CN109198049B - Fish oil microcapsule and preparation method and application thereof - Google Patents

Fish oil microcapsule and preparation method and application thereof Download PDF

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CN109198049B
CN109198049B CN201811368982.4A CN201811368982A CN109198049B CN 109198049 B CN109198049 B CN 109198049B CN 201811368982 A CN201811368982 A CN 201811368982A CN 109198049 B CN109198049 B CN 109198049B
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fish oil
oil microcapsule
homogenizing
drying
microcapsule
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CN109198049A (en
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吴铎
熊星星
张盛宇
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Suzhou University
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Suzhou University
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04Working-up

Abstract

The invention discloses a fish oil microcapsule and a preparation method and application thereof, belonging to the technical field of functional food processing. Selecting separated whey protein as a wall material and fish oil as a core material, and preparing the fish oil microcapsule particles with uniform and controllable sizes through unit operations such as dissolving, homogenizing, spray drying, sample collection and the like. The fish oil microcapsule particles with uniform particle size can be obtained by using the microfluidic spray drying tower; the obtained product is milky white, has no fishy smell, and has low water content. The product has the characteristic of high encapsulation efficiency and has good oxidation stability at low temperature. The invention realizes coating of fish oil by a single wall material, and the solution preparation is simple.

Description

Fish oil microcapsule and preparation method and application thereof
Technical Field
The invention relates to a fish oil microcapsule and a preparation method and application thereof, belonging to the technical field of functional food processing.
Background
Fish oil is rich in omega-3 unsaturated fatty acids, and the main omega-3 unsaturated fatty acids are docosahexaenoic acid (DHA) and eicosapentaenoic acid (EPA). The fish oil has very positive effect on the development of infants and the treatment of mental diseases, can effectively resist diseases such as inflammation, platelet aggregation, hyperlipidemia and the like, and has very high nutritional value. However, the high unsaturation degree of the fish oil makes the fish oil easy to be oxidized in the storage process, thereby generating peculiar smell and deteriorating; secondly, the fish oil in liquid state has strong fishy smell and is difficult to be directly added into food for eating, which greatly restricts the development and application of fish oil products.
Therefore, the active ingredients in the fish oil are effectively protected, and the taste and property performance of the fish oil are improved, so that the application value of the fish oil can be effectively improved, and the method has great significance for developing functional products of the fish oil.
The microcapsule technology is widely applied to the food field, and microcapsule particles have special structures, which can bring many advantages in application, such as reduction of the reaction of encapsulated substances; protecting the wrapped material from evaporation or loss; the processing, application and storage of the wrapped objects are facilitated; the slow release effect is improved; can mask bad smell and taste. The spray drying method is a common method for microencapsulating fish oil, and has the advantages of simple operation, high automation degree and easy process amplification. However, the microcapsule particles obtained by general spray drying have large differences in particle size, resulting in large differences in product property performance, and the quality of the product cannot be evaluated better. Meanwhile, most wall materials used in the existing research are composite, the prepared solution is complex, and the microcapsule has high redissolution property, so that the storage and the use of the product are not facilitated.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of the fish oil microcapsule coated by a single wall material, the prepared fish oil microcapsule has uniform particle size distribution, higher product encapsulation efficiency and lower redissolution property, and can well cover the peculiar smell of the fish oil.
The first purpose of the invention is to provide a preparation method of fish oil microcapsules, which comprises the following steps:
(1) weighing protein powder and fish oil, dissolving the protein powder and the fish oil in a solvent according to the solid content of the liquid being 4-8 wt%, stirring to obtain a primary emulsion, and carrying out high-pressure homogenization on the primary emulsion to obtain a precursor liquid;
(2) and (2) spray drying the precursor solution obtained in the step (1) by adopting a microfluidic spray drying tower to obtain the fish oil microcapsule particles.
Furthermore, the protein is one or more of separated whey protein, soy protein, casein and pea protein.
Further, the mass ratio of the protein powder to the fish oil is 1-5: 1.
Further, the rotating speed of the stirring is 400-1000 rpm, and the stirring time is 0.5-1 h.
Further, the pressure of the high-pressure homogenization is 400-600 MPa, and the homogenization time is 5-10 min.
Further, in the step (1), the solvent is water and/or an organic solvent.
Further, the drying temperature of the spray drying is 100-160 ℃.
Further, the feeding pressure of the spray drying is 0.2-0.6 kg/cm2
Furthermore, the piezoelectric ceramic frequency of the spray drying tower is 10kHz, and the amplitude is 5 Vpp.
The second object of the invention is the fish oil microcapsule prepared by the method.
The third purpose of the invention is to provide the application of the fish oil microcapsule in food and health care products.
The invention has the beneficial effects that:
the uniform fish oil microcapsule product obtained by the invention is milk white, has no fishy smell and other peculiar smell, and has lower water content; the particle size distribution of the particles is uniform.
The uniform fish oil microcapsule obtained by the invention has good protection effect on fish oil, and improves the oxidation resistance of the fish oil; the product has high encapsulation efficiency and low re-solubility, and can well cover the peculiar smell of the fish oil.
The invention has simple production process, high automation degree, rapidness and high efficiency.
The product has multiple effects, can be used for preparing functional foods, can also be used as an additive in foods, improves the nutritional value of the foods, and has wide application prospect.
Drawings
FIG. 1 is a scanning electron microscope image of O1W5 fish oil microcapsule prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of O1W3 fish oil microcapsule prepared in example 3 of the present invention;
FIG. 3 is a scanning electron microscope image of O1W1 fish oil microcapsule prepared in example 4 of the present invention;
FIG. 4 is a scanning electron microscope image of O2W1 fish oil microcapsule prepared in example 5 of the present invention;
figure 5 is a graph of peroxide number of fish oil microcapsules as a function of storage time.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The spraying process of the microfluidic spray drying tower is controlled by a microfluidic chip.
The method for measuring the water content comprises the following steps: weighing about 0.1g of sample, putting the sample into a 105 ℃ oven, standing for 24h, taking out the sample, weighing the mass, and taking the reduced mass as the moisture content.
The particle size measuring method comprises the following steps: about 100 particles were taken in a picture of a scanning electron microscope, and the particle diameter of each particle was measured.
The method for measuring the encapsulation efficiency comprises the following steps: the content of the encapsulated fish oil is obtained by subtracting the surface oil content of the fish oil microcapsules from the total fish oil amount, and the percentage of the encapsulated fish oil content to the total fish oil amount is the encapsulation rate.
Method for measuring oxidation stability: the oxidation stability of the fish oil microcapsules was determined using a low temperature dry storage experiment: the fish oil microcapsules were stored in a low temperature desiccator for 4 weeks. The samples are taken periodically, the peroxide value of the samples is measured, and the oxidation stability of the fish oil microcapsules is evaluated through the change of the peroxide value with time. The peroxide number is determined by titration.
Example 1:
(1) dissolving 3.0g of fish oil and 15.0g of whey protein isolate in 300ml of water, and stirring at 500rpm for 0.5h to obtain primary emulsion; (2) homogenizing and emulsifying the primary emulsion under high pressure to obtain emulsion liquid, wherein the homogenizing pressure is 400MPa, and the homogenizing time is 10 min; (3) spray drying the emulsion precursor to obtain fish oil microcapsule granules, wherein the drying temperature is 160 ℃, and the feeding pressure is 0.4kg/cm2
The water content, encapsulation efficiency and oxidation stability of the fish oil microcapsule particles prepared in this example were measured, and the morphology of the particles was observed by a scanning electron microscope, and the results are shown in fig. 1.
The specific measurement results are shown in Table 1.
TABLE 1
Figure GDA0003423219040000041
Example 2:
(1) dissolving 3.0g of fish oil and 15.0g of whey protein isolate in 300ml of water, and stirring at 500rpm for 0.5h to obtain primary emulsion; (2) homogenizing and emulsifying the primary emulsion under high pressure to obtain emulsion liquid, wherein the homogenizing pressure is 400MPa, and homogenizing for 3 times; (3) spray drying the emulsion to obtain fish oil microcapsule granules, wherein the tower top temperature is 100 deg.C, and the feeding pressure is 0.4kg/cm2
The water content, particle size, encapsulation efficiency and oxidation stability of the fish oil microcapsule particles prepared in this example were measured.
The specific measurement results are shown in Table 2.
TABLE 2
Figure GDA0003423219040000042
Example 3:
(1) dissolving 4.5g fish oil and 13.5g whey protein isolate in 300ml water, stirring at 500rpm for 0.5h to obtain primary emulsion; (2) homogenizing and emulsifying the primary emulsion under high pressure to obtain emulsion liquid, wherein the homogenizing pressure is 400MPa, and homogenizing for 3 times; (3) spray drying the emulsion to obtain fish oil microcapsule granules, wherein the tower top temperature is 100 deg.C, and the feeding pressure is 0.4kg/cm2
The water content, particle size, encapsulation efficiency and oxidation stability of the fish oil microcapsule particles prepared in this example were measured, and the morphology of the particles was observed by a scanning electron microscope, and the results are shown in fig. 2.
The specific measurement results are shown in Table 3.
TABLE 3
Figure GDA0003423219040000043
Figure GDA0003423219040000051
Example 4:
(1) dissolving 9.0g of fish oil and 9.0g of whey protein isolate in 300ml of water, and stirring at 500rpm for 0.5h to obtain primary emulsion; (2) homogenizing and emulsifying the primary emulsion under high pressure to obtain emulsion liquid, wherein the homogenizing pressure is 400MPa, and the homogenizing time is 5 min; (3) spray drying the emulsion to obtain fish oil microcapsule granules, wherein the drying temperature is 160 ℃, and the feeding pressure is 0.4kg/cm2
The water content, particle size, encapsulation efficiency and oxidation stability of the fish oil microcapsule particles prepared in this example were measured, and the morphology of the particles was observed by a scanning electron microscope, and the results are shown in fig. 3.
The specific measurement results are shown in Table 4.
TABLE 4
Figure GDA0003423219040000052
Example 5:
(1) dissolving 12.0g of fish oil and 6.0g of whey protein isolate in 300ml of water, and stirring at 500rpm for 0.5h to obtain primary emulsion; (2) homogenizing and emulsifying the primary emulsion under high pressure to obtain emulsion liquid, wherein the homogenizing pressure is 400MPa, and the homogenizing time is 5 min; (3) spray drying the emulsion to obtain fish oil microcapsule granules, wherein the drying temperature is 160 ℃, and the feeding pressure is 0.4kg/cm2
The water content, particle size, encapsulation efficiency and oxidation stability of the fish oil microcapsule particles prepared in this example were measured, and the morphology of the particles was observed by a scanning electron microscope, and the results are shown in fig. 4.
The results of the measurement are shown in Table 5.
TABLE 5
Figure GDA0003423219040000053
As can be seen from tables 1-5, the water content of the fish oil microcapsule particles prepared by the invention is low; from the aspect of encapsulation efficiency, the fish oil microcapsule particles prepared by the invention have higher encapsulation efficiency and better encapsulation effect; the standard deviation of the particle size of the fish oil microcapsule particles prepared by the invention is small, and the particle size distribution is uniform.
As can be seen from FIGS. 1-4, the fish oil microcapsules O1W5 and O1W3 have regular bowl-shaped structures, while the fish oil microcapsules O1W1 and O2W1 have irregular oval shapes, and the surface of the fish oil microcapsules has a plurality of dents, and the dents on the surface are increased and the dent stratification is increased as the WPI content is increased.
The results of oxidation stability are shown in fig. 5, wherein the SD particles PV of Fresh are minimal and increase with increasing oil content, and the PV values are all greater than raw oil, indicating that a portion of the fish oil is oxidized by the higher drying temperature during the drying phase; there was a very large increase in PV after one week, which was that the fish oil on the surface was substantially oxidized, when PV also increased with increasing oil content; at the second and fourth weeks the PV of O1W5, O1W3, O1W1 gradually decreased because the oxidized peroxides were further oxidized to aldones, which could not be detected, while the PV of O2W1 increased because the fish oil content was too high and a large amount of fish oil was still being oxidized; after four weeks, PV of O1W5, O1W3 decreased to around 65 and 83; however, O1W1 and O2W1 still have higher PV, because the fish oil cannot be protected better when the WPI content is low, and the lower encapsulation efficiency enables more fish oil to be continuously oxidized on the surface.
Therefore, the uniform fish oil microcapsule particles prepared by the invention are milk white, have no fishy smell, have low water content and uniform particle size distribution; the invention realizes that the fish oil is coated by a single wall material, the solution preparation is simple, and the uniform fish oil microcapsule particles with the core-shell structure are prepared by regulating the proportion of the fish oil and the separated whey protein and the drying temperature, the core-shell structure can obviously improve the encapsulation rate of the product, and can well protect the fish oil in the fish oil microcapsule particles; the oxidation stability of the fish oil microcapsule particles is improved; the uniform fish oil microcapsule particles prepared by the invention have lower solubility, and can well cover the fishy smell of the fish oil; the product has the effects of being beneficial to the health of human bodies, can be used for preparing functional foods, and can also be used as additives in foods to improve the nutritional value of the foods.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.

Claims (5)

1. The preparation method of the fish oil microcapsule is characterized by comprising the following steps:
(1) dissolving protein powder and fish oil in a solvent according to the solid content of the liquid being 4-8 wt%, stirring to obtain a primary emulsion, and carrying out high-pressure homogenization on the primary emulsion to obtain a precursor liquid; the mass ratio of the protein powder to the fish oil is 5:1, the protein is isolated whey protein, the stirring speed is 400-1000 rpm, the stirring time is 0.5-1 h, the high-pressure homogenizing pressure is 400-600 MPa, and the homogenizing time is 5-10 min;
(2) and (2) spray-drying the precursor solution obtained in the step (1) by adopting a microfluidic spray-drying tower to obtain the fish oil microcapsule particles, wherein the drying temperature of the spray-drying is 160 ℃.
2. The method according to claim 1, wherein in step (1), the solvent is water and/or an organic solvent.
3. The method of claim 1, wherein the feed pressure of the spray drying is 0.2 to 0.6kg/cm2
4. A fish oil microcapsule prepared by the method of any one of claims 1 to 3.
5. The use of the fish oil microcapsule of claim 4 in food and health care products.
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