AU2017258935A2 - Method of layer-by-layer self-assembly immobilizing flaxseed oil and composite oil thereof - Google Patents
Method of layer-by-layer self-assembly immobilizing flaxseed oil and composite oil thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
- A23D7/005—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by ingredients other than fatty acid triglycerides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
- A23D7/02—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by the production or working-up
- A23D7/04—Working-up
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/10—Complex coacervation, i.e. interaction of oppositely charged particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/20—After-treatment of capsule walls, e.g. hardening
- B01J13/206—Hardening; drying
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Abstract
Abstract The present invention discloses a method of layer-by-layer self-assembly immobilizing flaxseed oil and a composite oil thereof. The method comprises 5 the following steps: (1) dispersing the oil in a sodium alginate aqueous solution, and obtaining oil-sodium alginate microcapsules through shearing or homogenizing; (2) adding the oil-sodium alginate microcapsules into a calcium lactate aqueous solution, and obtaining immobilized oil-sodium alginate gel beads through stirring; (3) sequentially adding the immobilized 10 oil-sodium alginate gel beads into a chitosan aqueous solution, the sodium alginate aqueous solution and the calcium lactate aqueous solution, sequentially stirring, and obtaining a layer of self-assembly immobilized oil-sodium alginate gel beads; (4) repeating step (3) with the layer of self-assembly immobilized oil-sodium alginate gel beads, i.e. realizing the 15 layer by layer self-assembly immobilizing of the oil. The gel beads of the present invention has a high oil-loading rate, and when being calculated according to the mass ratio of a core material and a wall material, the oil-loading rate of the microcapsules in the present invention is up to 1700-7000%. The method of the present invention can be carried out under 20 room temperature, and the temperature required is lower than that required in the method of spray drying, thereby saving the cost.
Description
Method of laver-bv-laver seif-assembly immobilizing flaxseed oil and composite oil thereof
Technical Field
The present invention relates to a method of layer-by-layer self-assembly immobilizing flaxseed oil and composite oil thereof, and falls within the field of oil processing.
Background
The content of unsaturated fatty acids in flaxseed oil is up to 90% or more, wherein the content of α-linolenic acid is the highest (in some species, the content thereof exceeds 54%). α-linolenic acid is an n-3 essential fatty acid for human, can be converted into EPA and DHA in the body, and have physiological functions of promoting the growth and development of the brain of fetuses and infants, strengthening memory, enhancing immunity, improving and maintaining eyesight, and preventing cerebral thrombosis and myocardial infarction, etc. Studies have shown that intake of saturated fatty acid is positively related to the development of cardiovascular disease. If the intake of n-3 essential fatty acids is insufficient, both the learning ability and visual acuity of animals would decrease. At present, China diet is short of n-3 fatty acids, but the intake of saturated fatty acids and n-6 unsaturated fatty acids is more than enough.
Flaxseed oil, as an excellent n-3 unsaturated fatty acid source, is easily oxidized as the content of unsaturated fatty acids therein is too high, which in consequence produces unfavourable flavour and even harmful substances, affecting the shelf time of flaxseed oil. The microencapsulation embedding technology can greatly delay and avoid the oxidation of flaxseed oil in the process of processing, transportation and consumption. The microencapsulation of flaxseed oil not only contributes to its use, transportation and preservation, but also facilitates the development of many convenient foods, such as nutrition fortification milk powder; and the microencapsulation can also prevent the oxidation and deterioration of some unstable food raw excipients, and decrease or cover unpleasant flavours etc.
Currently, common encapsulation methods involve spray drying, emulsion diffusing, interfacial polymerization, and complex coacervation etc., wherein spray drying has a greater application because of its simple process. In spray drying, most frequently used are com starch, modified starch, whey powder, vegetable protein, gelatin, and arabic gum as the wall material or emulsion material to embed the flaxseed oil. The moisture of the emulsion is evaporated under the action of hot gas stream, and the core material is embedded with the wall material to form the microcapsule products. However, in spray drying, there are problems like high temperature, multi-excipients combination, wall adhering and low encapsulation rate. The temperature of the nozzle for spray drying is 150°C-190°C, while high temperature affects the quality of the product. At the same time, the temperature of the collection flask of many spraying equipment is also above 60°C, and hence the flaxseed oil still contacts a high-temperature environment during the preparation process of flaxseed oil microcapsules. In some other embedding methods, to sufficiently emulsify the wall material and the core material, generally a large amount of synthetic emulsifiers such as tween and span are used in the preparation process. At present, the security problems of emulsifiers also have attracted the attention of some scholars. Consequently, there is a need for providing a new oil encapsulation method.
Contents of Invention
The present invention may provide a method of layer-by-layer self-assembly immobilizing flaxseed oil and composite oil thereof. The present invention firstly prepares microcapsules of the oil, then uses calcium lactate for immobilizing, and finally carries out a layer by layer self-assembly to the immobilized oil gel beads, i.e. realizing the layer by layer encapsulation of the oil. The oil-loading rate of the gel beads prepared by the method of the present invention is high, and can reach 1700-7000%; and the encapsulation rate of the gel beads prepared with the method of the present invention is high, and can reach 92-99%.
The method of layer by layer self-assembly immobilizing oil provided in the present invention comprises the following steps: (1) dispersing the oil in a sodium alginate aqueous solution, and obtaining oil-sodium alginate microcapsules through shearing at a high speed or homogenizing; (2) adding the oil-sodium alginate microcapsules into a calcium lactate aqueous solution, and obtaining immobilized oil-sodium alginate gel beads through stirring; (3) sequentially adding the immobilized oil-sodium alginate gel beads into a chitosan aqueous solution, the sodium alginate aqueous solution and the calcium lactate aqueous solution, sequentially stirring, and obtaining a layer of self-assembly immobilized oil-sodium alginate gel beads; and (4) repeating step (3) with the layer of self-assembly immobilized oil-sodium alginate gel beads, i.e. realizing the layer by layer self-assembly immobilizing of the oil.
In the above-mentioned method, the oil can be at least one of flaxseed oil, peony seed oil, grape seed oil, camellia oil, peanut oil, germ oil, walnut oil, siritch, sesame oil, olive oil, deep sea fish oil, galic essential oil and ginger oleoresin. If an encapsulation treatment to the flaxseed oil alone or to the composite of the three of flaxseed oil, peony seed oil and grape seed oil is carried out, the ratio of the parts by mass of the three can be 40-50 parts: 10-20 parts: 10-20 parts, in particular for example: 45 parts: 15 parts: 15 parts.
In the above-mentioned method, the mass concentration of the sodium alginate aqueous solution may be 1.1-1.4%, and in particular can be 1.1% or 1.4%; the mass concentration of the chitosan aqueous solution may be 1-3%, in particular can be 1%, 2% or 3%; and the mass concentration of the calcium lactate aqueous solution may be 1-3%, and in particular can be 1%, 2% or 3%.
In the above-mentioned method, in step (1), the volume ratio of the oil and the sodium alginate aqueous solution can be 1 : 0.5-20, and in particular can be 1 : 2.5; the shearing time can be 1 -4 min, such as 2 min.
The particle size of the sodium alginate microcapsules can be regulated through a high-speed shearing machine or a homogenizer.
In the above-mentioned method, in step (2), an injector is used to add the oil-sodium alginate microcapsules into the calcium lactate aqueous solution; the particle size of the immobilized oil-sodium alginate gel beads can be prepared by adjusting the size of the needle of the injector; the stirring time can be 5-10 min, and in particular can be 5 min.
In the above-mentioned method, in step (3), the stirring time can be 5-10 min, and in particular can be 5 min;
The step uses the electrostatic adsorption between the chitosan and the sodium alginate to achieve the layer by layer assembly of the microcapsules, and the immobilizing is carried out using the calcium lactate after each layer of the wall is assembled.
In the above-mentioned method, in step (4), step (3) is repeated at least 1-2 times.
The layer by layer self-assembly immobilized oil-sodium alginate gel beads prepared in present invention can be dried or packaged: 8-10 h air blast drying at a low temperature; or a liquid packaging is carried out after irradiation sterilization.
The gel bead prepared with the method of the present invention has its oil-loading rate of up to 1700-7000%, such as 2900-3100%, wherein the oil-loading rate refers to the mass percentage of the core material and the wall material of the layer by layer self-assembly immobilized oil gel beads, the core material refers to the oil, and the wall material refers to the layer by layer self-assembly layer that encapsulates the oil.
The gel bead prepared with the method of the present invention has its encapsulation rate of up to 92-99%, wherein the encapsulation rate refers to the mass percentage of the oil encapsulated in the gel bead and the total oil added.
Brief Description of the Drawings
Figure 1 illustrates the electron microscope images of the sodium alginate-flaxseed oil microcapsules prepared in Example 1 of the present invention, wherein Figure l(a)-Figure 1(f) are respectively the electron microscope images of the flaxseed oil-sodium alginate microcapsules prepared in Examples 1)-6) of the present application.
Figure 2 illustrates the electron microscope images of the flaxseed oil-sodium alginate gel beads prepared in Example 2 of the present invention, wherein Figure 2(a) and Figure 2(b) are the electron microscope images after and before drying, respectively.
Particular Embodiments of the Invention
The experimental methods used in the following examples are all conventional methods, unless otherwise specified.
The materials, reagents and the like used in the following examples are all commercially available, unless otherwise specified.
Example 1. Examination of concentration of sodium alginate flaxseed oil-sodium alginate microcapsules are prepared according to the following six conditions, respectively: 1) add 8 mL flaxseed oil into 20 mL 0.5 wt% sodium alginate aqueous solution, and obtain the flaxseed oil-sodium alginate microcapsules after shearing for 2 min at 15000 r/min. 2) add 8 mL flaxseed oil into 20 mL 0.8 wt% sodium alginate aqueous solution, and obtain the flaxseed oil-sodium alginate microcapsules after shearing for 2 min at 15000 r/min. 3) add 8 mL flaxseed oil into 20 mL 1.1 wt% sodium alginate aqueous solution, and obtain the flaxseed oil-sodium alginate microcapsules after shearing for 2 min at 15000 r/min. 4) add 8 mL flaxseed oil into 20 mL 1.4 wt% sodium alginate aqueous solution, and obtain the flaxseed oil-sodium alginate microcapsules after shearing for 2 min at 15000 r/min. 5) add 8 mL flaxseed oil into 20 mL 1.7 wt% sodium alginate aqueous solution, and obtain the flaxseed oil-sodium alginate microcapsules after shearing for 2 min at 15000 r/min. 6) add 8 mL flaxseed oil into 20 mL 2.0 wt% sodium alginate aqueous solution, and obtain the flaxseed oil-sodium alginate microcapsules after shearing for 2 min at 15000 r/min.
The particle size and potential of the flaxseed oil-sodium alginate microcapsules prepared in the present Example are as shown in table 1.
Table 1. The particle size and potential of the flaxseed oil-sodium alginate microcapsules
Z-Ave d.nm Pdl ZP mV
20 mL 0.5% ALG + 8 mL , , ., 3389 ± 169.9 0.502 ±0.024 -85.1 ± 1.01
Flaxseed Oil
20 mL 0.8% ALG ± 8 mL , , ., 4387 ±267.9 0.5 ±0.14 -85.2 ±1.83
Flaxseed Oil
20 mL 1.1% ALG ± 8 mL , 7881 ±418.9 0.416 ±0.037 -84.6 ±1.76
Flaxseed Oil
20 mL 1.4% ALG ± 8 mL , , ., 9135 ±3100 0.451 ±0.107 -85.3 ±3.5
Flaxseed Oil
20 mL 1.7% ALG + 8 mL , , ., 7394 ± 1920 0.366 ±0.157 -81.3 ±1.96
Flaxseed Oil
20 mL 2.0% ALG + 8 mL , , 3284 ±568.7 0.842 ±0.274 -80.2 ±1.33
Flaxseed Oil
In table 1, ALG represents sodium alginate, and Flaxseed Oil means flaxseed oil.
It can be seen from the change of the value (Z-Ave d. ran) of the particle size in table 1, with the increase of the concentration of sodium alginate, the particle size of the flaxseed oil-sodium alginate microcapsules increases. But as the viscosity of 2 wt% sodium alginate aqueous solution is too high, the flaxseed oil cannot be encapsulated, and the phenomenon of layer separating is serious. And as the concentration of 0.5 wt% sodium alginate is too low, the content of oil is too high, and the microcapsules encapsulated are separated from the water phase. Sodium alginate at a low concentration cannot form gel beads with calcium lactate, though the oil can be encapsulated. It can be seen thereby that both sodium alginates at low concentration and high concentration are not suitable.
The PDI in table 1 represents the polydispersity index, which reflects the stability of a system, the value of PDI should be lower than 1, and the smaller the value is, the better. It can be seen from the value of PDI in table 1 that both the standard deviation of the sodium alginate at a high concentration and the value of PDI are comparatively high, indicating that a high concentration of the sodium alginate makes the system unstable. ZP in table 1 represents the potential, and since sodium alginate is electronegative, the bigger the absolute value of the potential is, more stable the system is.
Figure 1 illustrates the electron microscope images of the flaxseed oil-sodium alginate microcapsules prepared in the present Example, wherein Figure l(a)-Figure 1(f) are the electron microscope images of the flaxseed oil-sodium alginate microcapsules prepared in Examples 1)-6) of the present application, respectively.
In Figure 1, the bright white balls are oil drops not encapsulated, and it can be seen that the flaxseed oil is almost encapsulated by sodium alginate. It can be seen from Figure 1 that the particle size of the flaxseed oil-sodium alginate microcapsules and the change tendency thereof are consistent with that in table 1. The flaxseed oil-sodium alginate microcapsules appear in irregular strips or spheres, and their shapes are related to the high-speed shearing of the high-speed refiner.
To sum up, it can be determined that the optimum concentration of sodium alginate is 1.1-1.4%.
Example 2. Layer-by-layer self-assembly immobilizing of flaxseed oil
Layer by layer self-assembly immobilizing is carried out with the flaxseed oil-sodium alginate microcapsules prepared in 3) of Example 1. (1) Immobilizing of microcapsules
Flaxseed oil-sodium alginate microcapsules are sucked up with an injector, and added to 2 wt% calcium lactate aqueous solution, magnetically stirred for 5 min, and the immobilized flaxseed oil-sodium alginate gel beads are obtained. (3) Layer-by-layer self-assembly a) placing the immobilized flaxseed oil bead prepared in step (1) in 2 wt% chitosan aqueous solution, and magnetically stirring for 5 min; placing the bead in a 1.1 wt% sodium alginate solution after taking it out, and magnetically stirring the solution for 5 min; in the end, placing the beads in 2 wt% calcium lactate aqueous solution, magnetically stirring for 5 min, and obtaining a layer of self-assembly immobilized flaxseed oil-sodium alginate gel beads. b) repeating step a) twice with the layer of the self-assembly immobilized flaxseed oil-sodium alginate gel beads, i.e. realizing the layer by layer self-assembly immobilizing of flaxseed oil and obtaining flaxseed oil-sodium alginate gel beads.
Figure 2 illustrates the electron microscope images of the flaxseed oil-sodium alginate gel beads prepared in the present Example, wherein, Figure 2(a) and Figure 2(b) are the electron microscope images after and before drying, respectively. It can be seen from the images that no oil spills or oozes on the surface before or after drying. The particle size of the gel beads after drying is 0.8-1.5 mm, and the size of the gel beads without being dried is 1.5-2.5 mm.
The oil-loading rate of the flaxseed oil-sodium alginate gel beads prepared in the present Example is 3010%, and the encapsulation rate is 92%.
Example 3. Layer-by-layer self-assembly immobilizing of flaxseed oil
Layer by layer self-assembly immobilizing is carried out with the flaxseed oil-sodium alginate microcapsules prepared in 3) of Example 1. (1) Immobilizing of microcapsules
Flaxseed oil-sodium alginate microcapsules are sucked up with an injector, added to 1 wt% calcium lactate aqueous solution, magnetically stirred for 5 min, and the immobilized flaxseed oil-sodium alginate gel beads are obtained. (3) Layer-by-layer self-assembly a) placing the immobilized flaxseed oil beads prepared in step (1) in 1 wt% chitosan aqueous solution, and magnetically stirring for 5 min; placing the beads in a 1.1 wt% sodium alginate solution after taking them out, and magnetically stirring for 5 min; in the end, placing the beads in 1 wt% calcium lactate aqueous solution, magnetically stirring for 5 min, and obtaining a layer of self-assembly immobilized flaxseed oil-sodium alginate gel beads. b) repeating step a) one time with the layer of the self-assembly immobilized flaxseed oil-sodium alginate gel beads, i.e. realizing the layer by layer self-assembly immobilizing of flaxseed oil and obtaining flaxseed oil-sodium alginate gel beads.
The oil-loading rate of the flaxseed oil-sodium alginate gel beads prepared in the present Example is 3100%, and the encapsulation rate is 97%.
Example 4. Layer-by-layer self-assembly immobilizing of flaxseed oil
Layer by layer self-assembly is carried out with the flaxseed oil-sodium alginate microcapsules prepared in 3) of Example 1. (1) Immobilizing of microcapsules
Flaxseed oil-sodium alginate microcapsules are sucked up with an injector, added to 3 wt% calcium lactate aqueous solution, magnetically stirred for 5 min, and the immobilized flaxseed oil-sodium alginate gel beads are obtained. (3) Layer-by-layer self-assembly a) placing the immobilized flaxseed oil bead prepared in step (1) in 3 wt% chitosan aqueous solution, and magnetically stirring for 5 min; placing the beads in a 1.1 wt% sodium alginate solution after taking them out, and magnetically stirring for 5 min. In the end placing the beads in 3 wt% calcium lactate aqueous solution, magnetically stirring for 5 min, and obtaining a layer of self-assembly immobilized flaxseed oil-sodium alginate gel beads. b) repeating step a) twice with the layer of the self-assembly immobilized flaxseed oil-sodium alginate gel beads, i.e. realizing the layer by layer self-assembly immobilizing of flaxseed oil and obtaining flaxseed oil-sodium alginate gel beads.
The oil-loading rate of the flaxseed oil-sodium alginate gel beads prepared in the present Example is 3000%, and the encapsulation rate is 95%.
Example 5. Layer-by-layer self-assembly immobilizing of flaxseed oil
Layer by layer self-assembly is carried out with the flaxseed oil-sodium alginate microcapsules prepared in 4) of Example 1. (1) Immobilizing of microcapsules
Flaxseed oil-sodium alginate microcapsules are sucked up with an injector, added to 2 wt% calcium lactate aqueous solution, magnetically stirred for 5 min, and the immobilized flaxseed oil-sodium alginate gel beads are obtained. (3) Layer-by-layer self-assembly
Placing the immobilized flaxseed oil bead prepared in step (1) in 2 wt% chitosan aqueous solution, and magnetically stirring for 5 min; placing the beads in a 1.4 wt% sodium alginate solution after taking them out, and magnetically stirring for 10 min; in the end, placing the beads in 2 wt% calcium lactate aqueous solution, magnetically stirring for 5 min, and obtaining a layer of self-assembly immobilized flaxseed oil-sodium alginate gel beads. b) repeating step a) one time with the layer of the self-assembly immobilized flaxseed oil-sodium alginate gel beads, i.e. realizing the layer by layer self-assembly immobilizing of flaxseed oil and obtaining flaxseed oil-sodium alginate gel beads.
The oil-loading rate of the flaxseed oil-sodium alginate gel beads prepared in the present Example is 2910%.
Example 6. Layer-by-layer self-assembly immobilizing of flaxseed oil
Layer by layer self-assembly is carried out with the flaxseed oil-sodium alginate microcapsules prepared in 4) of Example 1. (1) Immobilizing of microcapsules
Flaxseed oil-sodium alginate microcapsules are sucked up with an injector, added to 1 wt% calcium lactate aqueous solution, magnetically stirred for 5 min, and the immobilized flaxseed oil-sodium alginate gel beads are obtained. (3) Layer-by-layer self-assembly
Placing the immobilized flaxseed oil bead prepared in step (1) in 1 wt% chitosan aqueous solution, and magnetically stirring for 5 min; placing the bead in a 1.4 wt% sodium alginate solution after taking it out, and magnetically stirring for 10 min; in the end, placing the beads in 1 wt% calcium lactate aqueous solution, magnetically stirring for 5 min, and obtaining a layer of self-assembly immobilized flaxseed oil-sodium alginate gel beads. b) repeating step a) twice with the layer of the self-assembly immobilized flaxseed oil-sodium alginate gel beads, i.e. realizing the layer by layer self-assembly immobilizing of flaxseed oil and obtaining flaxseed oil-sodium alginate gel beads.
The oil-loading rate of the flaxseed oil-sodium alginate gel beads prepared in the present Example is 2890%, and the encapsulation rate is 94%.
Example 7. Layer-by-layer self-assembly immobilizing of flaxseed oil
Layer by layer self-assembly is carried out to the flaxseed oil-sodium alginate microcapsules prepared in 4) of Example 1. (1) Immobilizing of microcapsules
Flaxseed oil-sodium alginate microcapsules are sucked up with an injector, added to 3 wt% calcium lactate aqueous solution, magnetically stirred for 5 min, and the immobilized flaxseed oil-sodium alginate gel beads are obtained. (3) Layer-by-layer self-assembly
Placing the immobilized flaxseed oil bead prepared in step (1) in 3 wt% chitosan aqueous solution, and magnetically stirring for 5 min; placing the bead in a 1.4 wt% sodium alginate solution after taking it out, and magnetically stirring for 10 min; in the end, placing the beads in 3 wt% calcium lactate aqueous solution, magnetically stirring for 5 min, and obtaining a layer of self-assembly immobilized flaxseed oil-sodium alginate gel beads. b) repeating step a) twice with the layer of the self-assembly immobilized flaxseed oil-sodium alginate gel beads, i.e. realizing the layer by layer self-assembly immobilizing of flaxseed oil and obtaining flaxseed oil-sodium alginate gel beads.
The oil-loading rate of the flaxseed oil-sodium alginate gel beads prepared in the present Example is 2900%, and the encapsulation rate is 95%.
Example 8. Layer-by-layer self-assembly immobilizing of flaxseed oil composite oil (1) Preparation of microcapsules
Take 20 mL 1.1 wt% sodium alginate aqueous solution, add it into 8 mL flaxseed oil composite oil, and obtain the flaxseed oil composite oil-sodium alginate microcapsules after shearing at 1 5,000 r/min for 2 minutes.
The composition of the flaxseed oil composite oil is: flaxseed oil, peony seed oil and grape seed oil, and the ratio of the parts by mass of the three parts is 45 parts: 15 parts: 15 parts. (2) Immobilizing of microcapsules
Sucking up flaxseed oil composite oil-sodium alginate microcapsules with an injector, adding them to 3 wt% calcium lactate aqueous solution, magnetically stirring for 5 min, and obtaining the immobilized flaxseed oil composite oil-sodium alginate gel beads. (3) Layer-by-layer self-assembly a) placing the immobilized flaxseed oil composite oil beads prepared in step (1) in 3 wt% chitosan aqueous solution, and magnetically stirring for 5 min; placing the beads in a 1.1 wt% sodium alginate solution after taking them out, and magnetically stirring for 5 min; in the end, placing the beads in 3 wt% calcium lactate aqueous solution, magnetically stirring for 5 min, and obtaining a layer of self-assembly immobilized flaxseed oil composite oil-sodium alginate gel beads. b) repeating step a) twice with the layer of the self-assembly immobilized flaxseed oil composite oil-sodium alginate gel beads, i.e. realizing the layer by layer self-assembly immobilizing of flaxseed oil and obtaining flaxseed oil composite oil-sodium alginate gel beads.
The oil-loading rate of the flaxseed oil composite oil-sodium alginate gel beads prepared in the present Example is 3100%, and the encapsulation rate is 99%.
Industrial Applications
The present invention has the following beneficial effects: 1. The encapsulation materials used in the method of the present invention comprise sodium alginate, chitosan and calcium lactate and do not contain the commonly used emulsifiers in the prior art such as Tween and Span, so they are all highly safe additives and have high availability. 2. The gel beads prepared in the present invention has a high oil-loading rate, and when being calculated according to the mass ratio of the core material and the wall material, the oil-loading rate of the microcapsules in the present invention is up to 1700-7000%. 3. The gel beads prepared in the present invention has a high encapsulation rate, and when being calculated according to the mass ratio of the oil encapsulated and the total oil added, the encapsulation rate of the microcapsules in the present invention is up to 92-99%. 4. The method of the present invention can be carried out under room temperature, and the temperature required is lower compared to that required by the method of spray drying, which thereby saves the cost. 5. The method of the present invention can encapsulate both flaxseed oil and other oils or composite oils.
Claims (5)
- Claims1. A method of layer-by-layer self-assembly immobilizing flaxseed oil and composite oil thereof, comprising the following steps: (1) dispersing the oil in a sodium alginate aqueous solution, and obtaining oil-sodium alginate microcapsules through shearing or homogenizing; (2) adding the oil-sodium alginate microcapsules into a calcium lactate aqueous solution, and obtaining immobilized oil-sodium alginate gel beads through stirring; (3) sequentially adding the immobilized oil-sodium alginate gel beads into a chitosan aqueous solution, the sodium alginate aqueous solution and the calcium lactate aqueous solution, sequentially stirring, and obtaining a layer of self-assembly immobilized oil-sodium alginate gel beads; (4) repeating step (3) with the layer of self-assembly immobilized oil-sodium alginate gel beads, i.e. realizing the layer by layer self-assembly immobilizing of the oil.
- 2. The method according to claim 1, wherein the oil is at least one of flaxseed oil, peony seed oil, grape seed oil, camellia oil, peanut oil, germ oil, walnut oil, siritch, sesame oil, olive oil, deep sea fish oil, galic essential oil and ginger oleoresin.
- 3. The method according to claim 1 or 2, wherein the mass concentration of the sodium alginate aqueous solution is 1.1-1.4%; the mass concentration of the chitosan aqueous solution is 1-3%; the mass concentration of the calcium lactate aqueous solution is 1-3%; and/or, wherein in step (1), the volume ratio of the oil and the sodium alginate aqueous solution is 1: 0.5-20; the shearing time is 1-4 min; and/or, wherein in step (2), an injector is used to add the oil-sodium alginate microcapsules into the calcium lactate aqueous solution; the stirring time is 5-10 min; and/or, wherein in step (3), the stirring time is 5-10 min; and/or, wherein in step (4), step (3) is repeated at least 1-2 times.
- 4. Gel beads prepared by the method according to claim 1 or2.
- 5. The gel beads according to claim 4, wherein an oil-loading rate of the gel beads is 1700-7000%, and the oil-loading rate refers to a mass percentage of a core material and a wall material of the gel beads, and/or, wherein an encapsulation rate of the gel beads is 92-99%, and the encapsulation rate refers to a mass percentage of the oil encapsulated in the gel beads and the total oil added.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN201610344195.0 | 2016-05-23 | ||
| PCT/CN2017/075835 WO2017202104A1 (en) | 2016-05-23 | 2017-03-07 | Layer-by-layer self-assembly of solidified linseed oil and lipid complex thereof |
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| AU2017258935A Pending AU2017258935A1 (en) | 2016-05-23 | 2017-03-07 | Method of layer-by-layer self-assembly immobilizing flaxseed oil and composite oil thereof |
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| CN106035739B (en) * | 2016-05-23 | 2019-05-17 | 中国农业大学 | A kind of method that LBL self-assembly solidifies linseed oil and its compounds grease |
| CN106732218A (en) * | 2016-12-05 | 2017-05-31 | 中山大学惠州研究院 | A kind of shell core spices and essence microcapsules and preparation method thereof |
| CN108420043A (en) * | 2018-01-29 | 2018-08-21 | 湖北工业大学 | Sodium alginate improves natural oil body dispersibility and its application in salad juice |
| CN108902356A (en) * | 2018-07-26 | 2018-11-30 | 广州利众生物科技有限公司 | A kind of linseed oil, flaxseed gum vegetable fat powder and preparation method thereof |
| CN111480848A (en) * | 2020-05-07 | 2020-08-04 | 河北东康乳业有限公司 | Preparation method of high-embedding-rate multi-layer wall material fat powder |
| CN111802643B (en) * | 2020-07-13 | 2023-04-28 | 沈阳师范大学 | Preparation method of peppermint oil powder grease based on supermolecule grease gel |
| CN113527717B (en) * | 2021-07-28 | 2023-04-28 | 青岛农业大学 | Starch emulsion gel bead and preparation method and application thereof |
| CN117414338B (en) * | 2023-10-09 | 2024-09-27 | 锦州本天药业有限公司 | Preparation process and process production line of compound chlorhexidine powder |
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| FR2824756B1 (en) * | 2001-05-16 | 2005-07-08 | Mainelab | MICROCAPSULES BASED ON PLANT PROTEINS |
| CN101125133B (en) * | 2007-09-27 | 2011-06-01 | 武汉麦可得生物技术有限公司 | Unsaturated fatty acid microcapsule preparing technology and application |
| CN102653704A (en) * | 2011-03-04 | 2012-09-05 | 上海爱普植物科技有限公司 | Preparation method of small peppermint essence soft capsule taking calcium alginate as wall material |
| CN102274280B (en) * | 2011-08-10 | 2013-03-06 | 华南农业大学 | Patchouli oil microcapsules and preparation method and application thereof |
| CN103404955B (en) * | 2013-06-28 | 2015-06-24 | 大连医诺生物有限公司 | Preparation method and device for multilayered embedded particles |
| CN103432970A (en) * | 2013-08-30 | 2013-12-11 | 黑龙江大学 | Method for preparing organic-inorganic composite microcapsule through complex coacervation |
| CN103548995B (en) * | 2013-11-06 | 2015-04-01 | 嘉应学院 | Litsea cubeba oil microcapsule and preparation method thereof |
| CN104209072A (en) * | 2014-09-05 | 2014-12-17 | 南京泽朗生物科技有限公司 | Preparation method of corn linoleic acid microcapsules |
| CN104745566A (en) * | 2015-03-11 | 2015-07-01 | 上海应用技术学院 | Lactic acid bacterium immobilized capsules and preparation method and application thereof |
| CN105165911B (en) * | 2015-07-14 | 2018-08-10 | 浙江理工大学 | The preparation method of schizonepeta essence oil nanometer mosquito repellent microcapsules |
| CN105063118A (en) * | 2015-07-19 | 2015-11-18 | 聊城大学 | Method for increasing lipstatin fermentation units by aid of added linoleic acid sustained-release micro-capsules |
| CN105533691B (en) * | 2015-12-15 | 2019-01-29 | 中国疾病预防控制中心营养与健康所 | A kind of micro/nano level fish oil/algae oil microcapsules and its preparation process |
| CN105533750A (en) * | 2016-01-13 | 2016-05-04 | 吉林大学 | Oviductus ranae microcapsules and preparation method thereof |
| CN105853391B (en) * | 2016-04-25 | 2019-12-10 | 东华大学 | Preparation method of sodium alginate/chitosan/gallnut external antibacterial microcapsule |
| CN106035739B (en) * | 2016-05-23 | 2019-05-17 | 中国农业大学 | A kind of method that LBL self-assembly solidifies linseed oil and its compounds grease |
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| WO2017202104A1 (en) | 2017-11-30 |
| AU2017258935A1 (en) | 2017-12-07 |
| AU2017101823A4 (en) | 2019-05-09 |
| CN106035739A (en) | 2016-10-26 |
| CN106035739B (en) | 2019-05-17 |
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