CN118203113A - Composite antarctic krill oil gel and preparation method thereof - Google Patents
Composite antarctic krill oil gel and preparation method thereof Download PDFInfo
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- Jellies, Jams, And Syrups (AREA)
Abstract
The application discloses a composite antarctic krill oil gel and a preparation method thereof, and belongs to the technical field of gel preparation. The gel comprises the following components in parts by mass: 2-5% amidated pectin aerogel template, 95-98% krill peptide capillary suspension. According to the preparation method, the antarctic krill oil gel is prepared by a composite method, and the aerogel template method and the capillary suspension are combined, so that the preparation method has high mechanical strength, can regulate the rheological property of the antarctic krill oil gel, is mild in preparation process conditions, does not influence krill oil and loaded active substances, is stable in property and good in biodegradability, and is an ideal carrier.
Description
Technical Field
The application belongs to the technical field of gel preparation, and particularly relates to a composite antarctic krill oil gel, a preparation method and application thereof.
Background
The antarctic krill oil is used as an emerging high-quality Omega-3 fatty acid source and has wide application in the industries of foods, health-care foods, biological medicines and the like. The compound contains rich phospholipid n-3 polyunsaturated fatty acid and astaxanthin, and has been proved to have good antioxidant and anti-inflammatory effects in various researches. Although antarctic krill oil has been available as a health food in a variety of soft capsule products, a single dosage form limits the use of antarctic krill oil.
Oleogel is a gel formed by immobilizing an oil phase through a three-dimensional network structure formed by organogelators. Research on oleogel is currently focused mainly on the fields of foods, medicines and cosmetics, as a substitute for saturated fatty acids, to load volatile components, to promote skin penetration of nonpolar compounds, or as a raw material for 3D printed foods. The physical properties of the euphausia superba oil gel can be changed by developing the euphausia superba oil gel, the loading capacity of water-soluble substances is increased, and the euphausia superba oil gel can meet the requirements of different application scenes. Among the methods for preparing oleogels, aerogel templating has received attention in recent years.
Aerogels have a highly porous structure, a complex three-dimensional network, and a large specific surface area. The use of aerogel to prepare oleogel can provide higher oil absorption and retention capacity, the aerogel being converted to oleogel by adsorption of krill oil by surface tension and capillary forces. Aerogel production and transport is more cost effective than pre-mixed oil gels, and aerogel templating is more suitable for loading heat sensitive materials because it involves only physical processes.
Capillary suspensions may be created by adding a small amount of an immiscible secondary fluid (e.g., water) to a suspension of particles dispersed in a primary fluid (e.g., oil), with agitation causing the particles to bind together by capillary forces to form a spatial network. The capillary suspension has adjustable rheological property, and the mechanical property of the oleogel prepared by the capillary suspension is easier to regulate and control so as to meet the use requirements of different scenes.
At present, researches on preparing antarctic krill oil gel by using an amidated pectin aerogel template and krill peptide capillary suspension are freshly reported, and the invention can provide technical support for the research and application in the field.
Disclosure of Invention
In order to solve the problems, the invention provides the compound euphausia superba oil gel and the preparation method thereof, wherein the euphausia superba oil gel is prepared by the compound method, and the aerogel template method and the capillary suspension are combined, so that the euphausia superba oil gel has higher mechanical strength, can regulate the rheological property, has mild preparation process conditions, does not influence the euphausia superba oil and loaded active substances, has stable properties and good biodegradability, and is an ideal carrier.
The invention provides a composite antarctic krill oil gel, which comprises the following components in parts by weight: 2-5% amidated pectin aerogel template, 95-98% krill peptide capillary suspension.
Optionally, the gel comprises the following components in parts by weight: 2-3% amidated pectin aerogel template, 97-98% krill peptide capillary suspension.
Optionally, the amidated pectin aerogel template is prepared by taking tertiary butanol aqueous solution as a solvent and freeze-drying the amidated pectin solution.
Optionally, the krill peptide capillary suspension is prepared by constructing a ternary liquid/solid system by taking krill peptide as suspended particles, taking antarctic krill oil as a first solvent and taking pure water as a second solvent.
The invention also provides a preparation method of the compound antarctic krill oil gel, which comprises the following steps:
(1) Adding the amidated pectin solution into a tertiary butanol aqueous solution to obtain a mixed solution;
(2) Crosslinking the mixed solution in the step (1) for 3-6 hours, then pre-freezing, and then freeze-drying for 30-40 hours to obtain an amidated pectin aerogel template;
(3) Adding 10-30wt% of krill peptide into the euphausia superba oil, homogenizing and shearing uniformly, and immersing the amidated pectin aerogel template obtained in the step (2) into the euphausia superba oil to obtain an oil phase system;
(4) Adding pure water with the mass fraction of 0.2-0.3wt% into the oil phase system in the step (3), and homogenizing and shearing uniformly to obtain the composite antarctic krill oil gel.
Optionally, the amidated pectin solution has a pH of 3.5-4.5 and a weight percentage of 1-3wt%.
Alternatively, the volume of the tertiary butanol aqueous solution is the same as that of the amidated pectin solution, and the tertiary butanol aqueous solution contains 60-80% v/v tertiary butanol and 1-3wt% Zn 2+.
Optionally, the pre-freezing condition of the step (2) is that the mixed solution is pre-frozen at a temperature of between-30 ℃ and-40 ℃ until the mixed solution is completely solidified.
Optionally, the condition of the step (3) of homogenizing and shearing is homogenizing for 10-15min under the condition of 1500-2500rpm, and the condition of the step (4) of homogenizing and shearing is homogenizing for 10-15min under the condition of 1500-2500 rpm.
The invention also provides a compound antarctic krill oil gel and/or application of the compound antarctic krill oil gel prepared by the preparation method of the compound antarctic krill oil gel in preparation of food, health-care food or drug carriers.
The beneficial effects of the application include, but are not limited to:
1. The composite antarctic krill oil gel provided by the application is prepared by adopting an aerogel template method, has higher oil absorption and oil holding performance and higher mechanical strength, and does not need complex organic solvents in the preparation process;
2. the compound antarctic krill oil gel provided by the application has the potential of forming high-strength hydrogel under the minimum limiting condition, and the requirement on the gel forming condition can be reduced in the process of preparing the aerogel template;
3. according to the compound euphausia superba oil gel, the tertiary butanol aqueous solution is used as a solvent in the preparation process of the amidated pectin aerogel template, so that the hydrophobic interaction between pectin chains is enhanced, the compound euphausia superba oil gel is more volatile during freeze-drying, and the freeze-drying efficiency is improved;
4. according to the compound euphausia superba oil gel provided by the application, euphausia superba peptide is used as water-soluble particles, and can be preferentially combined with a small amount of water in oil to form a three-dimensional network connected with capillary bridges, so that the rheological property of the oil gel is easy to adjust;
5. the preparation method of the compound antarctic krill oil gel provided by the application is simple and has strong universality, and the direction of application of antarctic krill oil in the field of medicines and foods is expanded.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute a limitation on the application. In the drawings:
Fig. 1 is a schematic view of the oil absorption properties of a composite antarctic krill oil gel according to examples and comparative examples of the present application.
Fig. 2 is a schematic illustration of the oil retention of the composite antarctic krill oleogel according to examples and comparative examples of the present application.
Detailed Description
In order to more clearly illustrate the general inventive concept, a detailed description is given below by way of example.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those described herein, and therefore the scope of the present invention is not limited to the specific embodiments disclosed below.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. In the description of the present specification, a description referring to the terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Hereinafter, the composite antarctic krill oil gel of the present invention and the preparation method thereof will be described in detail with reference to exemplary embodiments.
The invention provides a composite antarctic krill oil gel which comprises the following components in parts by weight: 2-5% amidated pectin aerogel template, 95-98% krill peptide capillary suspension. Further, the gel comprises the following components in parts by weight: 2-3% amidated pectin aerogel template, 97-98% krill peptide capillary suspension.
In one exemplary embodiment of the invention, the preparation method of the composite antarctic krill oil gel provided by the invention comprises the following steps:
(1) Adding amidated pectin solution with pH value of 3.5-4.5 and weight percentage of 1-3wt% into tert-butanol water solution with equal volume to obtain mixed solution.
Specifically, the aqueous t-butanol solution contains 60-80% v/v t-butanol and 1-3wt% Zn 2+ by weight. Tertiary butanol has the characteristics of high freezing point, high vapor pressure, low toxicity and the like, is easier to sublimate, and can improve the freeze-drying efficiency. In addition, tertiary butanol is added into the aqueous solution, needle crystals can be formed when freezing, the surface area is increased, and meanwhile, tubular channels left after ice crystal sublimation are beneficial to the flow of water vapor and accelerate drying. The solution proportion ensures that amidated pectin is fully crosslinked into gel, and simultaneously shortens the freeze-drying time and reduces the cost.
(2) And (3) crosslinking the mixed solution in the step (1) for 3-6 hours, then pre-freezing, and then freeze-drying for 30-40 hours to obtain the amidated pectin aerogel template.
In particular, pectin can crosslink with divalent metal ions under such conditions to form a gel. Pre-freezing after sufficient cross-linking, wherein the pre-freezing condition is that the mixed solution is pre-frozen at the temperature of minus 30 ℃ to minus 40 ℃ until the mixed solution is completely solidified. If the pre-freezing temperature is too low, energy waste can be caused; if the pre-freezing temperature is above-30 ℃, the solidified eutectic point can be reached, but in order to enable the gel to form a structurally stable ice crystal structure at a relatively rapid cooling rate, the pre-freezing temperature is between-30 ℃ and-40 ℃, and the set freeze-drying time can ensure the gel to be fully sublimated, so that the solvent residue is reduced.
(3) The krill peptide with the mass fraction of 10-30wt% is added into the euphausia superba oil, and homogenized for 10-15min under the condition of 1500-2500rpm, so that the krill peptide has better antioxidation capability, can remove free radicals, reduce the oxidative damage of the organism, can lighten the oxidation of the krill oil, improve the stability of the oil gel, and can be fully mixed with the euphausia superba oil when homogenized under the condition. And (3) immersing the amidated pectin aerogel template obtained in the step (2) into antarctic krill oil to obtain an oil phase system.
(4) Adding 0.2-0.3wt% of pure water into the oil phase system in the step (3), homogenizing for 10-15min under the condition of 1500-2500rpm, wherein the water is combined with hydrophilic particles preferentially, and a three-dimensional network structure connected by taking water as a capillary bridge is formed in an oil solvent after uniform mixing, so that the compound antarctic krill oil gel is obtained.
The present application prepares antarctic krill oil gel by using an amidated pectin aerogel template and a krill peptide capillary suspension. Amidated pectin is prepared through converting partial methyl ester into amide radical in the preparation process of high ester pectin, and has less required bivalent metal ion, less pre-gel, high heat reversibility and the potential of forming high strength hydrogel in minimum limiting condition. The compound antarctic krill oil gel disclosed by the application has the advantages of simple preparation method, high mechanical strength, good oil absorption, good oil retention and the like, can be used as a carrier to load various functional substances, and widens the application direction of antarctic krill oil.
Example 1
The preparation method adopted by the embodiment prepares the compound antarctic krill oil gel, which comprises the following specific steps:
(1) Adding 2wt% amidated pectin solution with pH of 4.0 to an equal volume of tertiary butanol aqueous solution containing 80% v/v tertiary butanol and 2wt% (relative to amidated pectin) of Zn2+;
(2) After the solution is crosslinked for 4 hours, the solution is placed at the temperature of minus 40 ℃ to be pre-frozen until the solution is completely solidified, and then freeze-drying is carried out for 36 hours, so as to obtain an aerogel template;
(3) Adding 20wt% of krill peptide into the antarctic krill oil, homogenizing and shearing uniformly at 2000rpm, and then immersing the obtained aerogel template into the antarctic krill oil to replace a solvent with an oil phase;
(4) Adding 0.2wt% of pure water into the system (3), homogenizing and shearing uniformly at 2000rpm, and connecting suspended krill peptide particles into a three-dimensional network through a water capillary bridge to obtain antarctic krill oil gel.
Example 2
The preparation method adopted by the embodiment prepares another compound antarctic krill oil gel, and comprises the following specific steps:
(1) Adding 1wt% amidated pectin solution with pH of 4.0 to an equal volume of tertiary butanol aqueous solution containing 60% v/v tertiary butanol and 1wt% (relative to amidated pectin) of Zn2+;
(2) After the solution is crosslinked for 4 hours, the solution is placed at the temperature of minus 40 ℃ to be pre-frozen until the solution is completely solidified, and then freeze-drying is carried out for 36 hours, so as to obtain an aerogel template;
(3) Adding 10wt% of krill peptide into the antarctic krill oil, homogenizing and shearing uniformly at 2000rpm, and then immersing the obtained aerogel template into the antarctic krill oil to replace a solvent with an oil phase;
(4) Adding 0.2wt% of pure water into the system (3), homogenizing and shearing uniformly at 2000rpm, and connecting suspended krill peptide particles into a three-dimensional network through a water capillary bridge to obtain antarctic krill oil gel.
Example 3
The preparation method adopted by the embodiment prepares another compound antarctic krill oil gel, and comprises the following specific steps:
(1) Adding 3wt% amidated pectin solution with pH of 4.0 to an equal volume of tertiary butanol aqueous solution containing 70% v/v tertiary butanol and 3wt% (relative to amidated pectin) of Zn2+;
(2) After the solution is crosslinked for 4 hours, the solution is placed at the temperature of minus 40 ℃ to be pre-frozen until the solution is completely solidified, and then freeze-drying is carried out for 36 hours, so as to obtain an aerogel template;
(3) Adding 30wt% of krill peptide into the antarctic krill oil, homogenizing and shearing uniformly at 2000rpm, and then immersing the obtained aerogel template into the antarctic krill oil to replace a solvent with an oil phase;
(4) Adding 0.3wt% of pure water into the system (3), homogenizing and shearing uniformly at 2000rpm, and connecting suspended krill peptide particles into a three-dimensional network through a water capillary bridge to obtain antarctic krill oil gel.
Comparative example 1
This comparative example a comparative antarctic krill oil gel was prepared using the same preparation as in example 1, except that: in step (1), the amidated pectin is replaced by high-ester pectin.
Comparative example 2
This comparative example another comparative antarctic krill oil gel was prepared using the same preparation method as in example 1, except that in example 1: ethanol is used to replace tert-butanol in step (1).
Comparative example 3
This comparative example another comparative antarctic krill oil gel was prepared using the same preparation method as in example 1, except that in example 1: starch is used to replace krill peptide in step (3).
1. Measurement of oil absorption
The method for measuring the oil absorption comprises the following steps: aerogel templates were weighed and immersed in antarctic krill oil mixed with krill peptide or starch according to the methods of preparation of each example and comparative example. After sufficient oil absorption, residual oil on the oleogel surface is removed. The resulting oleogel was immediately weighed and the oil absorption was calculated using the following formula: oil absorption= (weight of oil gel produced-initial weight of aerogel)/initial weight of aerogel. The results of the oil absorption test are shown in FIG. 1.
As shown in FIG. 1, the oil absorption of each example was about 50g/g, and the oil absorption of comparative example 1 was the lowest, which was only 28.6g/g. Since the oil is stored in the interstices of the aerogel network after the aerogel is converted to an oil gel, the pore size of the aerogel determines the oil absorption capacity of the aerogel. Comparative example 1 replaces amidated pectin with high ester pectin, which has high requirement on the gelling condition, and can not effectively form gel under the same condition, so the oil absorption is poor. In comparative example 2, ethanol is used for replacing tertiary butanol, the tertiary butanol has the function of enhancing hydrophobic interaction among pectin chains, so that the pectin chains are easier to gel, and meanwhile, the tertiary butanol has higher vapor pressure and lower melting volume, so that the freeze-drying efficiency can be improved, and the problems of collapse of an aerogel structure and the like are prevented; therefore, the aerogel of the embodiment has more perfect structure and stronger oil absorption after freeze-drying.
2. Measurement of oil holdability
The method for measuring the oil retention comprises the following steps: the samples of antarctic krill oil gel prepared in each example and comparative example were weighed and placed between two pieces of oil absorbing paper. Subsequently, they were placed in centrifuge tubes. The antarctic krill oil gel was then centrifuged at 8000rpm for 15 minutes. The oil retention was calculated using the following formula: oil retention (%) = mass of oleogel after centrifugation/mass of oleogel before centrifugation x 100%. The results of the oil retention test are shown in FIG. 2.
As shown in FIG. 2, the oil retention of the antarctic krill oil gel prepared in each example was about 50%, with comparative example 1 being the lowest, only 23.1%, and comparative example 2 being 27.9%. Since the combination of oil in an aerogel relies on capillary action and surface tension, the greater the capillary force, the higher the oil retention of the aerogel. Comparative example 1 has a low oil binding capacity due to a low degree of crosslinking, a large gap inside the gel, and a small capillary force; while comparative example 2 has an influence on its oil holding performance due to collapse of the structure. The aerogel of comparative example 3 was prepared in the same manner as in example 1, but the final overall oil retention was reduced because the starch was less tightly bound to water than the krill peptide.
3. Viscosity measurement
The viscosity measurement method comprises the following steps: the viscosity was measured separately for the antarctic krill oil gels prepared in each example and comparative example using a rotary viscometer at 25 ℃. The results of the viscosity test obtained are shown in Table 1.
TABLE 1 results of viscosity test
The viscosity of the antarctic krill oil gel is determined by both the properties of the aerogel and the properties of the capillary suspension, as shown in table 1, each example shows a better viscosity, whereas the viscosity of the comparative example is significantly lower than that of the example. Comparative examples 1 and 2 do not provide effective support for the structure of the antarctic krill oil gel because of the poor performance of the aerogel. Comparative example 3 uses starch instead of krill peptide, because starch is less hydrophilic than krill peptide, the resulting capillary suspension has lower strength and is less effective in improving the mechanical properties of the oleogel than krill peptide.
4. Determination of storage stability
The storage stability measurement method comprises the following steps: the antarctic krill oil gel prepared in each example and comparative example was monitored for the content of main nutrients by placing 1g of the antarctic krill oil gel at 25+ -2deg.C and 60+ -5% humidity, and samples were taken every 3 months until the end of month 12. The stability of the samples was evaluated by the loss rate of nutrients. The loss rate was calculated using the following formula: loss rate (%) = (initial mass of substance-remaining mass of substance)/initial mass of substance x 100%. The results of the loss rate test of the main nutrients obtained are shown in Table 2.
TABLE 2 results of loss rate test of major nutrients
As shown in table 2, the stability of the euphausia superba oil gel samples prepared in each example and comparative example under long-term storage conditions was compared by the loss rates of astaxanthin and phospholipids. Each example shows very good stability, and the loss rate of astaxanthin and phospholipids is within 3% after 12 months of storage. The stability of comparative example 1 was the worst, and after 12 months, the loss rates of astaxanthin and phospholipids were all 13% or more, because the structural strength of comparative example 1 was the lowest, the degree of crosslinking was low, and effective protection of the nutrients in the oil could not be achieved. Therefore, the krill oil gel prepared by the invention can obviously improve the stability of nutrient substances in the krill oil in the storage process.
The above description is only an example of the present application, and the scope of the present application is not limited to the specific examples, but is defined by the claims of the present application. Various modifications and variations of the present application will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. The compound antarctic krill oil gel is characterized by comprising the following components in parts by mass: 2-5% amidated pectin aerogel template, 95-98% krill peptide capillary suspension.
2. The composite antarctic krill oil gel of claim 1, wherein the gel comprises the following components in parts by mass: 2-3% amidated pectin aerogel template, 97-98% krill peptide capillary suspension.
3. The method for preparing the compound antarctic krill oil gel according to claim 2, wherein the amidated pectin aerogel template is prepared by taking tertiary butanol aqueous solution as a solvent and freeze-drying the amidated pectin solution.
4. The method for preparing the compound antarctic krill oil gel according to claim 2, wherein the krill peptide capillary suspension is prepared by constructing a ternary liquid/solid system by taking krill peptide as suspended particles, antarctic krill oil as a first solvent and pure water as a second solvent.
5. A method of preparing the composite antarctic krill oil gel of claim 1, comprising the steps of:
(1) Adding the amidated pectin solution into a tertiary butanol aqueous solution to obtain a mixed solution;
(2) Crosslinking the mixed solution in the step (1) for 3-6 hours, then pre-freezing, and then freeze-drying for 30-40 hours to obtain an amidated pectin aerogel template;
(3) Adding 10-30wt% of krill peptide into the euphausia superba oil, homogenizing and shearing uniformly, and immersing the amidated pectin aerogel template obtained in the step (2) into the euphausia superba oil to obtain an oil phase system;
(4) Adding pure water with the mass fraction of 0.2-0.3wt% into the oil phase system in the step (3), and homogenizing and shearing uniformly to obtain the composite antarctic krill oil gel.
6. The method for preparing a compound antarctic krill oil gel according to claim 5, wherein the amidated pectin solution has a pH of 3.5-4.5 and a weight percentage of 1-3wt%.
7. The method for preparing a composite antarctic krill oil gel according to claim 5, wherein the volume of the tertiary butanol aqueous solution is the same as that of the amidated pectin solution, and the tertiary butanol aqueous solution contains 60-80% v/v tertiary butanol and 1-3wt% Zn 2+.
8. The method of preparing a composite antarctic krill oil gel of claim 5, wherein the pre-freezing condition of step (2) is pre-freezing at a temperature of-30 ℃ to-40 ℃ until the mixed solution is completely frozen.
9. The method for preparing a composite antarctic krill oil gel according to claim 5, wherein the condition of homogenizing and shearing in the step (3) is homogenizing for 10-15min under 1500-2500rpm, and the condition of homogenizing and shearing in the step (4) is homogenizing for 10-15min under 1500-2500 rpm.
10. Use of a composite antarctic krill oil gel according to any one of claims 1 to 4, and/or a composite antarctic krill oil gel according to any one of claims 5 to 9, as prepared by a method for preparing a composite antarctic krill oil gel, for the preparation of a food, health food or pharmaceutical carrier.
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