CN113940401A - Composition containing chitosan and preparation method and application thereof - Google Patents
Composition containing chitosan and preparation method and application thereof Download PDFInfo
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- CN113940401A CN113940401A CN202111141269.8A CN202111141269A CN113940401A CN 113940401 A CN113940401 A CN 113940401A CN 202111141269 A CN202111141269 A CN 202111141269A CN 113940401 A CN113940401 A CN 113940401A
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- chitosan
- black fungus
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- 229920001282 polysaccharide Polymers 0.000 claims abstract description 33
- 239000005017 polysaccharide Substances 0.000 claims abstract description 33
- 150000004676 glycans Chemical class 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 25
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 23
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 23
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- 238000004321 preservation Methods 0.000 claims abstract description 5
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- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- 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
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3562—Sugars; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B4/00—General methods for preserving meat, sausages, fish or fish products
- A23B4/10—Coating with a protective layer; Compositions or apparatus therefor
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B4/00—General methods for preserving meat, sausages, fish or fish products
- A23B4/14—Preserving with chemicals not covered by groups A23B4/02 or A23B4/12
- A23B4/18—Preserving with chemicals not covered by groups A23B4/02 or A23B4/12 in the form of liquids or solids
- A23B4/20—Organic compounds; Microorganisms; Enzymes
-
- 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
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
-
- 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 belongs to the technical field of food preservation, and discloses a chitosan-containing composition, and a preparation method and application thereof. The composition comprises chitosan and Auricularia auricula extract; the black fungus extract comprises black fungus polysaccharide and protein; the particle size of the composition is 50-500 nm. The invention uses chitosan and black fungus extract together, and utilizes the gel property of protein in the chitosan and black fungus extract to prepare the nano-scale composition. The synergistic interaction of the chitosan and the black fungus extract and the unique performance of the nano particles are fully utilized, so that the composition has an excellent antibacterial function. The chitosan-containing composition provided by the invention is natural and safe, and can be widely applied to the antisepsis and preservation of various foods.
Description
Technical Field
The invention belongs to the technical field of food preservation, and particularly relates to a chitosan-containing composition, and a preparation method and application thereof.
Background
With the improvement of living standard, health and environmental issues are receiving increasing attention. The consumer trend is also more and more towards healthy, natural products. In the food field, consumer demands for freshness of food and health safety of additives are increasing.
The chitosan is taken as cationic polysaccharide with second-order natural content than cellulose, has better biocompatibility, degradability, good film-forming property and broad-spectrum antibacterial property, can inhibit common food spoilage bacteria such as escherichia coli, staphylococcus aureus and the like to a certain extent, and has a better antibacterial effect on gram-positive bacteria than gram-negative bacteria. The chitosan can be used as an antistaling agent, a thickening agent, an antioxidant, a fruit juice clarifying agent, a decoloring agent, an antibacterial agent and the like in the field of foods, and has wide application. However, chitosan alone hardly exhibits excellent antibacterial activity in a complex food spoilage system.
In recent years, some research reports about chitosan edible coating films are reported at home and abroad, and the chitosan edible coating films are mainly used for fresh-keeping coating films of fruits, vegetables and fresh meat. The existing chitosan edible coating is mainly compounded with a chemical preservative for use, and although the coating has a good fresh-keeping effect, the acceptance of consumers is low. The natural active product has certain antibacterial activity and oxidation resistance, and has strong safety and high acceptance of consumers; but because of poor stability and solubility, most natural active products can not act together with chitosan, thereby realizing good bacteriostatic and fresh-keeping effects.
Therefore, it is highly desirable to provide a chitosan-containing composition which has good antibacterial activity and fresh-keeping effect, is natural and safe, and has high consumer acceptance.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the chitosan-containing composition provided by the invention has good antibacterial activity and fresh-keeping effect by using the chitosan and natural products in a matching way, and can effectively prolong the shelf life of food.
In a first aspect, the present invention provides a composition comprising chitosan.
Specifically, a chitosan-containing composition comprises chitosan and an auricularia auricula extract; the black fungus extract comprises black fungus polysaccharide and protein; the particle size of the composition is 50-500 nm.
The black fungus extract is not pure black fungus polysaccharide, but contains a certain content of black fungus polysaccharide and protein, wherein the protein can form gel with chitosan, and the key point for controlling the particle size of the composition to be 50-500 nm. The matching of the black fungus extract and the chitosan oligosaccharide can fully utilize the bacteriostatic performance of the black fungus extract and the chitosan oligosaccharide, and the nano-scale bacteriostatic composition is prepared through the gel effect of the black fungus extract and the chitosan, so that the bacteriostatic performance can be remarkably improved.
Preferably, in the black fungus extract, the content of black fungus polysaccharide is 40-95% and the content of protein is 2-30% by weight percentage; more preferably, the content of the auricularia auricula polysaccharide is 40-75%, and the content of the protein is 2-20%; more preferably, the content of the auricularia auricula polysaccharide is 50-70%, and the content of the protein is 10-20%.
Preferably, the particle size of the composition is 100-450 nm; further preferably, the particle size of the composition is 180-390 nm; more preferably, the particle size of the composition is 200-390 nm.
Preferably, the composition further comprises a cross-linking agent. The addition of the cross-linking agent is beneficial to the formation of the composition, and can enhance the bacteriostatic effect of the composition, especially the bacteriostatic effect on the later period of food.
Preferably, the cross-linking agent comprises at least one of soy protein isolate, sodium alginate or polyphosphate.
Preferably, in the composition, the mass ratio of the chitosan to the black fungus extract to the cross-linking agent is 1: (1-8): (0.01-1); further preferably, the mass ratio of the chitosan to the black fungus extract to the cross-linking agent is 1: (2-5): (0.01-0.3).
Preferably, the chitosan has a degree of deacetylation of 80 to 99%. The chitosan is food-grade crustacean extract, plant and fungus cell wall extract.
In a second aspect, the invention provides a method for preparing a chitosan-containing composition.
Specifically, the preparation method of the chitosan-containing composition comprises the following steps:
respectively dissolving the black fungus extract and other components in a solvent, and then mixing to prepare a suspension; the suspension is then dried to prepare the chitosan-containing composition.
Preferably, the solvent is acetic acid and/or water.
Preferably, the drying mode is spray drying.
Preferably, the preparation method of the black fungus extract comprises the following steps:
pulverizing Auricularia, sieving, and extracting with water and/or ethanol to obtain extractive solution; and drying the leaching liquor to obtain the black fungus extract.
Preferably, during the leaching, the pH is controlled to be 4-7.
Preferably, the drying mode is freeze drying.
In a third aspect, the invention provides the use of a chitosan-containing composition.
In particular to application of a composition containing chitosan in food preservation or fresh keeping. Such as preservatives and preservative films.
In a fourth aspect, the present invention provides a preservative film coating solution.
Specifically, the fresh-keeping coating solution comprises the chitosan-containing composition, a film forming agent, an acidity regulator and water.
Preferably, the fresh-keeping coating solution comprises the following components in percentage by weight: 0.5-5.0% of film-forming agent, 0.1-5% of acidity regulator, 0.1-1% of chitosan-containing composition and the balance of water. Further preferably, the fresh-keeping coating solution comprises the following components in percentage by weight: 0.5-5.0% of film-forming agent, 0.3-2% of acidity regulator, 0.1-0.5% of chitosan-containing composition and the balance of water.
Preferably, the acidity regulator comprises one or more of acetic acid, citric acid, fumaric acid, malic acid, a carbonate or a bicarbonate.
Preferably, the film forming agent is selected from at least one of chitosan, water-soluble starch, flaxseed gum, guar gum, pectin, or tween 80. Further preferably, the film forming agent is chitosan and guar gum.
The fifth aspect of the invention provides a method for using the preservative film coating solution.
Specifically, the application method of the preservative film coating solution comprises the following steps:
taking meat, attaching the fresh-keeping coating solution to the meat in a mixing, smearing, spraying or soaking mode, and storing the meat in an environment with the temperature lower than 10 ℃ after film forming.
The spraying includes ordinary spraying and pressurized spraying; the impregnation comprises direct soaking in the preservative coating solution and vacuum impregnation.
Preferably, the film forming process can adopt an air drying mode; the air drying time is 1-600 s.
Preferably, after the film is formed, the chilled fresh meat is stored at 4-6 ℃.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention uses chitosan and black fungus extract together, and utilizes the gel property of protein in the chitosan and black fungus extract to prepare the nano-scale composition. Fully utilizes the synergistic effect of chitosan and black fungus extract (protein and polysaccharide) and the unique performance of nano particles, so that the composition has excellent bacteriostatic function. Wherein, by controlling the particle size of the composition to be 50-500nm, high load capacity and stability, sustained release and the ability of carrying hydrophilic or lipophilic substances across cell membranes and biological barriers can be provided, which is beneficial for the preservative to play a better role when acting on food.
(2) The chitosan-containing composition provided by the invention is natural and safe, and can be widely applied to the antisepsis and preservation of various foods.
Drawings
FIG. 1 is a graph showing the sustained-release dynamics of chitosan-containing compositions prepared in examples 1 and 2;
fig. 2 is a graph showing the freshness retaining effect of application example 19.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
In comparative example 2, the auricularia auricula polysaccharide is purchased from Hibiscus bioscience, Inc. with a purity of 95% -99%, and is pretreated first if the purity is not enough. The remaining materials, reagents or equipment may be obtained from conventional commercial sources or may be obtained by known methods, unless otherwise specified.
Example 1
A chitosan-containing composition comprises chitosan and a black fungus extract, wherein the mass ratio of the black fungus extract to the chitosan is 1: 5; in the black fungus extract, the content of polysaccharide is 55.98g/100g, the content of protein is 15.10g/100g, and the content of polyphenol is 0.75g/100 g. The particle size of the composition is 347 nm.
A method for preparing a chitosan-containing composition, comprising the following steps:
(1) preparing a black fungus extract: pulverizing naturally air-dried Auricularia auricula with a pulverizer, and sieving with 100 mesh sieve to obtain Auricularia auricula powder; and then adding black fungus powder into hot water for leaching for 2.0h, wherein the mass ratio of the black fungus powder to the water is 1: 30, leaching, filtering out filter residue after leaching, repeating the leaching for 3 times according to the steps, and combining leaching filtrate; concentrating under reduced pressure at 60 deg.C to 1/10 of the total volume of the filtrate to obtain Auricularia auricula (L.) Underw extract concentrated solution; and drying the black fungus extract concentrated solution in a freeze dryer to obtain the black fungus extract. (the contents of protein, sugar and polyphenol are detected by adopting a phenol-sulfuric acid method, a Coomassie brilliant blue dyeing method and an ultraviolet absorption method respectively, and the polysaccharide content, the protein content and the polyphenol content in the black fungus extract are respectively 55.98g/100g, 15.10g/100g and 0.75g/100 g).
(2) 5g of chitosan is dissolved in 100 ml of acetic acid solution (pH 5.5) to prepare chitosan solution, and 25 g of black fungus extract is dissolved in 500 ml of water to prepare black fungus extract solution. The black fungus extract solution was added dropwise to the chitosan solution using a syringe, and a turbid suspension was formed under vigorous magnetic stirring.
(3) And (3) performing spray drying on the suspension to obtain a chitosan-containing composition CS-AAE-NP 1.
Example 2
A composition containing chitosan comprises chitosan, black fungus extract and sodium tripolyphosphate, wherein the mass ratio of the black fungus extract to the chitosan to the sodium tripolyphosphate is 1: 2: 0.15; in the black fungus extract, the content of polysaccharide is 55.98g/100g, the content of protein is 15.10g/100g, and the content of polyphenol is 0.75g/100 g. The particle size of the composition was 261 nm.
A method for preparing a chitosan-containing composition, comprising the following steps:
(1) the procedure for preparing the black fungus extract was the same as in example 1.
(2) 5g of chitosan is dissolved in 100 ml of acetic acid solution (pH 5.5) to prepare chitosan solution, 10g of black fungus extract is dissolved in 500 ml of water to prepare black fungus extract solution, and 0.75g of sodium tripolyphosphate is dissolved in 500 ml of water to prepare sodium tripolyphosphate solution. The chitosan solution and the sodium tripolyphosphate solution were mixed using a syringe, and then the black fungus extract solution was added dropwise thereto, followed by vigorous magnetic stirring to form a turbid suspension.
(3) And (3) performing spray drying on the suspension to obtain a chitosan-containing composition CS-AAE-NP 2.
Example 3
Example 3 differs from example 2 in that: the cross-linking agent is sodium alginate.
Specifically, the chitosan-containing composition comprises chitosan, a black fungus extract and sodium alginate, wherein the mass ratio of the black fungus extract to the chitosan to the sodium alginate is 1: 2: 0.15; in the black fungus extract, the content of polysaccharide is 55.98g/100g, the content of protein is 15.10g/100g, and the content of polyphenol is 0.75g/100 g. The particle size of the composition is 421 nm.
A method for preparing a chitosan-containing composition, comprising the following steps:
(1) the procedure for preparing the black fungus extract was the same as in example 1.
(2) Dissolving 5g of chitosan in 100 ml of acetic acid solution (pH 5.5) to prepare chitosan solution, dissolving 10g of black fungus extract in 500 ml of water to prepare black fungus extract solution, and dissolving 0.75g of sodium alginate in 500 ml of water to prepare sodium alginate solution. The chitosan solution and the sodium alginate solution were mixed using a syringe, and then the black fungus extract solution was added dropwise thereto, followed by vigorous magnetic stirring to form a turbid suspension.
(3) And (3) performing spray drying on the suspension to obtain a chitosan-containing composition CS-AAE-NP 3.
Example 4
Example 4 differs from example 2 in that: the cross-linking agent is soybean protein isolate.
Specifically, the chitosan-containing composition comprises chitosan, a black fungus extract and soybean protein isolate, wherein the mass ratio of the black fungus extract to the chitosan to the soybean protein isolate is 1: 2: 0.15; in the black fungus extract, the content of polysaccharide is 55.98g/100g, the content of protein is 15.10g/100g, and the content of polyphenol is 0.75g/100 g. The particle size of the composition was 311 nm.
A method for preparing a chitosan-containing composition, comprising the following steps:
(1) the procedure for preparing the black fungus extract was the same as in example 1.
(2) Dissolving 5g of chitosan in 100 ml of acetic acid solution (pH 5.5) to obtain a chitosan solution, dissolving 10g of black fungus extract in 500 ml of water to obtain a black fungus extract solution, and dissolving 0.75g of soybean protein isolate in 500 ml of water to obtain a soybean protein isolate solution. The chitosan solution and the soy protein isolate solution were mixed using a syringe, and then the black fungus extract solution was added dropwise thereto, followed by vigorous magnetic stirring to form a turbid suspension.
(3) And (3) performing spray drying on the suspension to obtain a chitosan-containing composition CS-AAE-NP 4.
Example 5
A composition containing chitosan comprises chitosan, black fungus extract and sodium tripolyphosphate, wherein the mass ratio of the black fungus extract to the chitosan to the sodium tripolyphosphate is 1: 8: 0.05; in the black fungus extract, the content of polysaccharide is 55.98g/100g, the content of protein is 15.10g/100g, and the content of polyphenol is 0.75g/100 g. The particle size of the composition is 273 nm.
A method for preparing a chitosan-containing composition, comprising the following steps:
(1) the procedure for preparing the black fungus extract was the same as in example 1.
(2) 5g of chitosan is dissolved in 100 ml of acetic acid solution (pH 5.5) to prepare chitosan solution, 40 g of black fungus extract is dissolved in 500 ml of water to prepare black fungus extract solution, and 0.25 g of sodium tripolyphosphate is dissolved in 500 ml of water to prepare sodium tripolyphosphate solution. The chitosan solution and the sodium tripolyphosphate solution were mixed using a syringe, and then the black fungus extract solution was added dropwise thereto, followed by vigorous magnetic stirring to form a turbid suspension.
(3) And (3) performing spray drying on the suspension to obtain a chitosan-containing composition CS-AAE-NP 5.
Example 6
A composition containing chitosan comprises chitosan, black fungus extract and sodium tripolyphosphate, wherein the mass ratio of the black fungus extract to the chitosan to the sodium tripolyphosphate is 1: 2: 0.1; in the black fungus extract, the content of polysaccharide is 55.98g/100g, the content of protein is 15.10g/100g, and the content of polyphenol is 0.75g/100 g. The particle size of the composition is 258 nm.
A method for preparing a chitosan-containing composition, comprising the following steps:
(1) the procedure for preparing the black fungus extract was the same as in example 1.
(2) 5g of chitosan is dissolved in 100 ml of acetic acid solution (pH 5.5) to prepare chitosan solution, 10g of black fungus extract is dissolved in 500 ml of water to prepare black fungus extract solution, and 0.5 g of sodium tripolyphosphate is dissolved in 500 ml of water to prepare sodium tripolyphosphate solution. The chitosan solution and the sodium tripolyphosphate solution were mixed using a syringe, and then the black fungus extract solution was added dropwise thereto, followed by vigorous magnetic stirring to form a turbid suspension.
(3) And (3) performing spray drying on the suspension to obtain a chitosan-containing composition CS-AAE-NP 6.
Example 7
A chitosan-containing composition comprises chitosan and a black fungus extract, wherein the mass ratio of the black fungus extract to the chitosan is 1: 2; in the black fungus extract, the content of polysaccharide is 55.98g/100g, the content of protein is 15.10g/100g, and the content of polyphenol is 0.75g/100 g. The particle size of the composition is 295 nm.
A method for preparing a chitosan-containing composition, comprising the following steps:
(1) the procedure for preparing the black fungus extract was the same as in example 1.
(2) 5g of chitosan is dissolved in 100 ml of acetic acid solution (pH 5.5) to prepare chitosan solution, and 10g of black fungus extract is dissolved in 500 ml of water to prepare black fungus extract solution. The black fungus extract solution was added dropwise to the chitosan solution using a syringe, and a turbid suspension was formed under vigorous magnetic stirring.
(3) And (3) performing spray drying on the suspension to obtain a chitosan-containing composition CS-AAE-NP 7.
Comparative example 1
A mixture containing nano chitosan comprises chitosan, black fungus extract and sodium tripolyphosphate, wherein the mass ratio of the black fungus extract to the chitosan to the sodium tripolyphosphate is 1: 2: 0.15; in the black fungus extract, the content of polysaccharide is 55.98g/100g, the content of protein is 15.10g/100g, and the content of polyphenol is 0.75g/100 g. The particle size of the composition was 210 nm.
A method for preparing a mixture containing nano chitosan comprises the following steps:
(1) the procedure for preparing the black fungus extract was the same as in example 1.
(2) 5g of chitosan was dissolved in 100 ml of acetic acid solution (pH 5.5) and 0.75g of sodium tripolyphosphate was dissolved in 500 ml of water. After a turbid suspension was formed by dropping a sodium tripolyphosphate solution into the chitosan solution using a syringe under vigorous magnetic stirring, 2.5g of black fungus extract (without water dissolution) was directly added.
(3) And (3) preparing the mixture CS-NP-AAE containing the nano chitosan by a spray drying method.
Comparative example 2
The difference between the comparative example 2 and the example 2 is that the black fungus extract is replaced by the same amount of black fungus polysaccharide (the purity is 95-99%).
Specifically, the composition containing chitosan comprises chitosan, auricularia auricula polysaccharide and sodium tripolyphosphate, wherein the mass ratio of the auricularia auricula polysaccharide to the chitosan to the sodium tripolyphosphate is 1: 2: 0.15. the particle size of the composition is 660 nm.
A method for preparing a chitosan-containing composition, comprising the following steps:
(2) 5g of chitosan was dissolved in 100 ml of acetic acid solution (pH 5.5), 10g of auricularia auricula-polysaccharide was dissolved in 500 ml of water, and 0.75g of sodium tripolyphosphate was dissolved in 500 ml of water. The three solutions were mixed using a syringe and, under vigorous magnetic stirring, a cloudy suspension was formed.
(3) And (3) performing spray drying on the suspension to obtain a chitosan-containing composition which is marked as the auricularia auricula polysaccharide composition.
The chitosan-containing compositions prepared in examples 1 to 5 and comparative examples 1 to 2 were tested for bacteriostatic effects.
(1) The obtained chitosan-containing composition was characterized in terms of particle size (D) and polydispersity index (DPI) of the chitosan-containing composition using a nano-particle size potential analyzer, wherein DPI represents uniformity of particle size distribution of nanoparticles, and the smaller DPI, the more concentrated the nanoparticle distribution, the results are shown in table 1.
TABLE 1
D(nm) | DPI | |
CS-AAE-NP1 | 347 | 0.171 |
CS-AAE-NP2 | 261 | 0.162 |
CS-AAE-NP3 | 421 | 0.167 |
CS-AAE-NP4 | 311 | 0.161 |
CS-AAE-NP5 | 273 | 0.181 |
CS-NP-AAE | 210 | 0.151 |
Auricularia auricula polysaccharide composition | 660 | 0.183 |
As can be seen from Table 1, the smaller the crosslinking agent, the smaller the particle size of the nanoparticles formed after the crosslinking agent reacts with chitosan, wherein the nanoparticle CS-AAE-NP2 formed by adding the crosslinking agent sodium tripolyphosphate has the smaller particle size; meanwhile, the electronegativity of the cross-linking agent also influences the formation of the nano-particles, and the stronger the electronegativity of the cross-linking agent, the easier the cross-linking with the chitosan is. Wherein carboxyl in the sodium alginate in the embodiment 3 has stronger electronegativity, and the formed CS-AAE-NP3 nano-particle size is larger. The polydispersity of the nanoparticles is influenced by factors such as the molecular weight distribution of chitosan, the properties of the cross-linking agent, the proportion of the cross-linking agent to the chitosan and the like, and the table shows that the addition of the cross-linking agent is favorable for forming the nanoparticles with uniform particle size; example 5 the CS-AAE-NP5 nanoparticles DPI formed by the black fungus extract is larger due to the reduced proportion of the black fungus extract, namely the particle size distribution of the formed nanoparticles is wider. In the auricularia auricula polysaccharide composition prepared in the comparative example 2, auricularia auricula polysaccharide is adopted to replace an auricularia auricula extract, so that the composition with the particle size of 50-500nm cannot be prepared.
(2) To characterize the antimicrobial performance of chitosan-containing compositions, the Minimum Inhibitory Concentration (MIC) of each composition was tested against several common spoilage bacteria, respectively. The putrefying bacteria comprise gram-positive bacteria such as staphylococcus aureus, mesophilic normal temperature bacteria bacillus cereus, bacillus subtilis and acidophilic bacteria lactobacillus plantarum; gram-negative bacteria represent Pseudomonas aeruginosa and Escherichia coli. The results are shown in Table 2.
TABLE 2
Note: "-" indicates that the bacteria were not inhibited beyond a concentration of 4000 ppm.
The chitosan has good antibacterial performance on staphylococcus aureus; the black fungus extract has certain antibacterial performance on staphylococcus aureus, mesophilic normal temperature bacteria bacillus cereus, bacillus subtilis, acidophilic bacteria lactobacillus plantarum, pseudomonas aeruginosa and escherichia coli. After the chitosan and the black fungus extract are prepared into the nano composition, the antibacterial performance is further enhanced, and the minimum antibacterial concentration of the nano composition is obviously superior to that of the chitosan and the black fungus extract and is also superior to that of the comparative example 1 and the comparative example 2.
(3) Testing the kinetics of active substance Release
The chitosan-containing compositions prepared in examples 1-2 were tested for active substance release kinetics and the results are shown in fig. 1. In FIG. 1, the abscissa is Time (Time/day) and the ordinate is Cumulative release percentage (Cumulative release%), it can be seen from FIG. 1 that the sustained release rate of CS-AAE-NP2 is lower than that of CS-AAE-NP1, which indicates that as the protein in CS-AAE-NP2 gradually separates from the chitosan, the polysaccharide component in the nano-composition is released and the active ingredient consumed in the system can be continuously supplemented, therefore, the composition has more continuous antibacterial effect after adding the cross-linking agent polyphosphate.
Application examples 1 to 5
CS-AEE-NP1, CS-AEE-NP2, CS-AEE-NP3, CS-AEE-NP4, and CS-AEE-NP5 (corresponding to application examples 1 to 5), chitosan, sodium chitosan-tripolyphosphate, and the compositions prepared in comparative examples 1 and 2 were used for the preservation of beef marinated, respectively. The specific operation is as follows:
weighing 9 parts of beef tendon meat with the same amount, respectively adding halogen material and chitosan-containing composition with the same amount, wherein the addition amount of the chitosan-containing composition is 3000ppm (based on the weight of the brine), stirring uniformly, and marinating. The blank was not added with any composition.
The total number of colonies of the spiced beef is detected according to the method of GB 4789.2-2016 national standard for food safety-food microbiology test-total number of colonies detection, and the test results are shown in Table 3.
TABLE 3 fresh keeping Effect of the compositions in spiced beef
Application examples 6 to 10
The compositions prepared in examples 1-5, CS-AEE-NP1, CS-AEE-NP2, CS-AEE-NP3, CS-AEE-NP4, and CS-AEE-NP5 (corresponding to application examples 6-10), chitosan, sodium chitosan-tripolyphosphate, comparative example 1, and comparative example 2 were used as preservatives, respectively, in a fresh-keeping halogen in pork meatballs. The specific operation is as follows:
weighing 9 parts of pork ball mixed material with the same amount, respectively adding chitosan-containing compositions CS-AEE-NP1, CS-AEE-NP2, CS-AEE-NP3, CS-AEE-NP4 and CS-AEE-NP5, wherein the addition amount of the chitosan-containing composition is 5000ppm (based on the total weight of the mixed pork balls), uniformly stirring, chopping, molding, cooking and heat sealing. The blank was not added with any composition.
The total number of colonies of the meat products in application examples 1-5 were detected according to the method of GB 4789.2-2016 national standard for food safety-food microbiology test-total number of colonies determination, and the test results are shown in Table 4.
TABLE 4 fresh keeping Effect of nanoparticles in pork balls
Application examples 11 to 18, comparative application examples 1 to 2
CS-AEE-NP6 and CS-AEE-NP7 prepared in examples 6 and 7 were used to prepare a fresh coating solution having the composition shown in Table 5 (corresponding to application examples 11 to 18), respectively, and the fresh coating solution was applied to the fresh keeping of fresh chicken breast meat.
The CS-NP-AAE and auricularia auricula polysaccharide compositions prepared in comparative examples 1 and 2 are respectively used for preparing preservative film coating solutions, the components of which are shown in Table 1 (corresponding to application examples 1-2), and the preservative film coating solutions are applied to the preservation of fresh chicken breast meat.
The application process is as follows: (1) firstly, dissolving chitosan in acetic acid, then adding the compositions into the chitosan solution, and stirring until the compositions are uniformly dispersed to prepare the preservative coating solution. (2) Placing the cut fresh chicken breast meat in each fresh-keeping coating solution, soaking for several seconds, then sequentially air-drying for no more than 10min, placing the air-dried meat blocks in a culture dish, and finally placing the culture dish containing the meat blocks in an environment of 6 ℃ for refrigeration. The microbial status was measured at days 0, 4, and 7, and the test results are shown in Table 6.
TABLE 5
TABLE 6
D0(log cfu/g) | D4(log cfu/g) | D7(log cfu/g) | |
Comparative application example 1 | 4.18 | 5.14 | 7.35 |
Comparative application example 2 | 3.94 | 5.21 | 6.90 |
Application example 11 | 3.87 | 4.47 | 4.56 |
Application example 12 | 3.62 | 4.40 | 4.33 |
Application example 13 | 3.94 | 5.08 | 6.32 |
Application example 14 | 3.60 | 4.53 | 4.77 |
Application example 15 | 3.59 | 4.54 | 4.69 |
Application example 16 | 3.88 | 5.00 | 6.13 |
Application example 17 | 3.24 | 3.90 | 4.09 |
Application example 18 | 3.38 | 3.95 | 4.07 |
Application examples 19 to 21, comparative application examples 3 to 4
CS-AEE-NP2, CS-AEE-NP3, and CS-AEE-NP4 prepared in examples 2, 3, and 4 were used to prepare a fresh coating solution (corresponding to application examples 19 to 21 in this order) containing 12000ppm of chitosan, 10000ppm of acetic acid, 5000ppm of CS-AEE-NP6, and the balance of drinking water.
The CS-NP-AAE and auricularia auricula polysaccharide compositions prepared in comparative examples 1 and 2 were used to prepare preservative coating solutions (corresponding to comparative application examples 3 to 4).
(1) Respectively placing fresh-cut fish blocks, fresh-cut pork blocks, fresh-cut beef blocks and fresh oyster mushrooms in the fresh-keeping coating solution prepared in application example 19, soaking for several seconds, then sequentially air-drying for no more than 10min, placing the air-dried meat blocks in a culture dish, and finally placing the culture dish containing the meat blocks in an environment at 6 ℃ for refrigeration. The microbial status was measured at days 0, 4, and 7, and the test results are shown in table 7 and fig. 2. In FIG. 2, the ordinate represents the number of pairs of the total number of colonies (log cfu/g), and the abscissa represents time.
TABLE 7
(2) Placing the fresh-cut beef blocks into the fresh-keeping coating solution prepared in the application examples 18-20 and the comparative application examples 3-4, soaking for a plurality of seconds, then sequentially air-drying for no more than 10min, placing the air-dried beef blocks into a culture dish, and finally placing the culture dish containing the beef blocks in an environment at 6 ℃ for refrigeration. The microbial status was measured at days 0, 4, and 7, and the test results are shown in Table 8.
TABLE 8
D0(log cfu/g) | D4(log cfu/g) | D7(log cfu/g) | |
Blank group | 4.70 | 5.83 | 7.68 |
Application example 19 | 3.69 | 3.93 | 3.58 |
Application example 20 | 3.72 | 3.99 | 3.72 |
Application example 21 | 3.68 | 3.94 | 3.75 |
Comparative application example 3 | 3.85 | 4.23 | 4.75 |
Comparative application example 4 | 3.81 | 4.05 | 4.35 |
In table 8, it can be seen from comparison of application examples 19 to 21 that when the crosslinking agent is substituted with sodium tripolyphosphate instead of soy protein isolate and sodium alginate, the prepared fresh coating solution has a similar bacteriostatic effect at the early stage, but the composition using sodium tripolyphosphate as the crosslinking agent exhibits a more excellent bacteriostatic effect at the later stage.
Claims (13)
1. A composition containing chitosan is characterized by comprising chitosan and black fungus extract; the black fungus extract comprises black fungus polysaccharide and protein; the particle size of the composition is 50-500 nm.
2. The composition as claimed in claim 1, wherein the black fungus extract contains, in percentage by weight, 40-95% of black fungus polysaccharides and 2-30% of proteins.
3. The composition of claim 2, wherein the auricularia auricula polysaccharide is 40-75% and the protein is 2-20%.
4. The composition as claimed in claim 1, wherein the particle size of the composition is 100-450 nm.
5. The composition of claim 1, further comprising a cross-linking agent comprising at least one of soy protein isolate, sodium alginate, or polyphosphate.
6. The composition as claimed in claim 5, wherein the mass ratio of the chitosan to the black fungus extract and the cross-linking agent in the composition is 1: (1-8): (0.01-1).
7. A method for preparing a chitosan-containing composition according to any one of claims 1 to 6,
respectively dissolving the black fungus extract and other components in a solvent, and then mixing to prepare a suspension; the suspension is then dried to prepare the chitosan-containing composition.
8. The preparation method of claim 7, wherein the black fungus extract comprises the following steps: crushing black fungus, sieving, and adding water and/or ethanol for leaching to obtain leaching liquor; and drying the leaching liquor to obtain the black fungus extract.
9. The method of claim 8, wherein during the leaching, the pH is controlled to be 4-7.
10. Use of a chitosan-containing composition of any one of claims 1-6 for the preservation or freshness of food.
11. A fresh-keeping coating solution comprising the chitosan-containing composition of any one of claims 1 to 6, a film-forming agent, an acidity regulator and water.
12. The anti-staling coating solution as defined in claim 11 consisting of, in weight percent: 0.5-5.0% of film-forming agent, 0.1-5% of acidity regulator, 0.1-1% of chitosan-containing composition and the balance of water.
13. The method of using the fresh-keeping coating solution of claim 11 or 12, comprising the steps of:
taking meat, attaching the fresh-keeping coating solution to the meat in a mixing, smearing, spraying or soaking mode, and storing the meat in an environment with the temperature lower than 10 ℃ after film forming.
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CN1508175A (en) * | 2002-12-13 | 2004-06-30 | 上海爱普食品工业有限公司 | Method for preparing composite comestible shell polysaccharide membrane |
CN110876409A (en) * | 2019-11-26 | 2020-03-13 | 黑龙江惊哲森林食品集团有限公司 | Vegetable lactobacillus fermentation liquor for preserving pork and preparation method thereof |
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