristearate (Tween65), polyoxyethylene sorbitan trioleate (Tween85), polyoxyethylene sorbitan monolaurate (Tween21), polyoxyethylene sorbitan monostearate (Tween60), polyoxyethylene sorbitan monooleate (Tween80), polyoxyethylene sorbitan monopalmitate (Tween40), and polyoxyethylene sorbitan laurate (Tween 20).
Further preferably, the Tween-based emulsifier is at least one of polyoxyethylene sorbitan monostearate (Tween60), polyoxyethylene sorbitan monooleate (Tween80), polyoxyethylene sorbitan monopalmitate (Tween40), and polyoxyethylene sorbitan laurate (Tween 20).
The mass ratio of the Tween emulsifier in the microemulsion is 11-45%, and the mass ratio of the Span emulsifier in the microemulsion is 1-15%.
The carotenoid in the invention is at least one of natural, fermented and synthesized beta-carotene, lycopene, lutein ester, zeaxanthin, capsanthin, astaxanthin and curcumin; beta-carotene and lycopene are preferred.
The oil and fat in the present invention include common edible oils such as at least one of corn oil, peanut oil, soybean oil, sunflower oil, olive oil, perilla oil, camellia oil, canola oil, MCT oil (medium chain triglycerides); the oil and fat is more preferably at least one of soybean oil, peanut oil, perilla oil, and MCT oil (medium chain triglyceride). The mass percentage of the oil is more preferably 3-15%.
The antioxidant in the invention is lecithin, ascorbyl palmitate, ascorbic acid and salts thereof, alpha-tocopherol and other esters with antioxidant property; more preferably at least one of lecithin, ascorbyl palmitate, and alpha-tocopherol. The antioxidant is more preferably 0.1 to 1% by mass.
Preferably, the oil-in-water carotene microemulsion is characterized by comprising the following components in percentage by mass:
Figure BDA0002691341980000051
wherein the carotenoid is preferably one of beta-carotene, lycopene and astaxanthin; the compound emulsifier is selected from sorbitan oleate, sorbitan monostearate, sorbitan monolaurate, sorbitan monopalmitate, polyoxyethylene sorbitan monooleate, and polyoxyethylene sorbitan monopalmitate.
The preservative in the invention is sorbic acid and salts thereof.
A preparation method of oil-in-water carotenoid microemulsion is characterized by comprising the following steps:
a. mixing oil phase components in the microemulsion components, and melting at high temperature until no crystal exists to obtain a molten oil phase solution;
b. heating and stirring a Tween emulsifier in the microemulsion component in a water bath until a uniform and stable surfactant phase solution is formed;
c. heating and stirring the water phase components in the microemulsion component in a water bath until a uniform and stable water phase solution is formed;
d. and adding the oil phase solution into the surfactant phase, stirring the mixture under the condition of water bath at the temperature of 60-90 ℃ until the solution is uniformly mixed, adding the water phase solution into the mixture, and stirring the mixture for 10-30 min at the temperature of 60-90 ℃ until the mixture is transparent.
The oil phase comprises a water-insoluble substance and a Span emulsifier, the HLB value of the Span emulsifier is 1-9, the Span emulsifier has lipophilicity, the oil and a hydrophilic emulsifier with a higher HLB value are easily combined more tightly, and the oil phase can be used as a cosurfactant in the preparation of common microemulsion. Lipophilic carotenoids are melted in oil by means of high temperature heating and combined with emulsifiers of low HLB value to form the desired oil phase.
The oil phase in the invention comprises grease, carotenoid, an emulsifier with HLB value of 3-9 and an antioxidant, the surfactant phase comprises an emulsifier with HLB value of 10-18, and the water phase comprises a preservative and deionized water.
The melting temperature of the oil phase is preferably 180-220 ℃, and the heating temperature of the surfactant phase and the heating temperature of the water phase are both 60-90 ℃.
In the invention, the preparation temperature of the oil phase reaches the melting point of the carotenoid, so that the carotenoid is changed into a molten amorphous state from a crystal, and a Tween-Span system emulsifier generates a synergistic effect, so that the emulsifying effect is more obvious, the raw materials are better coated, and the particle size of the formed emulsion is smaller and uniform.
Compared with the prior art, the invention has the following advantages:
the invention replaces the common short-chain alcohol co-emulsifier in the traditional microemulsion preparation by emulsifier compounding, converts the fat-soluble carotenoid into a water-soluble preparation through emulsification processing, improves the solubility limit of the carotenoid and prolongs the storage time of functional components in the product.
The carotenoid microemulsion prepared by the invention is clear and transparent, makes up the defect of poor light transmission of the traditional water-soluble carotenoid preparation, and can be used as a coloring agent or a functional component to be added into a beverage without influencing the quality of the beverage; in addition, the particle size is small, the distribution is concentrated, the property is good, layering does not occur after centrifugation and long-time storage, the microemulsion system is stable, the bioavailability can be further improved, and the application range of the microemulsion system is greatly widened to meet different production requirements.
The carotenoid micro-emulsion system prepared by the invention does not contain short-chain alcohol such as ethanol, glycerol and the like, does not influence the taste of the beverage when added into the beverage, and widens the applicable population.
[ description of the drawings ]
FIG. 1 is a graph of the particle size distribution of the microemulsion of example 1 having a beta-carotene content of 1 wt%;
FIG. 2 is a particle size distribution plot of the microemulsion of example 2 having an astaxanthin content of 1 wt%;
FIG. 3 is a particle size distribution diagram of the microemulsion of example 3 having a lycopene content of 1 wt%;
FIG. 4 is a particle size distribution diagram of a microemulsion containing 1 wt% of beta-carotene of comparative example 1;
FIG. 5 is a particle size distribution diagram of the microemulsion of comparative example 2 having a beta-carotene content of 1 wt%.
[ detailed description ] embodiments
An oil-in-water carotenoid microemulsion comprises the following components in percentage by mass:
Figure BDA0002691341980000081
wherein the compound emulsifier is a Tween-Span system emulsifier;
the preparation method of the oil-in-water carotenoid microemulsion comprises the following steps:
a. mixing oil phase component grease in the microemulsion component, carotenoid, an emulsifier with an HLB value of 3-9 and an antioxidant, heating, stirring and melting at 180-220 ℃ until no crystal exists, and obtaining an oil phase solution;
b. heating and stirring an HLB (hydrophile-lipophile balance) 10-18 emulsifier in the microemulsion component in a water bath at 60-90 ℃ until a uniform and stable surfactant phase solution is formed;
c. heating and stirring the water phase components in the microemulsion component in a water bath at 60-90 ℃ until a uniform and stable water phase solution is formed;
d. and adding the oil phase solution into the surfactant phase, stirring the mixture under the condition of water bath at the temperature of 60-90 ℃ until the solution is uniformly mixed, adding the water phase solution into the mixture, and stirring the mixture for 10-30 min at the temperature of 60-90 ℃ until the mixture is transparent.
The present invention will be described in further detail with reference to specific examples.
Example 1: the mass percentages of the components are shown in table 1.
Table 1: the content unit of each component is wt%
Composition (I) Content (wt.) Composition (I) Content (wt.) Composition (I) Content (wt.)
Soybean oil 3 Alpha-tocopherol 0.1 Tween80 20
Beta-carotene crystals 1 Span80 2 Potassium sorbate 0.08
Ascorbyl palmitate 0.2 Span40 1 Deionized water Balance of
The preparation method comprises the following steps:
mixing soybean oil, beta-carotene crystals, sorbitan oleate (span80), sorbitan monopalmitate (span40), ascorbyl palmitate and alpha-tocopherol, heating and stirring in an oil bath kettle at 180 ℃ until no crystals exist, and obtaining an oil phase solution 1;
heating and stirring emulsifier polyoxyethylene sorbitan monooleate (Tween80) in water bath at 70 ℃ to form uniform and stable surfactant phase solution 2;
mixing deionized water and potassium sorbate, heating in 70 ℃ water bath, and stirring to form a uniform water phase solution 3;
and pouring the oil phase solution 1 into a surfactant phase solution 2 in the 70 ℃ water bath constant-temperature magnetic stirring process, continuously stirring for 5min until the solution is uniformly mixed, adding the water phase solution 3 into the mixed solution, and stirring for 10-30 min under the 70 ℃ water bath constant-temperature magnetic stirring process to obtain the microemulsion with the beta-carotene content of 1 wt%.
The prepared microemulsion is clear, transparent and good in flowability, the average particle size is 15.00 +/-0.7 nm, the PDI value is 0.24 +/-0.2, the particle size distribution of the prepared emulsion is uniform, and the measured particle size distribution diagram is shown in figure 1. The demixing phenomenon does not occur after 30min of 8000r/min centrifugation.
Example 2: the mass percentages of the components are shown in table 2.
Table 2:
composition (I) Content (wt%) Composition (I) Content (wt%)
MCT oil 3 Span40 1
Astaxanthin crystals 1 Tween80 12.5
Span60 2 Tween40 12.5
Ascorbyl palmitate 0.2 Potassium sorbate 0.08
Alpha-tocopherol 0.1 Deionized water Balance of
The preparation method comprises the following steps:
mixing MCT oil, astaxanthin crystals, sorbitan monostearate (span60), sorbitan monopalmitate (span40), ascorbyl palmitate and alpha-tocopherol, heating and stirring in an oil bath kettle at 220 ℃, and melting until no crystals exist to obtain a solution 1;
heating and stirring emulsifier polyoxyethylene sorbitan monooleate (Tween80) and polyoxyethylene sorbitan monopalmitate (Tween40) in water bath at 70 ℃ to form uniform stable solution 2;
mixing deionized water and potassium sorbate, heating in a water bath at 70 ℃, and stirring to form a uniform solution 3;
pouring the solution 1 into a solution 2 in the 70 ℃ water bath constant-temperature magnetic stirring, continuously stirring for 5min until the solution is uniformly mixed, adding the solution 3 into the mixed solution, and stirring for 10-30 min under the 70 ℃ water bath constant-temperature magnetic stirring to obtain the microemulsion with the astaxanthin content of 1 wt%.
The prepared microemulsion is clear, transparent and good in flowability, the average particle size is 17.50 +/-0.05 nm, the PDI value is 0.22 +/-0.06, the particle size distribution of the prepared emulsion is uniform, and the measured particle size distribution diagram is shown in figure 2. The demixing phenomenon does not occur after 30min of 8000r/min centrifugation.
Example 3: the mass percentages of the components are shown in table 3.
Table 3: the content unit of each component is wt%
Composition (I) Content (wt.) Composition (I) Content (wt.) Composition (I) Content (wt.)
Perilla oil 3 Alpha-tocopherol 0.1 Tween80 22
Lycopene crystal 1 Span80 1.5 Potassium sorbate 0.08
Ascorbyl palmitate 0.2 Span20 0.8 Deionized water Balance of
The preparation method comprises the following steps:
mixing perilla oil, lycopene crystal, sorbitan oleate (span80), sorbitan monolaurate (span20), ascorbyl palmitate and alpha-tocopherol, heating and stirring in a 185 ℃ oil bath kettle until no crystal exists, and obtaining a solution 1;
heating and stirring emulsifier polyoxyethylene sorbitan monooleate (Tween80) in water bath at 70 ℃ to form uniform stable solution 2;
mixing deionized water and potassium sorbate, heating in a water bath at 70 ℃, and stirring to form a uniform solution 3;
pouring the solution 1 into a solution 2 in the 70 ℃ water bath constant-temperature magnetic stirring process, continuously stirring for 5min until the solution is uniformly mixed, adding the solution 3 into the mixed solution, and stirring for 10-30 min under the 70 ℃ water bath constant-temperature magnetic stirring process to obtain the microemulsion with the lycopene content of 1 wt%.
The prepared microemulsion is clear, transparent and good in flowability, the average particle size is 20.00 +/-0.8 nm, the PDI value is 0.23 +/-0.05, the particle size distribution of the prepared emulsion is uniform, the measured particle size distribution diagram is shown in figure 3, and no layering phenomenon occurs after centrifugation at 8000r/min for 30 min.
Example 4: the mass percentages of the components are shown in table 4.
Table 4: the content unit of each component is wt%
Composition (I) Content (wt.) Composition (I) Content (wt.)
Soybean oil 3 Span40 0.5
Beta-carotene crystals 0.5 Tween80 11.2
Span80 0.3 Deionized water Balance of
Ascorbyl palmitate 0.2 Potassium sorbate 0.08
Alpha-tocopherol 0.1
The preparation method comprises the following steps:
mixing soybean oil, beta-carotene crystals, sorbitan oleate (span80), sorbitan monopalmitate (span40), ascorbyl palmitate and alpha-tocopherol, and stirring and melting at high temperature in an oil bath kettle at 180 ℃ until no crystals exist to obtain a solution 1;
heating emulsifier polyoxyethylene sorbitan monooleate (Tween80) in water bath at 70 deg.C to obtain solution 2;
mixing deionized water and potassium sorbate, heating in 70 ℃ water bath, and stirring to form a uniform solution 3;
pouring the solution 1 into a solution 2 in the 70 ℃ water bath constant-temperature magnetic stirring, continuously stirring for 5min until the solution is uniformly mixed, adding a solution 3 into the mixed solution, and stirring for 10-30 min under the 70 ℃ water bath constant-temperature magnetic stirring to obtain the microemulsion with the beta-carotene content of 0.5 wt%.
The prepared microemulsion is clear, transparent and good in flowability, the average particle size is less than 20nm, and the particle size distribution of the prepared emulsion is proved to be uniform by the PDI value of less than 0.2. The demixing phenomenon does not occur after 30min of 8000r/min centrifugation.
Example 5: the mass percentages of the components are shown in table 5.
Table 5: the content unit of each component is wt%
Composition (I) Content (wt.) Composition (I) Content (wt.)
MCT oil 15 Span40 10
Astaxanthin crystals 5 Tween80 45
Span80 5 Deionized water Balance of
Ascorbyl palmitate 2 Potassium sorbate 0.8
Alpha-tocopherol 1
The preparation method comprises the following steps:
mixing MCT oil, astaxanthin crystals, sorbitan monooleate (span80), sorbitan monopalmitate (span40), ascorbyl palmitate and alpha-tocopherol, stirring and melting at a high temperature in an oil bath kettle at 220 ℃ until no crystals exist to obtain a solution 1;
heating and stirring emulsifier polyoxyethylene sorbitan monooleate (Tween80) in water bath at 70 ℃ to form uniform stable solution 2;
mixing deionized water and potassium sorbate, heating in 70 deg.C water bath, and stirring to obtain uniform solution 3;
pouring the solution 1 into a solution 2 in the 70 ℃ water bath constant-temperature magnetic stirring process, continuously stirring for 5min until the solution is uniformly mixed, adding the solution 3 into the mixed solution, and stirring for 10-30 min under the 70 ℃ water bath constant-temperature magnetic stirring process to obtain the microemulsion with the astaxanthin content of 5 wt%.
The prepared microemulsion is clear, transparent and good in flowability, the average particle size is less than 50nm, and the PDI value is less than 0.3, so that the prepared emulsion is the microemulsion. The microemulsion is not layered after being centrifuged for 30min at 8000 r/min.
Comparative example 1: the mass percentages of the components are shown in table 6.
Table 6: the content unit of each component is wt%
Composition (I) Content (wt.) Composition (I) Content (wt.)
Soybean oil 3 Glyceryl monostearate 0.8
Beta-carotene crystals 1 Decaglycerol monolaurate 20
Ascorbyl palmitate 0.2 Potassium sorbate 0.08
Alpha-tocopherol 0.1 Deionized water Balance of
Glyceryl monooleate 0.6
The preparation method comprises the following steps:
mixing soybean oil, beta-carotene crystals, glyceryl monooleate, ascorbyl palmitate and alpha-tocopherol, heating, stirring and melting in an oil bath kettle at 180 ℃ until no crystals exist to obtain a solution 1;
heating and stirring emulsifier decaglycerol monolaurate in water bath at 70 ℃ to form a solution 2;
mixing deionized water and potassium sorbate, heating in a water bath at 70 ℃, and stirring to form a solution 3;
pouring the solution 1 into a solution 2 in the 70 ℃ water bath constant-temperature magnetic stirring, continuously stirring for 5min until the solution is uniformly mixed, adding the solution 3 into the mixed solution, and stirring for 10-30 min under the 70 ℃ water bath constant-temperature magnetic stirring to obtain the microemulsion with the beta-carotene content of 1 wt%.
The prepared sample is orange-red opaque emulsion with slightly poor fluidity, the average particle size is 1759nm, the PDI value is 0.9 +/-0.05, no microemulsion can be formed, and the measured particle size distribution diagram is shown in figure 4. The layering phenomenon occurs after 30min of 8000r/min centrifugation.
Comparative example 2: the mass percentages of the components are shown in table 7.
Table 7: the content unit of each component is wt%
Composition (I) Content (wt.) Composition (I) Content (wt.)
Soybean oil 3 Driver's cab40 1
Beta-carotene crystals 1 Tween80 20
Ascorbyl palmitate 0.2 Potassium sorbate 0.08
Alpha-tocopherol 0.1 Deionized water Balance of
Span80 2
The preparation method comprises the following steps:
mixing soybean oil, beta-carotene crystals, sorbitan oleate (span80), sorbitan monopalmitate (span40), ascorbyl palmitate and alpha-tocopherol, heating and stirring in an oil bath kettle at 140 ℃ to obtain an oil phase solution 1;
heating and stirring emulsifier polyoxyethylene sorbitan monooleate (Tween80) in water bath at 70 ℃ to form uniform and stable surfactant phase solution 2;
mixing deionized water and potassium sorbate, heating in 70 ℃ water bath, and stirring to form a uniform solution 3;
and pouring the oil phase solution 1 into a surfactant phase solution 2 in the 70 ℃ water bath constant-temperature magnetic stirring process, continuously stirring for 5min until the solution is uniformly mixed, adding the water phase solution 3 into the mixed solution, and stirring for 10-30 min under the 70 ℃ water bath constant-temperature magnetic stirring process to obtain the microemulsion with the beta-carotene content of 1 wt%.
The prepared emulsion has red crystals floating on the surface, a large amount of suspended crystals are arranged on the upper clear layer of the lower layer liquid after centrifugation at 8000r/min for 30min, and partial precipitates are arranged at the bottom of a centrifuge tube. The average particle size is 210 +/-0.7 nm, the PDI value is 0.35 +/-0.2, and the prepared sample is proved to have poor effect, uneven particle size distribution and partial crystals which cannot form microemulsion. The distribution of the measured particle size is shown in FIG. 5.

Claims (10)

1. An oil-in-water carotenoid microemulsion is characterized by comprising the following components in percentage by mass:
Figure FDA0002691341970000011
2. the oil-in-water carotenoid microemulsion according to claim 1, wherein said compound emulsifier is a Tween-Span system emulsifier.
3. The oil-in-water carotenoid microemulsion according to claim 2, wherein the compound emulsifier is composed of Span emulsifier with HLB value of 1-9 and Tween emulsion with HLB value of 10-18.
4. The oil-in-water carotenoid microemulsion according to claim 3, wherein the built emulsifier comprises 11-45% of Tween emulsifier and 1-15% of Span emulsifier.
5. The oil-in-water carotenoid microemulsion according to claim 3, wherein the mass ratio of the Span emulsifier with HLB value of 3-5 to the Span emulsifier with HLB value of 6-8 is 1: 0.1-10.
6. The oil-in-water carotenoid microemulsion according to claim 3, wherein said Span-like emulsifier is at least one of sorbitan oleic acid triester, sorbitan tristearate, sorbitan oleate, sorbitan stearate, sorbitan monopalmitate, sorbitan monolaurate.
7. The oil-in-water carotenoid microemulsion according to claim 3 wherein said Tween-type emulsifier is at least one of polyoxyethylene sorbitan tristearate, polyoxyethylene sorbitan trioleate, polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan monopalmitate, polyoxyethylene sorbitan laurate.
8. A process for the preparation of an oil-in-water carotenoid microemulsion according to any of claims 1-7, characterized in that it comprises the following steps:
a. mixing oil phase components in the microemulsion components, and melting at high temperature until no crystal exists to obtain a molten oil phase solution;
b. heating and stirring a Tween emulsifier in the microemulsion component in a water bath until a uniform and stable surfactant phase solution is formed;
c. heating and stirring the water phase components in the microemulsion component in a water bath until a uniform and stable water phase solution is formed;
d. and adding the oil phase solution into the surfactant phase, stirring the mixture under the condition of water bath at the temperature of 60-90 ℃ until the solution is uniformly mixed, adding the water phase solution into the mixture, and stirring the mixture for 10-30 min at the temperature of 60-90 ℃ until the mixture is transparent.
9. The method of claim 8, wherein said oil phase comprises lipids, carotenoids, emulsifiers with HLB value ranging from 3 to 9 and antioxidants, said surfactant phase comprises emulsifiers with medium HLB value ranging from 10 to 18, and said aqueous phase comprises preservatives and deionized water.
10. A process according to claim 8, wherein the oil phase has a melting temperature of 180 to 220 ℃.
CN202010992781.2A 2020-09-21 2020-09-21 Oil-in-water carotene microemulsion and preparation method thereof Pending CN112056558A (en)

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