CN112205628A - Composite condensate with double embedding functions and preparation method and application thereof - Google Patents
Composite condensate with double embedding functions and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 72
- 229920002494 Zein Polymers 0.000 claims abstract description 51
- 239000005019 zein Substances 0.000 claims abstract description 51
- 229940093612 zein Drugs 0.000 claims abstract description 51
- 229940109262 curcumin Drugs 0.000 claims abstract description 42
- VFLDPWHFBUODDF-FCXRPNKRSA-N curcumin Chemical compound C1=C(O)C(OC)=CC(\C=C\C(=O)CC(=O)\C=C\C=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-FCXRPNKRSA-N 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 29
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 claims abstract description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229920001661 Chitosan Polymers 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012296 anti-solvent Substances 0.000 claims abstract description 18
- 229960001285 quercetin Drugs 0.000 claims abstract description 18
- 235000012754 curcumin Nutrition 0.000 claims abstract description 15
- 239000004148 curcumin Substances 0.000 claims abstract description 15
- VFLDPWHFBUODDF-UHFFFAOYSA-N diferuloylmethane Natural products C1=C(O)C(OC)=CC(C=CC(=O)CC(=O)C=CC=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 claims abstract description 14
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 claims abstract description 14
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 235000005875 quercetin Nutrition 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000013305 food Nutrition 0.000 claims abstract description 6
- 230000000887 hydrating effect Effects 0.000 claims abstract description 6
- 238000012545 processing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 7
- 230000006196 deacetylation Effects 0.000 claims description 3
- 238000003381 deacetylation reaction Methods 0.000 claims description 3
- 230000036571 hydration Effects 0.000 claims description 3
- 238000006703 hydration reaction Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 7
- 239000000126 substance Substances 0.000 abstract description 6
- 239000002245 particle Substances 0.000 description 35
- 150000008442 polyphenolic compounds Chemical class 0.000 description 19
- 235000013824 polyphenols Nutrition 0.000 description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 229920001282 polysaccharide Polymers 0.000 description 14
- 239000005017 polysaccharide Substances 0.000 description 14
- 108090000623 proteins and genes Proteins 0.000 description 13
- 102000004169 proteins and genes Human genes 0.000 description 13
- 150000004676 glycans Chemical class 0.000 description 10
- 239000011246 composite particle Substances 0.000 description 9
- 230000003993 interaction Effects 0.000 description 9
- 230000002209 hydrophobic effect Effects 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 235000016709 nutrition Nutrition 0.000 description 5
- 229920001222 biopolymer Polymers 0.000 description 3
- 239000003623 enhancer Substances 0.000 description 3
- 230000035764 nutrition Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000002864 food coloring agent Nutrition 0.000 description 2
- 239000000576 food coloring agent Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
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- 238000002390 rotary evaporation Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 102000011632 Caseins Human genes 0.000 description 1
- 108010076119 Caseins Proteins 0.000 description 1
- 239000005714 Chitosan hydrochloride Substances 0.000 description 1
- 108010061711 Gliadin Proteins 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
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- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000000707 layer-by-layer assembly Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
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- 230000001105 regulatory effect Effects 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/17—Amino acids, peptides or proteins
- A23L33/185—Vegetable proteins
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- 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
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- 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
- A23L5/42—Addition of dyes or pigments, e.g. in combination with optical brighteners
- A23L5/43—Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
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- 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
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Abstract
The invention discloses a complex condensate with double embedding functions and a preparation method and application thereof. The preparation method comprises the following steps: (1) adding zein into an ethanol water solution, and stirring and dissolving to obtain a zein solution; (2) adding chitosan into an acetic acid solution, stirring for dissolving, and then hydrating overnight to obtain a chitosan anti-solvent solution; (3) adding curcumin and quercetin into a Zein solution, uniformly stirring and mixing, and hydrating overnight to obtain a Zein-Cur-Que mixed solution; (4) adding the chitosan anti-solvent solution into the Zein-Cur-Que mixed solution, stirring and mixing uniformly, then removing ethanol by rotary heating, and adjusting the pH value to 3.0-7.0 to obtain the composite condensate with the double embedding function. The complex coacervate of the invention simultaneously embeds two substances with different polarities, has high embedding rate and high bioavailability, and can be used in the field of food processing.
Description
Technical Field
The invention belongs to the field of modern health food processing, and particularly relates to a composite coacervate with a double-embedding function, and a preparation method and application thereof.
Background
Nanoparticles as biopolymers for delivering functional ingredients such as curcumin (Cur) have attracted considerable interest to researchers. In particular, proteins and polysaccharides are suitable materials as a nano-delivery system due to their good biocompatibility, biodegradability, non-antigenicity and low toxicity. Therefore, an increasing number of researchers are working on studying the biological significance of the system formed by protein-polysaccharide interactions and exploring the potential for the application of protein-polysaccharide complexes. The complex is formed primarily by electrostatic interactions between anionic and cationic biopolymers, followed by hydrophobic interactions, hydrogen bonding and steric interactions. Furthermore, the interaction between oppositely charged biopolymers is directly controlled by its own degree of ionization, and thus pH is an important factor for electrostatic control. The pH-induced interactions between proteins and polysaccharides have been extensively studied.
Zein (Zein) is a natural food-grade protein with great potential for micro-or nanostructures for drug and biological activity delivery due to its amphiphilic and self-assembling capabilities. Zein is based on the fact that it is rich in hydrophobic amino acids, so it is poorly soluble in water, but readily soluble in ethanol over a range of concentrations. This property makes zein a suitable delivery system material that can be used to encapsulate hydrophobic bioactive ingredients. However, most of the research has focused mainly on nanoparticles formed between water-soluble proteins and water-soluble polysaccharides.
The research on the protein-polysaccharide interaction at home and abroad mainly focuses on a nano delivery system formed by water-soluble protein and water-soluble polysaccharide. To our knowledge, studies on coacervate formation by alcohol-soluble proteins and water-soluble polysaccharides have been rarely reported. Recent studies have shown that alcohol-soluble proteins can be converted into water-soluble nanoparticles by an anti-solvent method, and then further stabilized using polysaccharides. Studies have shown that the stability of gliadin nanoparticles can be improved by pectin coating. The authors indicate that the polysaccharide/zein composite nanoparticles have improved pH and ionic stability. The influence of sodium caseinate and chitosan hydrochloride on the stability of thymol-zein nanoparticles is researched by scientific research teams. However, the delivery system of complex coacervates of alcohol-soluble proteins and water-soluble polysaccharides has been less studied.
At present, the research on protein-polysaccharide interaction at home and abroad is mainly focused on a nano conveying system formed by water-soluble protein and water-soluble polysaccharide, the research on the conveying system of a complex coacervate formed by alcohol-soluble protein and water-soluble polysaccharide is less, most of the research is limited to embedding a substance, and the report that substances with different polarities are embedded in the same conveying system is less.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a complex coacervate with double embedding functions.
The invention also aims to provide the complex coacervate with double embedding functions prepared by the method.
It is still another object of the present invention to provide the use of the complex coacervate with double embedding function.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a complex coacervate with double embedding functions comprises the following steps:
(1) adding zein into an ethanol water solution, and stirring and dissolving to obtain a zein solution;
(2) adding chitosan into an acetic acid solution, stirring for dissolving, and then hydrating overnight to obtain a chitosan anti-solvent solution;
(3) adding curcumin (Cur) and quercetin (Que) into the Zein solution obtained in the step (1), uniformly stirring and mixing, and hydrating overnight to obtain a Zein-curcumin-quercetin mixed solution (Zein-Cur-Que mixed solution);
(4) adding the chitosan anti-solvent solution obtained in the step (2) into the zein-curcumin-quercetin mixed solution obtained in the step (3), stirring and mixing uniformly, then rotating and heating to remove ethanol, and adjusting the pH value to 3.0-7.0 to obtain the ZCsNPs-Cur-Que composite coacervate, namely the composite coacervate with the double embedding function.
The ethanol water solution in the step (1) is 65-85% of ethanol water solution by volume percentage; preferably 80% by volume of ethanol in water.
The concentration of the zein solution in the step (1) is 10-30 mg/mL; preferably 20 mg/mL.
The mass ratio of the chitosan to the zein in the step (2) is 0.4-0.8: 2; preferably 0.7: 2.
The acetic acid solution in the step (2) is 0.8-1.2% by volume; preferably 1% by volume acetic acid solution.
The chitosan in the step (2) is chitosan with the molecular weight of 300kDa and the deacetylation degree of 95 percent.
The concentration of the chitosan anti-solvent solution in the step (2) is 0.8-1.2 mg/mL; preferably 1 mg/mL.
The temperature of the overnight hydration in the steps (2) and (3) is 0-6 ℃; preferably 4 deg.c.
The mass ratio of the total mass of the curcumin and the quercetin to the zein in the step (3) is 1: 5-20; preferably 1: 20.
The mass ratio of the curcumin to the quercetin in the step (3) is 1-4: 1-4; preferably 1: 1.
The rotating speed of stirring in the step (3) is 500-800 rpm; preferably 600 rpm.
The stirring conditions in the step (4) are as follows: stirring at 500-800 rpm for 1-3 min; preferably: stirring at 600rpm for 2 min.
The rotary heating conditions in the step (4) are as follows: rotating and heating at 70-90 rpm and 50-65 ℃ for 8-15 min; preferably: rotating and heating at 88rpm and 55 ℃ for 12 min.
The pH value is preferably adjusted to 3.0-6.5 in the step (4); more preferably, the pH value is adjusted to 4.0-5.0.
A complex coacervate with double embedding function, prepared by any one of the above-mentioned methods.
The complex coacervate with double embedding functions is applied to the field of food processing.
The food processing field comprises the aspects of being used as a nutrition enhancer and/or being used as a food coloring agent, and the like.
Compared with the prior art, the invention has the following advantages and effects:
(1) the invention discloses a preparation method of a zein-curcumin-quercetin-chitosan composite particle with a double-embedded hierarchical structure for the first time, which comprises the steps of loading two components with different polarities (curcumin and quercetin are taken as examples) by utilizing hydrophobic zein, further performing interaction with hydrophilic polysaccharide-chitosan, and further forming a composite condensate of a layer-by-layer assembly structure; the zein has rich sources and certain nutritional value, hydrophobic protein is converted into hydrophilic particles by an anti-solvent method, active ingredients are embedded in the hydrophilic particles, and the composite particles are further stabilized by chitosan, so that the nutritional value and the application value of the zein are further improved, and the zein has the potential of being used as a nutrition enhancer.
(2) The invention adopts the multi-core embedding technology to realize the embedding and carrying of two or more than two components with different polarities in a composite system, the components with different molecular properties can be distributed in each area of a core-shell system after complex coacervation to form a hierarchical structure, the protection and release effects on each active component are realized, the biological stability among the components is enhanced, the synergistic effect is achieved, and the interaction can be generated among the embedding substances, thereby improving the embedding efficiency.
(3) The hierarchical complex coacervate obtained by the invention has pH responsiveness and can be applied to foods with different pH ranges.
(4) The particle size of the hierarchical composite condensate which is prepared by embedding two substances with different polarities simultaneously has controllability, and the particle size of the composite particles can be regulated and controlled by the mass ratio of the zein to the total polyphenol, the mass ratio of the two polyphenols and the pH value (the pH range is 3.0-7.0) of a system, so that the composite particles with different sizes and structures can be formed.
(5) The zein-curcumin-quercetin-chitosan composite coacervate prepared by the method can be used for simultaneously embedding two substances with different polarities, has higher embedding rate, can be used as a nutrition enhancer to improve the bioavailability of hydrophobic active substances, and can also be used as a safe and effective food coloring agent to endow food with colorful colors.
Drawings
FIG. 1 is a graph of particle size and PDI of ZCsNPS-Cur-Que complex aggregates at different pH values.
FIG. 2 is a potential diagram of ZCsNPS-Cur-Que complex aggregates at different pH values.
FIG. 3 is an off-field scanning electron micrograph of a ZCsNPS-Cur-Que complex aggregate.
FIG. 4 is a graph showing the embedding rate of ZCsNPS-Cur-Que complex aggregates at different pH values and the particle size and PDI of ZCsNPS-Cur-Que complex aggregates at different mass mixing ratios (total amount of zein: polyphenols) at different pH values.
FIG. 5 is a graph showing particle diameters and PDI of ZCsNPS-Cur-Que complex aggregates at different mass mixing ratios (Zein: Cur & Que) at a pH of 4.0.
FIG. 6 is a graph showing particle diameters and PDI of ZCsNPS-Cur-Que complex aggregates at different mass mixing ratios (Zein: Cur & Que) at a pH of 5.0.
Fig. 7 is Zein: particle diameter and PDI of ZCsNPS-Cur-Que complex aggregates with different mass mixing ratios (Cur: Que) at a pH value of 4.0 at a mass ratio of Cur & Que of 20: 1.
Fig. 8 is Zein: particle diameter and PDI of ZCsNPS-Cur-Que complex aggregates with different mass mixing ratios (Cur: Que) at a pH value of 5.0 at a mass ratio of Cur & Que of 20: 1.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated. The test methods in the following examples, in which specific experimental conditions are not specified, are generally performed according to conventional experimental conditions or according to the experimental conditions recommended by the manufacturer. Unless otherwise specified, reagents and starting materials for use in the present invention are commercially available.
Example 1
(1) Preparation of 2% Zein solution (Zein):
0.2g of Zein (purchased from Sigma Aldrich inc., USA) was dissolved in 10mL of 80% (v/v) aqueous ethanol and stirred in a magnetic stirrer until the solution was clear to make a 2% (20mg/mL) solution of Zein.
(2) Preparation of chitosan (Cs) anti-solvent solution:
0.07g of chitosan (molecular weight about 300 kDa; degree of deacetylation 95%) was dissolved in 70mL of 1% (v/v) acetic acid solution, stirred with a magnetic stirrer until the solution was clear to give a 0.1% (1mg/mL) Cs antisolvent solution, and left to hydrate in a refrigerator at 4 ℃ overnight.
(3) Preparation of ZCsNPS-Cur-Que complex coacervate:
firstly, fixing the weight ratio of zein to the total weight of two polyphenols (curcumin and quercetin) to be 20:1, wherein the weight ratio of curcumin (Cur) to quercetin (Que) is 1: 1. Weighing a certain amount of curcumin and quercetin, dissolving in a 2% Zein solution, namely adding 0.01g (0.005g of Cur and 0.005g of Que) of two polyphenols into 10mL of a 2% Zein solution which is stirred in a magnetic stirrer, stirring at the speed of 600rpm, stirring the solution until the solution is clear, preparing a Zein-Cur-Que mixed solution, and placing the mixed solution in a refrigerator at 4 ℃ for overnight hydration.
② when preparing the ZCsNPS-Cur-Que complex condensate, rapidly pouring the Cs anti-solvent solution into the Zein-Cur-Que solution which is stirred on a magnetic stirrer, stirring at the speed of 600rpm for 2min, transferring the mixed solution to a rotary evaporation bottle, heating for 12min under the conditions of 88rpm and 55 ℃, and completely evaporating ethanol to obtain the ZCsNPS-Cur-Que complex condensate.
(4) Morphology, particle size, PDI, potential and embedding rate of ZCsNPs-Cur-Que composite condensate
The ZCsNPs-Cur-Que composite condensate is adjusted to a series of pH values with a range of 3.0-7.0 and a gradient of 0.5 by using 1M HCl solution and 1M NaOH solution; measuring the particle size, the particle size distribution index PDI and the potential of the particle size by using a Zen-3690 Malvern particle size and potential analyzer; observing the morphological characteristics of the composite condensate by adopting a JSM-7001F off-site emission electron microscope; several complex coacervates with pH representatives were selected for their encapsulation efficiency, pH 3.0, 3.5, 4.0, 5.0 and 7.0, respectively.
The results are shown in FIGS. 1 to 4:
as shown in FIG. 1, the particle size and PDI of the ZCsNPS-Cur-Que complex condensate are both less than 400nm in a wide range of pH 3.0-6.5, and when the pH is 7.0, the particle size reaches the maximum value and exceeds the nanometer particle size;
as can be seen from FIG. 2, the potential of the ZCsNPS-Cur-Que complex aggregate is almost constant with the increase of pH, and gradually decreases and approaches to zero after reaching the maximum value at pH 4.5;
as can be seen from FIG. 3, the prepared ZCsNPS-Cur-Que complex coacervate is round particles with more balanced sizes;
as shown in FIG. 4, the ZCsNPS-Cur-Que complex coacervate has higher embedding rate under the measured pH value, the embedding rate of the complex coacervate on curcumin is more than 90%, and the embedding rate on quercetin is slightly lower and is more than 80%.
Example 2
Referring to the preparation method in example 1, the pH of the fixed composite particle system is 4.0, the weight ratio between Cur and quee is 1:1, 2% Zein solution and the total amount of two polyphenols are mixed in the mass ratio of 20:1, 10:1, 5:1, that is, 0.01g (0.005g Cur and 0.005g quee), 0.02g (0.01g Cur and 0.01g quee), 0.04g (0.02g Cur and 0.02g quee) of two total polyphenols are added to three 10mL portions of 2% Zein solution stirred in a magnetic stirrer, and then Cs antisolvent solution is poured into dissolved Zein-Cur-quee solution stirred in a magnetic stirrer rapidly at a stirring rate of 600rpm, and the mixed solution is transferred to a retort bottle after stirring for 2 min. And (3) carrying out rotary heating for 12min at the speed of 88rpm and the temperature of 55 ℃, and completely evaporating ethanol to obtain 3 ZCsNPS-Cur-Que complex aggregates with different mixing mass ratios. The pH of the solution was adjusted to 4.0 by 1M HCl solution or 1M NaOH. The particle size and PDI were measured using a Zen-3690 Malvern particle size and potential analyzer.
The results are shown in FIG. 5: as can be seen from FIG. 5, the ZCsNPS-Cur-Que complex aggregates prepared at pH4.0 and having different mixing mass ratios (protein: total polyphenols) have the smallest particle size and smaller PDI at a mixing ratio of 20: 1.
Example 3
Referring to the preparation method in example 1, the pH of the fixed composite particle system was 5.0 and the weight ratio between Cur and Que was 1:1, 2% of Zein solution and the total amount of two pigments (Cur and Que) were mixed in the mass ratio of 20:1, 10:1, 5:1, that is, 0.01g (0.005g of Cur and 0.005g of Que), 0.02g (0.01g of Cur and 0.01g of Que), 0.04g (0.02g of Cur and 0.02g of Que), respectively, of two total polyphenols were added to 3 parts of 10mL of 2% Zein solution being stirred in a magnetic stirrer, followed by rapidly pouring Cs antisolvent solution into dissolved Zein-Cur-Que solution being stirred in a magnetic stirrer at a stirring rate of 600rpm, and after stirring for 2min, the mixed solution was transferred to a retort. And (3) carrying out rotary heating for 12min at the speed of 88rpm and the temperature of 55 ℃, and completely evaporating ethanol to obtain 3 ZCsNPS-Cur-Que complex aggregates with different mixing mass ratios. The pH was adjusted to 5.0 by 1M HCl solution or 1M NaOH solution. The particle size and PDI were measured using a Zen-3690 Malvern particle size and potential analyzer.
The results are shown in FIG. 6: as can be seen from FIG. 6, the particle size of the ZCsNPS-Cur-Que complex aggregates prepared at pH5.0 and having different mixing mass ratios (protein: total polyphenols) was the smallest at a mixing ratio of 20:1, and the PDI was about 0.2.
Example 4
Referring to the preparation method in example 1, the pH of the fixed composite particle system was 4.0, the total weight ratio of Zein to Cur and quee was 20:1, and 0.01g of two polyphenols (Cur and quee) were mixed in the ratio of 1: 1. weighing two polyphenols in different mixing mass ratios in an electronic balance according to the proportion of 1:2, 1:3, 1:4, 2:1, 3:1 and 4:1, respectively adding the two polyphenols into 10mL of 2% Zein solution which is stirred in a magnetic stirrer, then respectively and rapidly pouring the Cs antisolvent solution into the dissolved Zein-Cur-Que solution which is stirred in the magnetic stirrer at the stirring speed of 600rpm for 2min, and transferring the mixed solution to a rotary evaporation bottle. And (3) carrying out rotary heating for 12min at the speed of 88rpm and the temperature of 55 ℃, and completely evaporating ethanol to obtain 7 ZCsNPS-Cur-Que complex aggregates with different polyphenol mixing mass ratios. The pH was adjusted to 4.0 by 1M HCl solution or 1M NaOH solution. The particle size and PDI were measured using a Zen-3690 Malvern particle size and potential analyzer.
The results are shown in FIG. 7: as can be seen from FIG. 7, when the pH of the complex coacervate system was 4.0 and the total weight ratio of Zein to Cur and Que was 20:1, the particle size of the ZCsNPS-Cur-Que complex coacervate tended to increase regardless of whether the Cur or Que ratio was large, and when the mass ratio of the two polyphenols mixed was 1:1, the particle size was the smallest, the PDI was about 0.3, and when the mixing ratio was 1:3, the particle size was the largest, and the PDI value was also large.
Example 5
Referring to the preparation method in example 1, the pH of the composite particle system was fixed to 5.0, the total weight ratio of Zein to Cur to Que was 20:1, 0.01g of two polyphenols (Cur and Que) were weighed in an electronic balance at the ratio of 1:1, 1:2, 1:3, 1:4, 2:1, 3:1, and 4:1, respectively, the two polyphenols at different mixing mass ratios were added to 7 parts of 10mL of 2% Zein solution, respectively, which was stirred in a magnetic stirrer, and then the Cs antisolvent solution was rapidly poured into the dissolved Zein-Cur-Que solution, which was stirred in a magnetic stirrer at a stirring rate of 600rpm, and the mixed solution was transferred to a rotary retort after stirring for 2 min. And (3) carrying out rotary heating for 12min at the speed of 88rpm and the temperature of 55 ℃, and completely evaporating ethanol to obtain 7 ZCsNPS-Cur-Que complex aggregates with different polyphenol mixing mass ratios. The pH was adjusted to 5.0 by 1M HCl solution or 1M NaOH solution. The particle size and PDI were measured using a Zen-3690 Malvern particle size and potential analyzer.
The results are shown in FIG. 8: as can be seen from fig. 8, when the pH of the composite particle system was 5.0 and the total weight ratio of Zein to Cur and quee was 20:1, the particle size of the ZCsNPS-Cur-quee composite agglomerate tended to increase regardless of whether the total weight ratio of Cur was large or the total weight ratio of quee was large, and when the mass ratio of the two polyphenols was 1:1, the particle size was the smallest and the PDI was the smallest, and around 0.2, the particle size was the largest at a mixing ratio of 1:4, and the PDI value was close to 1.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a complex coacervate with double embedding functions is characterized by comprising the following steps:
(1) adding zein into an ethanol water solution, and stirring and dissolving to obtain a zein solution;
(2) adding chitosan into an acetic acid solution, stirring for dissolving, and then hydrating overnight to obtain a chitosan anti-solvent solution;
(3) adding curcumin and quercetin into the zein solution obtained in the step (1), uniformly stirring and mixing, and hydrating overnight to obtain a zein-curcumin-quercetin mixed solution;
(4) and (3) adding the chitosan anti-solvent solution obtained in the step (2) into the zein-curcumin-quercetin mixed solution obtained in the step (3), stirring and mixing uniformly, then rotating and heating to remove ethanol, and adjusting the pH value to 3.0-7.0 to obtain the composite coacervate with the double embedding function.
2. The method for producing a complex coacervate with double embedding function according to claim 1, wherein:
the mass ratio of the total mass of the curcumin and the quercetin to the zein in the step (3) is 1: 5-20;
the mass ratio of the curcumin to the quercetin in the step (3) is 1-4: 1-4.
3. The method for producing a complex coacervate with double embedding function according to claim 2, wherein:
the mass ratio of the total mass of the curcumin and the quercetin to the zein in the step (3) is 1: 20;
the mass ratio of the curcumin to the quercetin in the step (3) is 1: 1.
4. The method for producing a complex coacervate with double embedding function according to claim 1, wherein:
and (4) adjusting the pH value to 3.0-6.5.
5. The method for producing a complex coacervate with double embedding function according to claim 4, wherein:
and (4) adjusting the pH value to 4.0-5.0.
6. The method for producing a complex coacervate with double embedding function according to claim 1, wherein:
the ethanol water solution in the step (1) is 65-85% of ethanol water solution by volume percentage;
the concentration of the zein solution in the step (1) is 10-30 mg/mL;
the mass ratio of the chitosan to the zein in the step (2) is 0.4-0.8: 2;
the acetic acid solution in the step (2) is 0.8-1.2% by volume;
the chitosan in the step (2) has the molecular weight of 300kDa and the deacetylation degree of 95 percent;
the concentration of the chitosan anti-solvent solution in the step (2) is 0.8-1.2 mg/mL.
7. The method for producing a complex coacervate with double embedding function according to claim 6, wherein:
the ethanol water solution in the step (1) is 80% by volume of ethanol water solution;
the concentration of the zein solution in the step (1) is 20 mg/mL;
the mass ratio of the chitosan to the zein in the step (2) is 0.7: 2;
the acetic acid solution in the step (2) is 1% by volume of acetic acid solution;
the concentration of the chitosan anti-solvent solution in the step (2) is 1 mg/mL.
8. The method for producing a complex coacervate with double embedding function according to claim 1, wherein:
the temperature of the overnight hydration in the steps (2) and (3) is 0-6 ℃;
the rotating speed of stirring in the step (3) is 500-800 rpm;
the stirring conditions in the step (4) are as follows: stirring at 500-800 rpm for 1-3 min;
the rotary heating conditions in the step (4) are as follows: rotating and heating at 70-90 rpm and 50-65 ℃ for 8-15 min.
9. A complex coacervate with double embedding function, characterized in that: prepared by the method of any one of claims 1 to 8.
10. Use of the complex coacervate with double embedding function according to claim 9 in the field of food processing.
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| CN113527712B (en) * | 2021-06-17 | 2023-07-07 | 广州大学 | Corn peptide-microcrystalline chitin compound and preparation method of double pickering emulsion thereof |
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| CN114868916B (en) * | 2022-03-18 | 2023-07-25 | 江南大学 | Curcumin/ascorbic acid stabilized core-shell particles and preparation method thereof |
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