CN112191199A - Microcapsule for embedding liquid grease and preparation method thereof - Google Patents
Microcapsule for embedding liquid grease and preparation method thereof Download PDFInfo
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- CN112191199A CN112191199A CN202011026569.7A CN202011026569A CN112191199A CN 112191199 A CN112191199 A CN 112191199A CN 202011026569 A CN202011026569 A CN 202011026569A CN 112191199 A CN112191199 A CN 112191199A
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- microcapsule
- sodium alginate
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- liquid oil
- embedding
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- 239000007788 liquid Substances 0.000 title claims abstract description 102
- 239000003094 microcapsule Substances 0.000 title claims abstract description 102
- 239000004519 grease Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 84
- 229920001661 Chitosan Polymers 0.000 claims abstract description 35
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 33
- 239000000661 sodium alginate Substances 0.000 claims abstract description 33
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 33
- 239000011162 core material Substances 0.000 claims abstract description 22
- 239000011257 shell material Substances 0.000 claims abstract description 20
- 238000004132 cross linking Methods 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 4
- 239000003921 oil Substances 0.000 claims description 50
- 235000019198 oils Nutrition 0.000 claims description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 claims description 20
- 235000001815 DL-alpha-tocopherol Nutrition 0.000 claims description 20
- 239000011627 DL-alpha-tocopherol Substances 0.000 claims description 20
- GVJHHUAWPYXKBD-UHFFFAOYSA-N d-alpha-tocopherol Natural products OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims description 20
- 229960000984 tocofersolan Drugs 0.000 claims description 20
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 claims description 20
- 229940117916 cinnamic aldehyde Drugs 0.000 claims description 18
- KJPRLNWUNMBNBZ-UHFFFAOYSA-N cinnamic aldehyde Natural products O=CC=CC1=CC=CC=C1 KJPRLNWUNMBNBZ-UHFFFAOYSA-N 0.000 claims description 18
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 claims description 17
- JBYXPOFIGCOSSB-GOJKSUSPSA-N 9-cis,11-trans-octadecadienoic acid Chemical compound CCCCCC\C=C\C=C/CCCCCCCC(O)=O JBYXPOFIGCOSSB-GOJKSUSPSA-N 0.000 claims description 16
- 229940108924 conjugated linoleic acid Drugs 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 239000003813 safflower oil Substances 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 16
- 238000005469 granulation Methods 0.000 claims description 14
- 230000003179 granulation Effects 0.000 claims description 14
- 239000001110 calcium chloride Substances 0.000 claims description 13
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 13
- 238000005253 cladding Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 235000019197 fats Nutrition 0.000 claims description 8
- 230000006196 deacetylation Effects 0.000 claims description 3
- 238000003381 deacetylation reaction Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 claims description 2
- 235000020661 alpha-linolenic acid Nutrition 0.000 claims description 2
- 229960004488 linolenic acid Drugs 0.000 claims description 2
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 claims description 2
- 235000021388 linseed oil Nutrition 0.000 claims description 2
- 239000000944 linseed oil Substances 0.000 claims description 2
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 claims 1
- 235000020778 linoleic acid Nutrition 0.000 claims 1
- 229960004232 linoleic acid Drugs 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001424 calcium ion Inorganic materials 0.000 abstract description 4
- 239000003208 petroleum Substances 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 abstract description 2
- 239000005003 food packaging material Substances 0.000 abstract 1
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 24
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000011575 calcium Substances 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 230000000968 intestinal effect Effects 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 101100476609 Arabidopsis thaliana SAC4 gene Proteins 0.000 description 1
- 101100041620 Arabidopsis thaliana SAC5 gene Proteins 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 101001025773 Homo sapiens Germinal-center associated nuclear protein Proteins 0.000 description 1
- 101000869523 Homo sapiens Phosphatidylinositide phosphatase SAC2 Proteins 0.000 description 1
- 101000869517 Homo sapiens Phosphatidylinositol-3-phosphatase SAC1 Proteins 0.000 description 1
- 101000827703 Homo sapiens Polyphosphoinositide phosphatase Proteins 0.000 description 1
- 238000012695 Interfacial polymerization Methods 0.000 description 1
- 241000764238 Isis Species 0.000 description 1
- 239000007836 KH2PO4 Substances 0.000 description 1
- 102100032287 Phosphatidylinositide phosphatase SAC2 Human genes 0.000 description 1
- 102100032286 Phosphatidylinositol-3-phosphatase SAC1 Human genes 0.000 description 1
- 102100023591 Polyphosphoinositide phosphatase Human genes 0.000 description 1
- 102000004142 Trypsin Human genes 0.000 description 1
- 108090000631 Trypsin Proteins 0.000 description 1
- AXMVYSVVTMKQSL-UHFFFAOYSA-N UNPD142122 Natural products OC1=CC=C(C=CC=O)C=C1O AXMVYSVVTMKQSL-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 150000003385 sodium Chemical class 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000012588 trypsin Substances 0.000 description 1
Images
Classifications
-
- 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
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
-
- 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
-
- 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
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The invention discloses a microcapsule for embedding liquid grease by taking sodium alginate/chitosan as a shell material and a preparation method thereof. The microcapsule uses liquid oil as core material, water-soluble sodium alginate and Ca2+And (3) performing crosslinking to obtain an intermediate layer, performing crosslinking of chitosan and water-soluble sodium alginate to obtain an outer shell layer, and preparing the microcapsule by using a microcapsule granulator. The average particle size of the microcapsule prepared by the invention is about 500 mu m, the microcapsule presents an obvious multilayer structure, has excellent mechanical property, oxidation resistance and slow release performance, realizes the controllable load of liquid grease, realizes the effective protection of functional grease by natural, nontoxic and degradable natural food packaging materials, and replaces petroleum-based synthetic plastics.
Description
Technical Field
The invention relates to the field of high polymer materials, and particularly relates to a microcapsule for embedding liquid grease by taking sodium alginate/chitosan as a shell material and a preparation method thereof.
Background
The microcapsule technology is a kind of protection technology, and is characterized by that it utilizes natural or synthetic high-molecular material to wrap some substances with reactivity, volatility or sensitivity to form fine granules. The substance encapsulated in the microcapsule is called a core material, and the material encapsulated in the microcapsule is called a shell material (or wall material). Microcapsule technology is also known as a protective technology, and can play a role in protecting the core material by virtue of the shielding effect of the capsule wall. The product prepared by the microcapsule technology has good functionality and storage stability, is convenient to use, and can solve a plurality of problems which cannot be solved in the traditional process. However, the existing microcapsule for embedding liquid oil and fat comprises a spray drying method, an electrostatic combination method and an interfacial polymerization method, and has a plurality of immature parts, some key problems still need to be solved, such as the defects of liquid oil and fat leakage, single function, difficult realization of controlled release and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing the microcapsule for embedding the liquid oil by taking the sodium alginate/chitosan as the shell material and the preparation method thereof, aiming at the defects in the prior art, the obtained microcapsule has good mechanical property, oxidation resistance and slow release property, and the controllable load of the liquid oil is realized.
The technical scheme adopted by the invention for solving the problems is as follows:
a microcapsule for embedding liquid oil comprises core material as liquid oil, modified sodium alginate and Ca2+Crosslinking to form gel as a middle cladding, and taking the modified sodium alginate and the chitosan together as an external shell material; wherein, the modified sodium alginate is obtained by blending and modifying cinnamyl aldehyde and DL-alpha-tocopherol in solvent water.
According to the scheme, the average particle size of the microcapsule is 150-900 microns.
The preparation method of the microcapsule for embedding the liquid grease mainly comprises the following steps:
(1) mixing sodium alginate, cinnamaldehyde and DL-alpha-tocopherol in solvent water to obtain a modified sodium alginate solution;
(2) selecting liquid grease as a core material;
(3) chitosan and CaCl2Mixing in solvent water to obtain a solidified liquid;
(4) and (2) introducing the modified sodium alginate solution obtained in the step (1) into a shell material inlet of a microcapsule granulation instrument, introducing the liquid oil in the step 2) into a core material inlet of the microcapsule granulation instrument, allowing the modified sodium alginate solution and the liquid oil to flow through a concentric nozzle to pre-form an intermediate coating layer, and then jointly spraying the intermediate coating layer and the intermediate coating layer into the curing liquid in the step (3) to form a microcapsule, wherein the microcapsule is the microcapsule for embedding the liquid oil.
Further, in the step 1), the mass fraction of sodium alginate in the modified sodium alginate solution is 0.5-5%, the mass fraction of cinnamaldehyde is 0.25-1.25%, and the mass fraction of DL-alpha-tocopherol is 0.2-1.0%.
Further, in the step 2), the liquid oil may be safflower seed oil, linseed oil, conjugated linoleic acid, linolenic acid, and the like. Furthermore, the liquid oil adopts safflower seed oil and conjugated linoleic acid, and the mass ratio of the safflower seed oil to the conjugated linoleic acid is 1: 1-9: 1.
Further, the mass fraction of chitosan in the curing liquid in the step 3) is 0.5-5.0%, and CaCl is added2The mass fraction is 1.0-5.0%. Wherein the chitosan is water-soluble chitosan, and the deacetylation degree is more than 85%.
Further, in the step 4), the volume ratio of the modified sodium alginate solution to the liquid oil is (1.5-2.5): 1, preferably 2: 1.
further, in the step 4), the volume of the curing liquid is 1-3 times of the sum of the volumes of the modified sodium alginate and the liquid grease, and the curing time is 30-120 minutes.
Further, in the step 4), the diameter of a concentric nozzle of the microcapsule granulator is 300-900 μm, the frequency of a vibration unit is 1000-3000 Hz, the voltage of an electrode is 500-1500V, the air pressure is 150-300 mbar, and the flow rate is 5-10 mL/min. In the step, a modified sodium alginate solution and liquid grease are sprayed from a concentric nozzle and do not contact with a solidifying solution to primarily form a microcapsule with a middle cladding structure, wherein the shell layer is the modified sodium alginate, and the core material isIs liquid grease; after contacting the curing liquid, modifying sodium alginate and Ca2+Reacting and curing, reacting and crosslinking the chitosan and the modified sodium alginate to form the microcapsule again, wherein the core material liquid grease, the middle cladding layer modified sodium alginate and the Ca are sequentially arranged from inside to outside2+A cross-linked gel layer, an outer shell layer chitosan and a cross-linked layer of modified sodium alginate. In addition, the microcapsule granulator can change nozzles with different calibers, and the size of the microcapsule can be adjusted.
Compared with the prior art, the invention has the beneficial effects that:
firstly, the invention also solves the problem of easy leakage of the liquid oil microcapsule, the sodium alginate calcium ion is crosslinked to form a reticular middle layer as a framework to ensure that the microcapsule is not easy to deform, the sodium alginate and the chitosan are crosslinked to form a compact structure to coat the outermost layer of the microcapsule, the microcapsule can be effectively prevented from breaking and the leakage of the liquid oil in the core material, and simultaneously, the sodium alginate and the Ca are crosslinked to form a compact structure to coat the outermost layer of the microcapsule2+The intermediate layer formed by crosslinking forms a spherical skeleton, and the spherical structure of the microcapsule is packaged.
Secondly, the microcapsule prepared by the invention has good oxidation resistance and long-acting release function, and the controllable load of the liquid grease is realized. The embedding method provided by the invention expands the construction method of the microcapsule with a multilayer structure, compared with the microcapsule with a single structure, the microcapsule with the multilayer structure breaks through the definition of the shell material of the microcapsule in the traditional sense, chitosan and water-soluble sodium alginate are crosslinked to be used as the outer shell layer, and water-soluble sodium alginate and Ca are used as the outer shell layer2+The intermediate layer is formed by crosslinking, the compact chitosan layer makes up the defects of leakage and poor mechanical property of the sodium alginate, the sodium alginate is chemically modified, and the purpose of prolonging the shelf life is achieved by a physicochemical combination means. In order to solve the problem of liquid oil deterioration, the invention uses a construction method combining chemical protection and physical protection to prepare the multilayer structure microcapsule which takes sodium alginate/chitosan as a shell material to embed the liquid oil. In the aspect of a chemical protection method, sodium alginate and chitosan are used as raw materials, and cinnamaldehyde and DL-alpha-tocopherol are used for modifying the sodium alginate, so that the sodium alginate has excellent oxidation resistance; in the aspect of physical protection method, chitosan is on the surface of modified sodium alginateA compact protective film is formed, and the function of blocking bacteria and oxygen is achieved.
Thirdly, the invention provides a new solution for sodium alginate and chitosan as food packaging delivery materials, namely a multilayer protection and physicochemical combination means, belongs to cheap and environment-friendly materials, can be widely applied to embedding and delivery of functional grease, effectively protects the functional grease, and replaces petroleum-based synthetic plastics.
Drawings
FIG. 1 is a schematic diagram of the preparation process and structure of the microcapsule of the present invention.
FIG. 2 is a scanning electron micrograph of the microcapsules obtained in example 1.
Fig. 3 is a graph showing the antioxidant property test of the microcapsules obtained in example 1.
Fig. 4 is a simulated intestinal fluid release kinetics of the microcapsules obtained in example 1.
Detailed description of the invention
For better understanding of the technical problems, technical solutions and technical effects solved by the present invention, the following detailed description of the present invention is provided with reference to the accompanying drawings and embodiments, but should not be construed as limiting the present invention.
In the following examples, all chitosans were water-soluble chitosans, with a degree of deacetylation of greater than 85%; the viscosity of the sodium alginate is 200 +/-20 mPa.s. The microcapsule granulator is BUCHI, and model B-390.
Example 1
A preparation method of microcapsules for embedding liquid grease comprises the following specific steps:
(1) mixing sodium alginate, cinnamaldehyde and DL-alpha-tocopherol in solvent water to obtain a modified sodium alginate solution; wherein the mass fractions of sodium alginate, cinnamaldehyde and DL-alpha-tocopherol are respectively 1.5%, 0-1.0% (respectively 0, 0.2%, 0.4%, 0.6%, 0.8%, 1.0%) and 0-1.25% (respectively 0, 0.25%, 0.50%, 0.75%, 1.0%, 1.25%), as shown in Table 1;
(2) selecting a mixture of safflower seed oil and conjugated linoleic acid as a core material, wherein the mass ratio of the safflower seed oil to the conjugated linoleic acid is 9: 1;
(3) chitosan and CaCl2Mixing in solvent water to obtain a solidified liquid; in the curing liquid, the concentrations of chitosan and calcium chloride are respectively 1% and 3%;
(4) and (2) introducing the modified sodium alginate solution obtained in the step (1) into a shell material inlet of a microcapsule granulation instrument, introducing the liquid oil in the step (2) into a core material inlet of the microcapsule granulation instrument, wherein the volume ratio of the modified sodium alginate to the liquid oil is 2:1, allowing the modified sodium alginate to flow through a concentric nozzle to pre-form an intermediate cladding structure, then jointly spraying the intermediate cladding structure into the curing liquid (the curing liquid is the sum of the volumes of the modified sodium alginate and the liquid oil) in the step (3), and curing for 10 minutes in solid-liquid to obtain a multilayer-structure microcapsule, and washing the multilayer-structure microcapsule for multiple times (more than 5 times) by using deionized water to obtain. In the step, the caliber of a concentric nozzle of the microcapsule granulator is 400 microns, the frequency of a vibration unit is 1000Hz, the electrode voltage is 500V, the air pressure is 200mbar, and the flow rate is 7-8 mL/min.
FIG. 2 is a scanning electron micrograph of the microcapsule with multilayer structure prepared in example 1, and the average particle size is 500 μm.
FIG. 3 is a graph showing the antioxidant property of the multi-layered microcapsule of example 1, in which cinnamaldehyde and DL-alpha-tocopherol are added in amounts shown in SAC0-5 in FIG. 2, as shown in Table 1 below. As shown in FIG. 2, the SCA2-5 has strong oxidation resistance.
FIG. 4 is a graph showing simulated intestinal fluid release kinetics of the microcapsules of example 1 having a multi-layer structure. Wherein 6.8g KH2PO4 and 10g trypsin were dissolved in deionized water and made up to volume in a 1L volumetric flask to prepare a simulated intestinal fluid, pH 7.5. As can be seen from fig. 3, the microcapsule to which cinnamaldehyde and DL- α -tocopherol are added has a long-lasting release effect.
TABLE 1
| SAC0 | SAC1 | SAC2 | SAC3 | SAC4 | SAC5 | |
| DL-alpha-tocopherol (w%) | 0 | 0.2 | 0.4 | 0.6 | 0.8 | 1.0 |
| Cinnamic aldehyde (w%) | 0％ | 0.25 | 0.5 | 0.75 | 1.0 | 1.25 |
Example 2
A preparation method of microcapsules for embedding liquid grease comprises the following specific steps:
(1) mixing sodium alginate, cinnamaldehyde and DL-alpha-tocopherol in solvent water to obtain a modified sodium alginate solution; wherein the mass fractions of sodium alginate, cinnamaldehyde and DL-alpha-tocopherol are respectively 1.5%, 0.4% and 0.5%;
(2) selecting a mixture of safflower seed oil and conjugated linoleic acid as a core material, wherein the mass ratio of the safflower seed oil to the conjugated linoleic acid is 7: 1;
(3) chitosan and CaCl2Mixing in solvent water to obtain a solidified liquid; in the curing liquid, the concentrations of chitosan and calcium chloride are respectively 1% and 3%;
(4) and (2) introducing the modified sodium alginate solution obtained in the step (1) into a shell material inlet of a microcapsule granulation instrument, introducing the liquid oil in the step (2) into a core material inlet of the microcapsule granulation instrument, wherein the volume ratio of the modified sodium alginate to the liquid oil is 2:1, allowing the modified sodium alginate to flow through a concentric nozzle to pre-form an intermediate cladding structure, injecting the modified sodium alginate and the liquid oil together into the curing liquid (the sum of the volumes of the modified sodium alginate and the liquid oil) in the step (3), curing for 20 minutes in the solid liquid to obtain a multi-layer structure microcapsule, and washing the multi-layer structure microcapsule for more than 5 times by using deionized water to obtain the multi-layer structure microcapsule. In the step, the caliber of a concentric nozzle of the microcapsule granulator is 500 micrometers, the frequency of a vibration unit is 1500Hz, the electrode voltage is 500V, the air pressure is 200mbar, and the flow rate is 5-6 mL/min.
Example 3
A preparation method of microcapsules for embedding liquid grease comprises the following specific steps:
(1) mixing sodium alginate, cinnamaldehyde and DL-alpha-tocopherol in solvent water to obtain a modified sodium alginate solution; wherein the mass fractions of sodium alginate, cinnamaldehyde and DL-alpha-tocopherol are respectively 1.5%, 0.6% and 0.75%;
(2) selecting a mixture of safflower seed oil and conjugated linoleic acid as a core material, wherein the mass ratio of the safflower seed oil to the conjugated linoleic acid is 7: 1;
(3) chitosan and CaCl2Mixing in solvent water to obtain a solidified liquid; in the curing liquid, the concentrations of chitosan and calcium chloride are respectively 1% and 3%;
(4) and (2) introducing the modified sodium alginate solution obtained in the step (1) into a shell material inlet of a microcapsule granulation instrument, introducing the liquid oil in the step (2) into a core material inlet of the microcapsule granulation instrument, wherein the volume ratio of the modified sodium alginate to the liquid oil is 2:1, allowing the modified sodium alginate to flow through a concentric nozzle to pre-form an intermediate cladding structure, injecting the modified sodium alginate and the liquid oil together into the curing liquid (the sum of the volumes of the modified sodium alginate and the liquid oil) in the step (3), curing for 20 minutes in the solid liquid to obtain a multi-layer structure microcapsule, and washing the multi-layer structure microcapsule for more than 5 times by using deionized water to obtain the multi-layer structure microcapsule. In the step, the caliber of a concentric nozzle of the microcapsule granulator is 500 micrometers, the frequency of a vibration unit is 1500Hz, the electrode voltage is 500V, the air pressure is 200mbar, and the flow rate is 9-10 mL/min.
Example 4
A preparation method of microcapsules for embedding liquid grease comprises the following specific steps:
(1) mixing sodium alginate, cinnamaldehyde and DL-alpha-tocopherol in solvent water to obtain a modified sodium alginate solution; wherein the mass fractions of sodium alginate, cinnamaldehyde and DL-alpha-tocopherol are respectively 1.5%, 0.8% and 1.0%;
(2) selecting a mixture of safflower seed oil and conjugated linoleic acid as a core material, wherein the mass ratio of the safflower seed oil to the conjugated linoleic acid is 7: 1;
(3) chitosan and CaCl2Mixing in solvent water to obtain a solidified liquid; in the curing liquid, the concentrations of chitosan and calcium chloride are respectively 1% and 3%;
(4) and (2) introducing the modified sodium alginate solution obtained in the step (1) into a shell material inlet of a microcapsule granulation instrument, introducing the liquid oil in the step (2) into a core material inlet of the microcapsule granulation instrument, wherein the volume ratio of the modified sodium alginate to the liquid oil is 2:1, allowing the modified sodium alginate to flow through a concentric nozzle to pre-form an intermediate cladding structure, injecting the modified sodium alginate and the liquid oil together into the curing liquid (the sum of the volumes of the modified sodium alginate and the liquid oil) in the step (3), curing for 20 minutes in the solid liquid to obtain a multi-layer structure microcapsule, and washing the multi-layer structure microcapsule for more than 5 times by using deionized water to obtain the multi-layer structure microcapsule. In the step, the caliber of a concentric nozzle of the microcapsule granulator is 900 micrometers, the frequency of a vibration unit is 1500Hz, the electrode voltage is 500V, the air pressure is 200mbar, and the flow rate is 7-8 mL/min.
Example 5
A preparation method of microcapsules for embedding liquid grease comprises the following specific steps:
(1) mixing sodium alginate, cinnamaldehyde and DL-alpha-tocopherol in solvent water to obtain a modified sodium alginate solution; wherein the mass fractions of sodium alginate, cinnamaldehyde and DL-alpha-tocopherol are respectively 1.5%, 1.0% and 1.25%;
(2) selecting a mixture of safflower seed oil and conjugated linoleic acid as a core material, wherein the mass ratio of the safflower seed oil to the conjugated linoleic acid is 5: 1;
(3) chitosan and CaCl2Mixing in solvent water to obtain a solidified liquid; in the curing liquid, the concentrations of chitosan and calcium chloride are respectively 1% and 3%;
(4) and (2) introducing the modified sodium alginate solution obtained in the step (1) into a shell material inlet of a microcapsule granulation instrument, introducing the liquid oil in the step (2) into a core material inlet of the microcapsule granulation instrument, wherein the volume ratio of the modified sodium alginate to the liquid oil is 2:1, allowing the modified sodium alginate to flow through a concentric nozzle to pre-form an intermediate cladding structure, injecting the intermediate cladding structure and the liquid oil into the curing liquid (the sum of the volumes of the modified sodium alginate and the liquid oil) in the step (3) together, curing for 20 minutes in the solid liquid to obtain microcapsules with a multi-layer structure, and washing the microcapsules with deionized water for multiple times (more than 5 times) to obtain the microcapsules with the multi-. In the step, the caliber of a concentric nozzle of the microcapsule granulator is 300 microns, the frequency of a vibration unit is 1500Hz, the electrode voltage is 500V, the air pressure is 200mbar, and the flow rate is 7-8 mL/min.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the protection scope of the present invention.
Claims (10)
1. A microcapsule for embedding liquid oil is characterized in that a core material is used as the liquid oil, and modified sodium alginate and Ca are used2+Crosslinking to form gel as a middle cladding, and taking the modified sodium alginate and the chitosan together as an external shell material; wherein, the modified sodium alginate is obtained by blending and modifying cinnamyl aldehyde and DL-alpha-tocopherol in solvent water.
2. The microcapsule according to claim 1, wherein the average particle size of the microcapsule is 150 to 900 μm.
3. A preparation method of microcapsules for embedding liquid grease is characterized by comprising the following steps:
(1) mixing sodium alginate, cinnamaldehyde and DL-alpha-tocopherol in solvent water to obtain a modified sodium alginate solution;
(2) selecting liquid grease as a core material;
(3) chitosan and CaCl2Mixing in solvent water to obtain a solidified liquid;
(4) and (2) introducing the modified sodium alginate solution obtained in the step (1) into a shell material inlet of a microcapsule granulation instrument, introducing the liquid oil in the step 2) into a core material inlet of the microcapsule granulation instrument, allowing the modified sodium alginate solution and the liquid oil to flow through a concentric nozzle to pre-form an intermediate cladding structure, and then jointly spraying the intermediate cladding structure and the liquid oil into the curing liquid in the step (3) to form a microcapsule, wherein the microcapsule is the microcapsule for embedding the liquid oil.
4. The method for preparing microcapsules for embedding liquid oil and fat as claimed in claim 3, wherein in step 1), the mass fraction of sodium alginate in the modified sodium alginate solution is 0.5-5%, the mass fraction of cinnamaldehyde is 0.25-1.25%, and the mass fraction of DL-alpha-tocopherol is 0.2-1.0%.
5. The method for preparing microcapsules for embedding liquid oil according to claim 3, wherein in the step 2), the liquid oil is one or more of safflower seed oil, linseed oil, conjugated linoleic acid, linoleic acid and linolenic acid.
6. The preparation method of the microcapsule embedding liquid oil and fat as claimed in claim 5, wherein the liquid oil and fat adopts safflower seed oil and conjugated linoleic acid, and the mass ratio of the safflower seed oil to the conjugated linoleic acid is 1: 1-9: 1.
7. The method for preparing the microcapsule embedding the liquid oil and fat according to claim 3, wherein the mass fraction of the chitosan in the curing liquid in the step 3) is 0.5-5.0％，CaCl2The mass fraction is 1.0-5.0%; wherein the chitosan is water-soluble chitosan, and the deacetylation degree is more than 85%.
8. The preparation method of the microcapsule embedding liquid oil and fat according to claim 3, wherein in the step 4), the volume ratio of the modified sodium alginate solution to the liquid oil and fat is (1.5-2.5): 1.
9. the preparation method of the microcapsule embedding liquid grease as claimed in claim 3, wherein in the step 4), the volume of the curing liquid is 1-3 times of the sum of the volumes of the modified sodium alginate and the liquid grease, and the curing time is 30-120 minutes.
10. The method for preparing the microcapsule with the three-layer structure for embedding the liquid oil according to claim 3, wherein in the step 4), the diameter of a concentric nozzle of a microcapsule granulator is 300-900 μm, the frequency of a vibration unit is 1000-3000 Hz, the voltage of an electrode is 500-1500V, the air pressure is 150-300 mbar, and the flow rate is 5-10 mL/min.
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