CN110999954B - Edible fresh-keeping film spraying agent and preparation method thereof - Google Patents
Edible fresh-keeping film spraying agent and preparation method thereof Download PDFInfo
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- CN110999954B CN110999954B CN201911264154.0A CN201911264154A CN110999954B CN 110999954 B CN110999954 B CN 110999954B CN 201911264154 A CN201911264154 A CN 201911264154A CN 110999954 B CN110999954 B CN 110999954B
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- film
- stirring
- spraying agent
- carboxymethyl chitosan
- litchi
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- 238000005507 spraying Methods 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 71
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229920001661 Chitosan Polymers 0.000 claims abstract description 59
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims abstract description 49
- 238000003756 stirring Methods 0.000 claims abstract description 38
- 108010073771 Soybean Proteins Proteins 0.000 claims abstract description 35
- 235000019710 soybean protein Nutrition 0.000 claims abstract description 30
- 244000183278 Nephelium litchi Species 0.000 claims abstract description 27
- 239000003755 preservative agent Substances 0.000 claims abstract description 24
- 230000002335 preservative effect Effects 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000341 volatile oil Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
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- 239000012153 distilled water Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
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- 239000003623 enhancer Substances 0.000 claims abstract description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 6
- 229940001941 soy protein Drugs 0.000 claims abstract description 5
- 235000013305 food Nutrition 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 7
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims description 7
- 239000000284 extract Substances 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
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- 238000002390 rotary evaporation Methods 0.000 claims description 3
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- 238000000034 method Methods 0.000 abstract description 7
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 8
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- 229910052739 hydrogen Inorganic materials 0.000 description 6
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- 229920002472 Starch Polymers 0.000 description 2
- 235000003095 Vaccinium corymbosum Nutrition 0.000 description 2
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- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- YYGNTYWPHWGJRM-UHFFFAOYSA-N (6E,10E,14E,18E)-2,6,10,15,19,23-hexamethyltetracosa-2,6,10,14,18,22-hexaene Chemical compound CC(C)=CCCC(C)=CCCC(C)=CCCC=C(C)CCC=C(C)CCC=C(C)C YYGNTYWPHWGJRM-UHFFFAOYSA-N 0.000 description 1
- 108010082495 Dietary Plant Proteins Proteins 0.000 description 1
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- 229920000426 Microplastic Polymers 0.000 description 1
- BHEOSNUKNHRBNM-UHFFFAOYSA-N Tetramethylsqualene Natural products CC(=C)C(C)CCC(=C)C(C)CCC(C)=CCCC=C(C)CCC(C)C(=C)CCC(C)C(C)=C BHEOSNUKNHRBNM-UHFFFAOYSA-N 0.000 description 1
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- PRAKJMSDJKAYCZ-UHFFFAOYSA-N dodecahydrosqualene Natural products CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 description 1
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
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- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000008863 intramolecular interaction Effects 0.000 description 1
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- 239000010410 layer Substances 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
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- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229940071440 soy protein isolate Drugs 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229940031439 squalene Drugs 0.000 description 1
- TUHBEKDERLKLEC-UHFFFAOYSA-N squalene Natural products CC(=CCCC(=CCCC(=CCCC=C(/C)CCC=C(/C)CC=C(C)C)C)C)C TUHBEKDERLKLEC-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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Images
Classifications
-
- 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
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/16—Coating with a protective layer; Compositions or apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Zoology (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
- Storage Of Fruits Or Vegetables (AREA)
Abstract
The invention provides an edible preservative film spraying agent and a preparation method thereof, belonging to the technical field of preservative films. The film spraying agent comprises the following raw materials in percentage by mass: 1.8-2.5% of carboxymethyl chitosan, 1.1-1.5% of soybean protein isolate, 1.2-1.7% of polyvinylpyrrolidone-K, 0.15-0.22% of glycerol, 20-25% of absolute ethyl alcohol, 3-6% of litchi essential oil and the balance of distilled water. When the film spraying agent is prepared, firstly adding carboxymethyl chitosan into distilled water, and stirring until the carboxymethyl chitosan is completely dissolved; then adding the isolated soy protein, stirring and then carrying out ultrasonic treatment; continuously adding polyvinylpyrrolidone as a film forming enhancer, stirring, then adding glycerol as a plasticizer, and stirring; adding litchi essential oil and stirring; slowly adding absolute ethyl alcohol, stirring, and ultrasonically removing bubbles in the solution; and finally filtering to obtain the uniform edible fresh-keeping film spraying agent. The preparation method has the advantages of simple process, convenient carrying, convenient operation and use, stable quality and quick film forming time.
Description
Technical Field
The invention relates to the technical field of preservative films, in particular to an edible preservative film spraying agent and a preparation method thereof.
Background
As China walks into the well-being society, the requirements of people on the quality of life are higher and higher, people hope to adopt a safe and green antiseptic fresh-keeping method to ensure the safety of fruits while pursuing delicious fruits, but the fresh-keeping film sold on the market at present is synthesized by a chemical method, the micro plastic particle transfer in the film causes certain harm to the food safety, and the plastic has the defect of difficult degradation and is easy to cause white pollution, thus being an environment-unfriendly material. As a new material with biodegradability, the edible preservative film can effectively reduce white pollution and has good protection effect on environment and ecology, so that the edible preservative film gradually becomes a research hotspot.
The edible film is generally a film having a porous network structure formed by interaction or crosslinking of one or more substances selected from edible substances such as proteins, lipids, polysaccharides, and starch, and has biodegradability and renewability.
The carboxymethyl chitosan is prepared by carboxymethylation of chitosan, not only solves the defect that the chitosan is insoluble in water, but also inherits the excellent characteristics of degradability, film forming property, air resistance, antibiosis and the like of the chitosan. Carboxymethyl chitosan is cross-linked into a net structure by its hydrogen bonds, and can be made into a transparent film with a porous structure by using a proper solvent, wherein the film has semi-permeability and is O-resistant 2 、CO 2 Has certain selective permeation function and certain water retention. On the one hand, external air is prevented from entering the membrane layer, so that the respiration of the fruit and vegetable raw materials is inhibited, on the other hand, carbon dioxide generated by respiration is allowed to escape, and anaerobic fermentation is prevented. Meanwhile, the film forming property and the antibacterial activity of the carboxymethyl chitosan also prevent pathogenic bacteria from directly contacting parasitic tissues and cells, and the effective invasion of the pathogenic bacteria is reduced, so that the aim of keeping fresh is fulfilled.
As a vegetable protein with excellent quality, low price and rich resources, the isolated soy protein has natural film-forming property. The soybean protein isolate is used as natural macromolecule, and is rich in hydroxyl (-OH), carboxyl (-COOH) and amino (-NH) 2 ) The active groups have a large amount of hydrophobic bonds, ionic bonds and hydrogen bonds, so that the emulsion has various functional properties such as emulsifying property, water-retaining property, gelling property, solubility, film-forming property and the like. When the sulfur radical in protein is denatured, disulfide bond is formed to combine and strengthen the interaction between molecules, so as to form water insoluble stereo net structure and obtain film with certain strength and blocking performance.
Disclosure of Invention
The invention aims to solve the problem that the existing chemical synthesis preservative film transfers micro-plastics of food, if people eat the food preserved by the film for a long time, the micro-plastics are easy to accumulate in the body and harm health, and the film is difficult to biodegrade and is easy to cause environmental problems such as white pollution and the like. Therefore, the invention provides an edible fresh-keeping film spraying agent and a preparation method thereof, which meet the requirements of people.
The fresh-keeping film spraying agent comprises the following raw materials in percentage by mass: 1.8-2.5% of carboxymethyl chitosan, 1.1-1.5% of soybean protein isolate, 1.2-1.7% of polyvinylpyrrolidone-K, 0.15-0.22% of glycerol, 20-25% of absolute ethyl alcohol, 3-6% of litchi essential oil and the balance of distilled water.
Further, the preferable content mass percentage of each component is as follows: 2% of carboxymethyl chitosan, 1.3% of soybean protein isolate, 1.5% of polyvinylpyrrolidone-K, 0.2% of glycerol, 23.7% of absolute ethyl alcohol, 4% of litchi essential oil and the balance of distilled water.
Wherein, the deacetylation degree of the carboxymethyl chitosan is 90-95 percent, and the carboxylation degree is more than or equal to 80 percent; the soybean protein isolate is in food grade; the average molecular weight of polyvinylpyrrolidone-K30 is 58000, and the polyvinylpyrrolidone is food grade; the average molecular weight of glycerol is 95, and the glycerol is food grade; the absolute ethyl alcohol content is more than or equal to 99.5 percent, and the food grade is realized.
The extraction method of the litchi essential oil comprises the following steps: cleaning and airing litchi shells or litchi seeds, crushing and sieving with a 80-mesh sieve, weighing powder in a round-bottom flask, adding petroleum ether according to a certain material-liquid ratio, carrying out ultrasonic treatment at a certain temperature, carrying out vacuum filtration on an extract liquid after ultrasonic treatment, and carrying out rotary evaporation on the extract liquid to obtain the litchi essential oil.
Wherein, the ratio of the materials to the liquid is 1:4-1:10,g/mL; the boiling range of the petroleum ether is 60-90 ℃.
The ultrasonic temperature is 45-50 ℃, the ultrasonic power is 300W, and the ultrasonic time is 60 minutes.
The preparation method of the edible fresh-keeping film spraying agent comprises the following specific steps:
(1) Adding carboxymethyl chitosan into distilled water, and stirring until the carboxymethyl chitosan is completely dissolved;
(2) Adding the isolated soy protein into the solution obtained in the step (1), and quickly stirring at 300r/min for 30min; then carrying out ultrasonic treatment for 20min under the power of 350-450W;
(3) Adding polyvinylpyrrolidone-K30 serving as a film-forming enhancer into the solution treated in the step (2), and stirring at 300r/min for 20min;
(4) Continuously adding glycerol as plasticizer, and stirring at 300r/min for 20min;
(5) Adding litchi essential oil, and stirring at 200r/min for 20min;
(6) Slowly adding absolute ethyl alcohol into the solution obtained in the step (5), and stirring at 200r/min for 30min;
(7) Performing ultrasonic treatment on the solution obtained in the step (6) for 20min at the power of 100W to remove bubbles in the solution;
(8) Filtering to remove solid residues in the solution to obtain the uniform edible fresh-keeping film spraying agent.
The technical scheme of the invention has the following beneficial effects:
(1) The edible preservation film-spraying agent disclosed by the invention adopts carboxymethyl chitosan with good water solubility and soybean protein isolate with high nutritional ingredients as main materials, and the prepared film-spraying agent has the characteristics of naturalness, no toxicity, greenness, good preservation effect, edibility, convenience in carrying, good film-forming property, rapid film-forming property and the like, can improve the quality and shelf life of food, can be biodegraded into oligomers under a certain condition, does not have the problem of environmental pollution, and is environment-friendly and green.
(2) According to the invention, the litchi essential oil is extracted by using an ultrasonic-assisted simultaneous distillation extraction method, and the extracted litchi essential oil rich in squalene is added into an edible fresh-keeping film spraying agent, so that the oxidation resistance and the antibacterial performance of the litchi essential oil are improved.
(3) The invention utilizes ultrasonic technology to process the mixed liquid of carboxymethyl chitosan and soybean protein isolate. The ultrasonic wave is utilized to generate cavitation, mechanical action and super-mixing effect, so that some hydrogen bonds in protein molecules in the soybean protein isolate are broken, the compact rigid structure of the soybean protein isolate is changed, the exposure of internal hydrophobic groups is increased, the action sites of the soybean protein isolate and the carboxymethyl chitosan are increased, more intermolecular and intramolecular hydrogen bonds are formed, the compact network structure is further formed, and the tensile strength of the membrane is increased.
(4) The preparation method and the conditions and the process are simple and easy to operate.
(5) The prepared edible fresh-keeping film spraying agent has good viscosity, smooth and compact film spraying surface and good gas barrier property. On the basis of the mixed solution of carboxymethyl chitosan and soybean protein isolate, polyvinylpyrrolidone-K30 is added to strengthen the intramolecular bonding effect of the edible fresh-keeping film spraying agent, so that a more compact reticular structure is formed, the smoothness and stability of the film are facilitated, and the mechanical property and the moisture resistance of the film are further facilitated to be improved; the glycerol is added, and the micromolecular compound of the glycerol is permeated among macromolecular polymers, so that the intramolecular interaction between adjacent carboxymethyl chitosan or adjacent soybean protein isolate polymer chains is reduced, the flexibility of the film is improved, and the adhesion of the preservative film spraying agent to the surface of the fruit is facilitated.
(6) The prepared edible fresh-keeping film spraying agent has better fresh-keeping effect, better film spraying effect and shorter film forming time. The addition of ethanol and the utilization of the rapid volatility of the ethanol can greatly shorten the film forming time of the preservative film spraying agent.
Drawings
FIG. 1 is a comparison of scanning electron microscope images of an edible preservative film spray prepared by the present invention and a carboxymethyl chitosan single film, wherein, (a) is a carboxymethyl chitosan single film scanning electron microscope image (5.00K), (b) is a scanning electron microscope image (5.00K), (c) is a carboxymethyl chitosan single film scanning electron microscope image (50K), and (d) is a scanning electron microscope image (50K) of an edible preservative film spray prepared by the present invention;
FIG. 2 is an infrared spectrum of the edible preservative film-spraying agent, the carboxymethyl chitosan film and the soybean protein isolate film prepared by the invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
The invention provides an edible preservation film spraying agent and a preparation method thereof.
The fresh-keeping film spraying agent comprises the following raw materials in percentage by mass: 1.8-2.5% of carboxymethyl chitosan, 1.1-1.5% of soybean protein isolate, 1.2-1.7% of polyvinylpyrrolidone-K, 0.15-0.22% of glycerol, 20-25% of absolute ethyl alcohol, 3-6% of litchi essential oil and the balance of distilled water.
Wherein, the deacetylation degree of the carboxymethyl chitosan is 90-95 percent, and the carboxylation degree is more than or equal to 80 percent; the soybean protein isolate is in food grade; the average molecular weight of polyvinylpyrrolidone is 58000, and the polyvinylpyrrolidone is food grade; the average molecular weight of glycerol is 95, and the glycerol is food grade; the absolute ethyl alcohol content is more than or equal to 99.5 percent, and the food grade is realized.
The extraction method of the litchi essential oil comprises the following steps: cleaning and airing litchi shells or litchi seeds, crushing and sieving with a 80-mesh sieve, weighing powder in a round-bottom flask, adding petroleum ether according to a certain material-liquid ratio, carrying out ultrasonic treatment at a certain temperature, carrying out vacuum filtration on an extract liquid after ultrasonic treatment, and carrying out rotary evaporation on the extract liquid to obtain the litchi essential oil.
Wherein, the ratio of the materials to the liquid is 1:4-1:10,g/mL; the boiling range of the petroleum ether is 60-90 ℃.
The ultrasonic temperature is 45-50 ℃, the ultrasonic power is 300W, and the ultrasonic time is 60 minutes.
The preparation method of the edible fresh-keeping film spraying agent comprises the following steps:
(1) Adding carboxymethyl chitosan into distilled water, and stirring until the carboxymethyl chitosan is completely dissolved;
(2) Adding the isolated soy protein into the solution obtained in the step (1), and quickly stirring at 300r/min for 30min; then carrying out ultrasonic treatment for 20min under the power of 350W-450W;
(3) Adding polyvinylpyrrolidone-K30 serving as a film-forming enhancer into the solution treated in the step (2), and stirring at 300r/min for 20min;
(4) Continuously adding glycerol as plasticizer, and stirring at 300r/min for 20min;
(5) Adding litchi essential oil, and stirring at 200r/min for 20min;
(6) Slowly adding absolute ethyl alcohol into the solution obtained in the step (5), and stirring for 30min at 200 r/min;
(7) Performing ultrasonic treatment on the solution obtained in the step (6) at 100W power for 20min to remove bubbles in the solution;
(8) Filtering to remove solid residues in the solution to obtain the uniform edible fresh-keeping film spraying agent.
The following description is given with reference to specific embodiments.
Example 1
Adding 2.5g of carboxymethyl chitosan into 70mL of distilled water, stirring until the carboxymethyl chitosan is completely dissolved, then adding 1.5g of soybean protein isolate as a film forming raw material into the film forming solution, quickly stirring for 30min at 300r/min, continuously adding 1.5g of polyvinylpyrrolidone-K30 as a film forming enhancer into the film forming solution, quickly stirring for 20min at 300r/min, then adding 1mL of glycerol as a plasticizer into the film forming solution, quickly stirring for 20min at 300r/min, then adding 5mL of litchi essential oil as an antioxidant, and stirring for 20min at 200 r/min; and adding 25mL of absolute ethyl alcohol, stirring at 200r/min for 30min, finally performing ultrasonic treatment at 100W power for 20min to perform defoaming, and filtering to obtain the edible preservative film spraying agent.
1mL of the edible preservative film spraying agent is dripped on a glass plate and is evenly coated by a coater, and the film forming time is measured to be 16s.
Accurately transferring 3mL of edible fresh-keeping film spraying agent and 3mL of 0.1mmol/LDPPH solution, adding the edible fresh-keeping film spraying agent and the 3mL of 0.1mmol/LDPPH solution into the same colorimetric tube, shaking uniformly, standing at room temperature in the dark for 30min, determining the absorbance As of the edible fresh-keeping film spraying agent, determining the absorbance Ac of the mixture of 3mL of 30% absolute ethyl alcohol and 3mL of LDPPH solution, and determining the absorbance Ab of the mixture of 3mL of edible fresh-keeping film spraying agent and 3mL of 30% absolute ethyl alcohol. The DPPH radical clearance was calculated to be 19.857% using the formula DPPH radical clearance = (1- (As-Ab)/Ac) × 100%.
Accurately transferring 5mL of the edible preservative film spraying agent into a circular mold with the diameter of 6.3cm, putting the circular mold into a drying oven with the temperature of 65 ℃, softening the circular mold, and demolding to obtain the preservative film.
And (3) sealing the preservative film, and calculating the amount of oxygen permeating and the amount of carbon dioxide permeating according to the amount of consumed sodium thiosulfate and the amount of hydrochloric acid by using a starch indicator method and an acid-base indicator method. The oxygen transmission rate of the preservative film is measured to be 0.672 mg/(m) 2 H), carbon dioxide transmission rate 67.657 mg/(m) 2 H), oxygen transmission rate with blank 9.554 mg/(m) 2 H), carbon dioxide transmission rate 74.263 mg/(m) 2 H) comparison, the edible preservation film spraying agent of the inventionHas stronger oxygen and carbon dioxide transmission blocking performance.
The preservation effect on fresh-cut apples shows that within 6 hours, the surfaces of apples without the edible preservation film-spraying agent of the invention are browned, the surfaces of apples treated by the edible preservation film-spraying agent of the invention are not browned, the weight loss rate of the apples treated by the edible preservation film-spraying agent of the invention is only 12.264%, and compared with the weight loss rate of 17.048% of a blank group, the edible preservation film-spraying agent of the invention has better preservation effect and anti-browning capability on apples.
Comparative example
The conventional chitosan film spraying agent, carboxymethyl chitosan film spraying agent and soybean protein isolate film spraying agent in the field are taken as comparative examples, which shows that the preservation film spraying agent provided by the invention has excellent preservation performance, high-efficiency preservation effect and shorter film forming time.
Adding 2.0g of carboxymethyl chitosan, 2.0g of chitosan and 2.0g of soybean protein isolate into 70mL of distilled water respectively, stirring uniformly, then adding 0.2mL of glycerol serving as a plasticizer into the film forming solution, stirring uniformly and filtering to obtain a carboxymethyl chitosan film spraying agent, a chitosan film spraying agent and a soybean protein isolate film spraying agent respectively.
Transferring 5mL of the film spraying agent into a circular mold with the diameter of 6.3cm, respectively, drying in a 65 ℃ oven, softening, and demolding to respectively obtain the carboxymethyl chitosan film, the chitosan film and the soybean protein isolate film.
The film forming time of the carboxymethyl chitosan film spraying agent is 53s. The DPPH free radical clearance rate is 12.739%, and the oxygen transmission rate is 1.179 mg/(m) 2 H), carbon dioxide transmission rate 70.205 mg/(m) 2 .h)
The film forming time of the chitosan film spraying agent is measured to be 70s. The DPPH radical clearance rate is 11.140%. The oxygen transmission rate is 1.250 mg/(m) 2 H), carbon dioxide transmission rate of 75.866 mg/(m) 2 .h)
The film forming time of the soybean protein isolate film spraying agent is 209s. The clearance of DPPH free radicals is 0.782%. The oxygen transmission rate is 1.840 mg/(m) 2 H), oxidizing with oxygenCarbon transmittance 70.017 mg/(m) 2 .h)
The 6-hour fresh-keeping effect on the fresh-cut apples shows that the weight loss rates of the apples subjected to the film spraying treatment by the carboxymethyl chitosan film spraying agent, the chitosan film spraying agent and the soybean protein isolate film spraying agent are respectively 18.23%,20.75% and 22.62%. The edible preservation film spraying agent has stronger barrier property than carboxymethyl chitosan film spraying agent, chitosan film spraying agent and soybean protein isolate film spraying agent, and can effectively prevent the loss of water.
Example 2
Adding 2g of carboxymethyl chitosan into 70mL of distilled water, stirring until the carboxymethyl chitosan is completely dissolved, then adding 1.3g of soybean protein isolate as a film forming raw material into the film forming solution, quickly stirring for 30min at 300r/min, continuously adding 1.5g of polyvinylpyrrolidone as a film forming enhancer into the film forming solution, quickly stirring for 20min at 300r/min, then adding 0.2mL of glycerol as a plasticizer into the film forming solution, quickly stirring for 20min at 300r/min, then adding 4mL of litchi essential oil as an antioxidant, and stirring for 20min at 200 r/min; and adding 20mL of absolute ethyl alcohol, stirring at 200r/min for 30min, finally performing ultrasonic treatment at 100W power for 20min for defoaming, and filtering to obtain the fresh-keeping film spraying agent.
The film forming time of the fresh-keeping film spraying agent is 19s, the DPPH free radical clearance rate is 20.46%, and the oxygen transmission rate is 0.648 mg/(m) 2 H), carbon dioxide transmission rate 65.389 mg/(m) 2 .h)
The fresh-keeping effect on fruits such as apples, grapes and blueberries shows that the spoilage rates of the apples, the grapes and the blueberries treated by the fresh-keeping film spraying agent are 0% after 7 days.
The microstructure of the preservative film-spraying agent film and the single carboxymethyl chitosan film is observed by a scanning electron microscope, and the distribution condition of the auxiliary film-forming material in the carboxymethyl chitosan is known. The scanning electron micrographs of the CMCTS/SPI composite membrane and the carboxymethyl chitosan single membrane magnified 5000 times are shown in FIG. 1 (a) and FIG. 1 (b), and the micrographs magnified 5 ten thousand times are shown in FIG. 1 (c) and FIG. 1 (d).
As can be seen from the scanning electron microscope photograph of the film surface in FIG. 1, the prepared carboxymethyl chitosan film and the preservation film spraying agent film have uniform, smooth and compact surface layers, and the preservation film spraying agent film surface is more uniform and smooth than the carboxymethyl chitosan film surface, which shows that the carboxymethyl chitosan and the soybean protein isolate can be completely penetrated and fused, and no large gap exists between the carboxymethyl chitosan and the soybean protein isolate, so that the blended film has good performance.
FIG. 2 shows that the concentration of the edible preservative film-spraying agent (CMCTS/SPI composite film-spraying agent) and the control group (carboxymethyl chitosan film-spraying agent (CMCTS film), soy protein isolate film-spraying agent (SPI film)) is 4000-500cm -1 The wavelength range exhibits similar infrared spectra. Wherein the edible fresh-keeping film spraying agent is 3428cm -1 、1641cm -1 、1078cm -1 Corresponding to-OH and-NH in 3 membranes, respectively 2 Contraction vibration of amide I band C = O, contraction vibration of C-O, and the spectrum is 1641cm -1 The vibration was strongly absorbed, and the presence of carboxyl groups was confirmed, while the peak of-COOH was 1710cm -1 The edible preservation film-spraying agent of the invention is described as COO in carboxyl - Is in the form of 2921cm -1 、1401cm -1 、580cm -1 Respectively corresponding to CH in the composite film spraying agent and the SPI 2 -CH 3 C-N and amide II with N-H contraction vibration and C = C trans contraction vibration, and compared with the spectral lines of the experimental group and the comparative group, the edible fresh-keeping film spraying agent is 1401cm -1 The peak is narrowed and shifted, which is probably due to the formation of hydrogen and ionic bonds, making-NH 2 The number is reduced. As shown above, no new covalent bond is generated in the edible fresh-keeping film spraying agent, but hydrogen bonds and ionic bonds are formed, and the bonds are probably the reason why the carboxymethyl chitosan can be assembled with the soybean protein isolate into a film.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (5)
1. An edible fresh-keeping film spraying agent is characterized in that: the raw materials comprise the following components in percentage by mass: 1.8-2.5% of carboxymethyl chitosan, 1.1-1.5% of soybean protein isolate, 301.2-1.7% of polyvinylpyrrolidone-K, 0.15-0.22% of glycerol, 20-25% of absolute ethyl alcohol, 3-6% of litchi essential oil and the balance of distilled water;
the deacetylation degree of the carboxymethyl chitosan is 90-95%, and the carboxylation degree is more than or equal to 80%; the soybean protein isolate is in food grade; the average molecular weight of polyvinylpyrrolidone-K30 is 58000, and the polyvinylpyrrolidone is food grade; the average molecular weight of the glycerol is 95, and the glycerol is food grade; the absolute ethyl alcohol content is more than or equal to 99.5 percent, and the food grade is realized;
the preparation method of the film spraying agent comprises the following steps:
(1) Adding carboxymethyl chitosan into distilled water, and stirring until the carboxymethyl chitosan is completely dissolved;
(2) Adding the isolated soy protein into the solution obtained in the step (1), and quickly stirring at 300r/min for 30min; then carrying out ultrasonic treatment for 20min under the power of 350-450W;
(3) Adding polyvinylpyrrolidone-K30 serving as a film-forming enhancer into the solution treated in the step (2), and stirring at 300r/min for 20min;
(4) Continuously adding glycerol as plasticizer, and stirring at 300r/min for 20min;
(5) Adding litchi essential oil, and stirring at 200r/min for 20min;
(6) Slowly adding absolute ethyl alcohol into the solution obtained in the step (5), and stirring for 30min at 200 r/min;
(7) Performing ultrasonic treatment on the solution obtained in the step (6) for 20min at the power of 100W to remove bubbles in the solution;
(8) Filtering to remove solid residues in the solution to obtain the uniform edible fresh-keeping film spraying agent.
2. The edible preservative film spray according to claim 1, wherein: the raw materials comprise the following components in percentage by mass: 2% of carboxymethyl chitosan, 1.3% of soybean protein isolate, 301.5% of polyvinylpyrrolidone-K, 0.2% of glycerol, 23.7% of absolute ethyl alcohol, 4% of litchi essential oil and the balance of distilled water.
3. The edible preservative film spray according to claim 1, wherein: the extraction method of the litchi essential oil comprises the following steps: cleaning and airing litchi shells or litchi seeds, crushing and sieving with a 80-mesh sieve, weighing powder in a round-bottom flask, adding petroleum ether according to a certain material-liquid ratio, carrying out ultrasonic treatment at a certain temperature, carrying out vacuum filtration on an extract liquid after ultrasonic treatment, and carrying out rotary evaporation on the extract liquid to obtain the litchi essential oil.
4. An edible preservative film spray according to claim 3, wherein: the ratio of the material to the liquid is 1:4-1:10,g/mL; the petroleum ether boiling range is 60-90 ℃.
5. An edible preservative film spray according to claim 3, wherein: the ultrasonic temperature is 45-50 ℃, the ultrasonic power is 300W, and the ultrasonic time is 60 minutes.
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