CN112048090B - Water-absorbing antibacterial degradable fresh-water fish preservative film and preparation method thereof - Google Patents
Water-absorbing antibacterial degradable fresh-water fish preservative film and preparation method thereof Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/46—Applications of disintegrable, dissolvable or edible materials
- B65D65/466—Bio- or photodegradable packaging materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/04—Oxycellulose; Hydrocellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2425/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2425/02—Homopolymers or copolymers of hydrocarbons
- C08J2425/04—Homopolymers or copolymers of styrene
- C08J2425/06—Polystyrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/04—Polyamides derived from alpha-amino carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biodiversity & Conservation Biology (AREA)
- Mechanical Engineering (AREA)
- Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
Abstract
The invention discloses a water-absorbing antibacterial degradable fresh-water fish preservative film and a preparation method thereof, wherein the preservative film comprises microcrystalline cellulose aqueous suspension, gamma-polyglutamic acid aqueous suspension, epsilon-polylysine and plasticizer; the mass ratio of the microcrystalline cellulose aqueous suspension to the gamma-polyglutamic acid aqueous suspension is 2:1; the addition amount of epsilon-polylysine is 1-5wt% of the total mass of the microcrystalline cellulose aqueous suspension and the gamma-polyglutamic acid aqueous suspension; the addition amount of the plasticizer is 1-2 wt% of the total mass of the microcrystalline cellulose aqueous suspension and the gamma-polyglutamic acid aqueous suspension. According to the invention, three edible substrates of epsilon-polylysine, polyglutamic acid and microcrystalline cellulose are used, microcrystalline cellulose is used as a film forming matrix, polyglutamic acid is used as a water absorbent, epsilon-polylysine is used as an antibacterial agent, and a three-in-one functional preservative film material integrating bacteriostasis, moisture regulation and degradation is developed, and the three-in-one functional preservative film material has a three-dimensional net-shaped hydrogel structure, so that effective adsorption of blood water of meat products is realized, and bacterial contamination is avoided; meanwhile, the hydrogel has the effects of moisturizing and locking water, so that the product can be prevented from excessive water loss and deterioration.
Description
Technical Field
The invention belongs to the technical field of preservation of aquatic products, and particularly relates to a water-absorbing antibacterial degradable fresh-water fish preservative film and a preparation method thereof.
Background
The fresh water fish is easy to cause the decomposition of fish protein after capturing and during processing to cause the fish to generate bad smell so as to change the original flavor of the fish, meanwhile, the fresh water fish is easy to be infected by spoilage bacteria, endogenous enzymes and chemical actions to lose freshness and deteriorate in the storage process due to various microorganisms which cause the spoilage of fish bodies. The fresh fish flesh is also inevitably free from juice flowing out during the storage and transportation process, and the flowing-out juice not only affects the appearance and sense of fish flesh products, but also can cause secondary pollution and seriously affects the commercial value of the fish flesh. Refrigeration and preservative combined preservation are traditional methods for controlling food spoilage, but the food spoilage caused by various factors and serious harm to economy and human health can be caused by damage to organisms after people eat due to the residues of the preservatives.
Therefore, how to keep good eating quality of the freshwater fish and improve the appearance of fish products has important significance for the fresh-keeping processing industry of the freshwater fish. Most of the traditional PE (polyethylene) preservative films used in the market at present have the basic functions of isolating air, reducing pollution of mixed bacteria in the air to products and the like, but can only enable fresh fish to be continuously preserved for 2-3 days, and the shelf life is short; the traditional PE preservative film has poor degradability, and long-term overstock can cause great hidden trouble to the environment and human health; and the traditional PE preservative film has poor water absorbability, can not absorb the common bleeding and exudation problems of meat products, and has great influence on the quality and economic and environmental protection of the meat products. Therefore, we propose an application of the water-absorbing antibacterial degradable preservative film in fresh-keeping of freshwater fish, so as to make up for the defect of the performance of the traditional preservative film, and focus on increasing the application range of the preservative film in absorbing blood exudation of meat products.
Disclosure of Invention
The invention aims to: the technical problem to be solved by the invention is to provide the fresh-water fish preservative film with water absorption, bacteriostasis and degradability and the preparation method thereof aiming at the common problem of the traditional PE preservative film in the preservation of meat products, so as to solve two key problems that the appearance and bacterial contamination and spoilage are affected by the blood extravasation of the fresh-water fish products in the processing, storage and transportation processes.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a water-absorbing bacteriostatic degradable fresh-water fish preservative film, comprising:
an aqueous suspension of microcrystalline cellulose (MCC),
an aqueous suspension of gamma-polyglutamic acid (gamma-PGA),
epsilon-polylysine (epsilon-PL), and
a plasticizer;
wherein the mass ratio of the microcrystalline cellulose (MCC) aqueous suspension to the gamma-polyglutamic acid (gamma-PGA) aqueous suspension is 2:1;
the addition amount of the epsilon-polylysine (epsilon-PL) is 1-5wt% of the total mass of the microcrystalline cellulose aqueous suspension and the gamma-polyglutamic acid aqueous suspension;
the addition amount of the plasticizer is 1-2 wt% of the total mass of the microcrystalline cellulose aqueous suspension and the gamma-polyglutamic acid aqueous suspension.
Microcrystalline cellulose (MCC) is a linear polysaccharide connected by beta-1, 4 glucosidic bonds, is a white powdery substance obtained by physical or chemical treatment of natural cellulose, is a pure depolymerized product of cellulose, has a large specific surface area and a low degree of polymerization, has an average degree of polymerization reaching the limit of the degree of polymerization, has strong water absorption, can form gel after being subjected to shearing stress in an aqueous medium, and is used as a film forming matrix of a preservative film.
The repulsive effect of a large number of carboxyl negative charges on the gamma-PGA side chain makes the space extension of the molecular chain very large, even at lower concentration, the molecular interaction is strong, the gamma-PGA is an amino acid homopolymer with the molecular weight reaching millions, the gamma-PGA has high water absorption performance, biological safety and salt resistance, and the leached blood component in the chilled fresh fish meat belongs to a complex electrolyte solution, and the main factor influencing the film adsorption is NaCl, so the gamma-PGA can be used as an excellent high salt resistance water absorbent.
The epsilon-PL has good inhibition effect on gram-positive bacteria, gram-negative bacteria, saccharomycetes, mould and the like, has broad-spectrum antibacterial property, and can be used as an excellent antibacterial agent.
The addition of plasticizer can improve the film performance, reduce the film cohesion, and increase the flexibility and the folding resistance of the polymer chain.
Preferably, the concentration of the aqueous microcrystalline cellulose suspension is between 6 and 10wt%.
Preferably, the concentration of the gamma-polyglutamic acid aqueous suspension is 5-15wt%, wherein the molecular weight of gamma-polyglutamic acid is 50-100 Da.
Preferably, the plasticizer is any one of glycerin, xylitol, sorbitol, ethylene glycol or polystyrene. Glycerol is preferred.
Further, the invention also provides a preparation method of the water-absorbing antibacterial degradable fresh water fish preservative film, which comprises the following steps:
(1) Preparing microcrystalline cellulose aqueous suspension and gamma-polyglutamic acid aqueous suspension respectively;
(2) Mixing and stirring the microcrystalline cellulose aqueous suspension prepared in the step (1) and the gamma-polyglutamic acid aqueous suspension to obtain microcrystalline cellulose-gamma-polyglutamic acid mixed solution;
(3) Sequentially adding epsilon-polylysine and a plasticizer into the microcrystalline cellulose-gamma-polyglutamic acid mixed solution obtained in the step (2), homogenizing, uniformly stirring at the temperature of 40-60 ℃ in a water bath, naturally cooling, and degassing to obtain a membrane solution;
(4) And (3) uniformly pouring the film liquid obtained in the step (3) into a mold disc, standing for film formation, and then drying to obtain the film.
Specifically, in the step (2), the magnetic stirrer is adopted for stirring for 30-60 min at the rotating speed of 600-1200 r/min.
In the step (3), homogenizing for 5-10min at 15000-20000 rpm by adopting a high-speed dispersing machine; the stirring speed in the water bath is 600-800 r/mm, and the time is 15-30min; the degassing adopts ultrasonic degassing, the frequency of the ultrasonic degassing is 35-45HZ, and the time of the ultrasonic degassing is 20-30 min.
In the step (4), pouring the film liquid into a mould disc, and standing for film forming for 18-24 hours; the temperature of the drying is 35-40 ℃ and the time is controlled to be 20-24 hours.
The invention further provides a fresh-keeping method for fresh-water fish by adopting the water-absorbing and bacteria-inhibiting degradable fresh-water fish preservative film, which comprises the steps of killing fresh-water fish, removing viscera, cleaning with deionized water, slicing, wrapping with the water-absorbing and bacteria-inhibiting degradable fresh-water fish preservative film, putting into a refrigerator, and refrigerating at the temperature of 4+/-1 ℃.
The beneficial effects are that:
1. according to the invention, three edible substrates of epsilon-polylysine, polyglutamic acid and microcrystalline cellulose are used, microcrystalline cellulose is used as a film forming matrix, polyglutamic acid is used as a water absorbent, epsilon-polylysine is used as an antibacterial agent, and a three-in-one functional preservative film material integrating bacteriostasis, moisture regulation and degradation is developed, and the three-in-one functional preservative film material has a three-dimensional net-shaped hydrogel structure, so that effective adsorption of blood water of meat products is realized, and bacterial contamination is avoided; meanwhile, the hydrogel has the effects of moisturizing and locking water, so that the product can be prevented from excessive water loss and deterioration.
2. The invention realizes the food active package combining the antistaling agent and the packaging material, and has the characteristics of safety, no toxicity, strong antibacterial property, broad antibacterial spectrum and the like. The combined fresh-keeping method of low temperature and organisms, which is developed aiming at the special spoilage characteristics of the freshwater fish, can effectively adsorb blood of the freshwater fish, inhibit the growth and propagation of microorganisms, has good biodegradability, better prolongs the quality of the freshwater fish and application thereof, and solves the technical problems of poor edible quality, potential safety hazard, short fresh-keeping period and the like of the freshwater fish after being treated by the traditional fresh-keeping method.
Drawings
The foregoing and/or other advantages of the invention will become more apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings and detailed description.
Fig. 1 is an appearance diagram of the preservative film prepared in example 3.
Fig. 2 is an appearance diagram of the preservative film prepared in example 5.
Fig. 3 is a graph showing the change in the volatile basic nitrogen value (TVB-N) of fresh water fish meat during storage of the preservative film of each of the experimental group and the control group.
Fig. 4 is a graph showing the change in total colony count (TVC) of fresh water fish meat during storage of the preservative film in each of the experimental group and the control group.
Fig. 5 is an adsorption power curve of the preservative films of each experimental group and the control group.
FIG. 6 is a graph showing the change in the weight loss rate of each of the experimental group and the control group in the indoor soil-buried degradation test.
Detailed Description
The invention will be better understood from the following examples.
Example 1
The embodiment provides a fresh-water fish preservative film, which is prepared by the following steps:
(1) Weighing MCC, dissolving in distilled water to prepare an MCC water suspension with the concentration of 6wt% (when the MCC is dissolved, the MCC is slowly added into the distilled water under the action of a magnetic stirrer), and magnetically stirring for 30min;
weighing gamma-PGA (molecular weight of 50 Da) and dissolving in distilled water to prepare gamma-PGA water suspension with concentration of 5wt% (when the gamma-PGA is dissolved, the gamma-PGA is slowly added into the distilled water under the action of a magnetic stirrer) and magnetically stirring for 30min;
(2) Stirring the MCC water suspension and the gamma-PGA water suspension prepared in the step (1) for 30min at the rotating speed of 600r/min by adopting a magnetic stirrer according to the mass ratio of 2:1 to obtain an MCC-gamma-PGA mixed solution;
(3) Sequentially adding epsilon-PL (the addition amount is 1% of the mass of the microcrystalline cellulose-gamma-polyglutamic acid mixed solution) and plasticizer (the addition amount is 2% of the mass of the microcrystalline cellulose-gamma-polyglutamic acid mixed solution) into the microcrystalline cellulose-gamma-polyglutamic acid mixed solution obtained in the step (2), homogenizing for 5min by adopting a high-speed dispersing machine at 15000rpm, then stirring for 15min at the rotating speed of 600r/min at the temperature of 60 ℃ in an electric constant-temperature water bath kettle, naturally cooling, and performing ultrasonic degassing for 20min at the temperature of 35HZ to obtain film liquid;
(4) And (3) uniformly pouring the film liquid obtained in the step (3) into a mold disc, standing for 18h to form a film, then placing the film liquid into an oven, drying at 35 ℃ for 20h, and cooling to obtain the preservative film.
Example 2
(1) Weighing MCC, dissolving in distilled water to prepare an MCC water suspension with the concentration of 8wt% (when the MCC is dissolved, the MCC is slowly added into the distilled water under the action of a magnetic stirrer), and magnetically stirring for 30min;
weighing gamma-PGA (molecular weight of 100 Da), dissolving in distilled water to prepare gamma-PGA water suspension with concentration of 15wt% (when gamma-PGA is dissolved, gamma-PGA is slowly added into distilled water under the action of a magnetic stirrer), and magnetically stirring for 30min;
(2) Stirring the MCC water suspension and the gamma-PGA water suspension prepared in the step (1) for 30min at the rotating speed of 1000r/min by adopting a magnetic stirrer according to the mass ratio of 2:1 to obtain an MCC-gamma-PGA mixed solution;
(3) Sequentially adding epsilon-PL (the addition amount is 5% of the mass of the microcrystalline cellulose-gamma-polyglutamic acid mixed solution) and plasticizer (the addition amount is 1% of the mass of the microcrystalline cellulose-gamma-polyglutamic acid mixed solution) into the microcrystalline cellulose-gamma-polyglutamic acid mixed solution obtained in the step (2), homogenizing for 10min by adopting a high-speed dispersing machine at 18000rpm, then stirring for 20min at the rotating speed of 800r/min in a water bath constant-temperature magnetic stirrer, and carrying out ultrasonic degassing for 25min at the rotating speed of 40HZ after natural cooling to obtain a film liquid;
(4) And (3) uniformly pouring the film liquid obtained in the step (3) into a mold disc, standing for 24 hours to form a film, then placing the film liquid into an oven, drying the film liquid at 35 ℃ for 24 hours, and cooling the film liquid to obtain the preservative film.
Example 3
(1) Weighing MCC, dissolving in distilled water to prepare an MCC water suspension with the concentration of 10wt% (when the MCC is dissolved, the MCC is slowly added into the distilled water under the action of a magnetic stirrer), and magnetically stirring for 30min;
weighing gamma-PGA (molecular weight of 50 Da) and dissolving in distilled water to prepare a gamma-PGA aqueous suspension with concentration of 10wt% (when the gamma-PGA is dissolved, the gamma-PGA is slowly added into the distilled water under the action of a magnetic stirrer) and magnetically stirring for 30min;
(2) Stirring the MCC water suspension and the gamma-PGA water suspension prepared in the step (1) for 30min at the rotating speed of 1000r/min by adopting a magnetic stirrer according to the mass ratio of 2:1 to obtain an MCC-gamma-PGA mixed solution;
(3) Sequentially adding epsilon-PL (the addition amount is 3% of the mass of the microcrystalline cellulose-gamma-polyglutamic acid mixed solution) and plasticizer (the addition amount is 1% of the mass of the microcrystalline cellulose-gamma-polyglutamic acid mixed solution) into the microcrystalline cellulose-gamma-polyglutamic acid mixed solution obtained in the step (2), homogenizing for 5min by adopting a high-speed dispersing machine at 20000rpm, then stirring for 30min at the rotating speed of 800r/min at the temperature of 60 ℃ in an electric heating constant-temperature water bath kettle, naturally cooling, and performing ultrasonic degassing for 30min at the temperature of 40HZ to obtain film liquid;
(4) And (3) uniformly pouring the film liquid obtained in the step (3) into a mold disc, standing for 24 hours to form a film, then placing the film liquid into an oven, drying the film liquid at 35 ℃ for 24 hours, and cooling the film liquid to obtain the preservative film, wherein the preservative film is shown in figure 1.
Example 4
(1) Weighing MCC, dissolving in distilled water to prepare an MCC water suspension with the concentration of 8wt% (when the MCC is dissolved, the MCC is slowly added into the distilled water under the action of a magnetic stirrer), and magnetically stirring for 30min;
weighing gamma-PGA (molecular weight of 80 ten thousand Da), dissolving in distilled water to prepare gamma-PGA water suspension with concentration of 10wt% (when gamma-PGA is dissolved, gamma-PGA is slowly added into distilled water under the action of a magnetic stirrer), and magnetically stirring for 30min;
(2) Stirring the MCC water suspension and the gamma-PGA water suspension prepared in the step (1) for 45min at the rotating speed of 1000r/min by adopting a magnetic stirrer according to the mass ratio of 2:1 to obtain an MCC-gamma-PGA mixed solution;
(3) Sequentially adding epsilon-PL (the addition amount is 5% of the mass of the microcrystalline cellulose-gamma-polyglutamic acid mixed solution) and plasticizer (the addition amount is 1.5% of the mass of the microcrystalline cellulose-gamma-polyglutamic acid mixed solution) into the microcrystalline cellulose-gamma-polyglutamic acid mixed solution obtained in the step (2), homogenizing for 8min by adopting a high-speed dispersing machine at 20000rpm, then stirring for 30min at the speed of 800r/min in an electric heating constant-temperature water bath kettle, and carrying out ultrasonic degassing for 30min at the speed of 40HZ after natural cooling to obtain film liquid;
(4) And (3) uniformly pouring the film liquid obtained in the step (3) into a mold disc, standing for 24 hours to form a film, then placing the film liquid into an oven, drying the film liquid at 38 ℃ for 22 hours, and cooling the film liquid to obtain the preservative film.
Example 5
(1) Weighing MCC, dissolving in distilled water to prepare an MCC water suspension with the concentration of 10wt% (when the MCC is dissolved, the MCC is slowly added into the distilled water under the action of a magnetic stirrer), and magnetically stirring for 30min;
weighing gamma-PGA (molecular weight of 50 Da) and dissolving in distilled water to prepare a gamma-PGA aqueous suspension with concentration of 12wt% (when the gamma-PGA is dissolved, the gamma-PGA is slowly added into the distilled water under the action of a magnetic stirrer) and magnetically stirring for 30min;
(2) Stirring the MCC water suspension and the gamma-PGA water suspension prepared in the step (1) for 60min at the rotating speed of 1200r/min by adopting a magnetic stirrer according to the mass ratio of 2:1 to obtain an MCC-gamma-PGA mixed solution;
(3) Sequentially adding epsilon-PL (the addition amount is 3% of the mass of the microcrystalline cellulose-gamma-polyglutamic acid mixed solution) and plasticizer (the addition amount is 2% of the mass of the microcrystalline cellulose-gamma-polyglutamic acid mixed solution) into the microcrystalline cellulose-gamma-polyglutamic acid mixed solution obtained in the step (2), homogenizing for 5min by adopting a high-speed dispersing machine at 20000rpm, then stirring for 30min at the rotating speed of 700r/min in an electric heating constant-temperature water bath kettle, naturally cooling, and performing ultrasonic degassing for 30min at the temperature of 45HZ to obtain film liquid;
(4) And (3) uniformly pouring the film liquid obtained in the step (3) into a mold plate, standing for 20 hours to form a film, then placing the film liquid into an oven, drying at 40 ℃ for 24 hours, and cooling to obtain the preservative film, wherein the preservative film is shown in figure 2.
The parameter values of examples 1 to 5 are given in table 1.
Table 1 parameter values for different embodiments
The parameters of the different embodiments range from: microcrystalline cellulose concentration 6-10wt%; the concentration of the gamma-polyglutamic acid is 5-15wt%; the molecular weight of the gamma-polyglutamic acid is 50 ten thousand-100 ten thousand Da; the concentration of epsilon-polylysine is 1-5%; plasticizer concentration 1-2%; the rotation speed and the stirring time of the magnetic stirrer are 600-1200 and 30-60 respectively; the rotating speed and the homogenizing time of the high-speed homogenizer are 15000-20000 and 5-10min respectively; the temperature, the rotating speed and the time of the water bath constant temperature magnetic stirrer are respectively 40-60 ℃, 600-800 r/mm and 15-30min; the ultrasonic degassing frequency and time are respectively 35-45HZ and 20-30min; standing the membrane liquid for 18-24 hours; the film drying temperature and time are respectively 35-40 ℃ and 20-24 hours.
To demonstrate the synergistic effect of the four components of the present invention (MCC, γ -PGA, ε -PL, glycerol), two comparative experiments, MCC+γ -PGA+glycerol and MCC+ε -PL+glycerol, were added, and the specific parameters are shown in Table 2.
Table 2 parameter values for comparative experiments
Test 1 specific procedure:
(1) Respectively preparing MCC aqueous suspension and gamma-PGA aqueous suspension, stirring for 30min at the rotating speed of 1000r/min by adopting a magnetic stirrer according to the mass ratio of 2:1, and mixing to obtain MCC-gamma-PGA mixed solution;
(2) Adding plasticizer glycerol (the addition amount is 1-2% of the mass of the MCC-gamma-PGA mixed solution) into the MCC-gamma-PGA mixed solution obtained in the step (1);
(3) Homogenizing for 5min at 20000rpm by adopting a high-speed dispersing machine, then stirring for 30min at the speed of 800r/min in an electric heating constant-temperature water bath kettle, naturally cooling, ultrasonically degassing for 30min at 40HZ to obtain film liquid, uniformly pouring the film liquid into a mould plate, standing for 24h to form a film, then placing in an oven, drying for 24h at the temperature of 35 ℃, and cooling to obtain the preservative film.
The difference from test 1 is that test 2 gives a MCC-. Epsilon. -PL mixture, and the rest are the same.
The fresh freshwater fish is killed, eviscerated, washed by deionized water, sliced, wrapped by the water-absorbing antibacterial degradable freshwater fish preservative film and the common preservative film (PE) prepared in examples 1-5 and comparative experiments 1 and 2 respectively, and put into a refrigerator for refrigeration at the temperature of 4+/-1 ℃.
The TVB-N (volatile basic nitrogen) evaluation method is one of main chemical indexes for judging the freshness of the fish, and according to the industry standard specification of the freshness of aquatic products in China, the TVB-N value of a first-grade product of the freshwater fish is less than or equal to 13mg/100g, the TVB-N value of a second-grade product is less than or equal to 20mg/100g, and the acceptable TVB-N value of the fish meat is 35-40 mg/100g. The freshness measurement was carried out by referring to the semi-trace nitrogen determination method in national standard GB 5009.44-2003, the unit being expressed in mg/100g of sample. The specific operation is as follows: weighing about 10.0g of a sample refrigerated for a certain time, homogenizing by using a homogenizer, pouring into a conical flask, adding 100mL of water, soaking for 30min, filtering, and collecting filtrate in a refrigerator for later use; placing a conical flask containing 10mL of boric acid absorption liquid (20 g/L) and 5-6 drops of mixed indicator liquid (equal amount of mixed methyl red ethanol indicator of 2g/L and methylene blue indicator of 1 g/L) at the lower end of a condensing tube, accurately sucking 5.0mL of sample filtrate in a distiller reaction chamber, adding 5mL of magnesium oxide suspension (10 g/L), rapidly covering a plug, introducing steam for distillation, stopping distillation for 5min, titrating the absorption liquid with 0.010mol/L hydrochloric acid standard solution until the end point reaches bluish purple, and simultaneously performing reagent blank test.
The TVB-N change during storage of the fillets (experimental groups) of each example is shown in FIG. 3, and the preservative film (PE) wrapped group is used as a blank control group. The results show that the TVB-N content of the fresh grass carp is close to 6mg/100g, the TVB-N value of each group of fillets is obviously increased during the storage period, and the content of the 3 sky white control group before the storage is obviously higher than that of the other five groups of samples, which indicates that the fillets of each experimental group maintain good freshness for 3 days before the refrigeration. The TVB-N values of the control group and the experimental group are both increased rapidly, but the TVB-N values of the examples of each group at the end of storage are respectively much smaller than those of the control group.
The TVB-N value is less than or equal to 13mg/100g and is used as the critical value of fish spoilage, and the storage shelf life of the fish slices under different conditions in each group is shown in Table 3.
TABLE 3 shelf life of fish filets in TVB-N assessment for different examples
Wherein, examples 1, 2, 3, 4 and 5 respectively compare with blank control PE group, have prolonged fresh water fish shelf life 5.5 days, 7 days, 11 days, 6 days, 8 days respectively, and example 3 shows relatively more apparent fresh-keeping effect, and it can be seen that this kind of water absorption antibacterial degradable preservative film can prolong fresh water fish 6-11 days. And compared with a blank control PE group, the comparative experiments 1 and 2 respectively prolong the shelf life of the freshwater fish by 2 days and 1.5 days. The four components of MCC+gamma-PGA+epsilon-PL+glycerin are compared with the three components of MCC+gamma-PGA+glycerin and MCC+epsilon-PL+glycerin, and the four formulations of MCC+gamma-PGA+epsilon-PL+glycerin have more remarkable fresh-keeping effect.
Microbial activity is an important cause of fish spoilage, and among various criteria, the total number of colonies is a hard index for evaluating fish spoilage. Under the general condition, the total colony count (TVC) of fresh fish is between 2 and 4log10cfu/g, when the TVC is increased to 6 to 7log10cfu/g, the fish is in the early stage of spoilage, and the maximum TVC allowable value of the prior nuisanceless aquatic product safety standard in China is 6log10cfu/g. The method for evaluating the freshwater fish meat by the microorganisms comprises the following steps: cutting fish sample, weighing 10g, placing in sterile homogenizing bag, adding 90mL of 0.9% sterile physiological saline, homogenizing for 4min, sucking 1mL of the uniform mixture, and performing 10-fold gradient dilution (10) -1 、10 -2 、10 -3 ......10 -10 ) The microorganisms were uniformly spread and cultured by sucking dilutions of different concentrations, and then the colony count was calculated, all operations were performed under aseptic conditions, and the microorganism count unit was 1g 1o cfu/g.
Changes in TVC during storage of the fish filets of each group example as shown in fig. 4, a preservative film (PE) wrap group served as a blank control group. As the storage time was prolonged, the TVC of the blank group continued to increase, in contrast to the TVC of each group of examples which did not significantly change 3 days before storage, and then continued to increase, each group of examples having significantly smaller TVC values at the end of storage than the control group.
TVC is less than or equal to 6.0log 10 cfu/g was used as a threshold for fish spoilage and the shelf life of the fillet under various conditions for each group as shown in Table 4.
Table 4 different embodiments fillet shelf life in TVC evaluation
Wherein, examples 1, 2, 3, 4 and 5 respectively compare with blank control PE group, have prolonged fresh water fish shelf life 1.7 days, 3 days, 5 days, 2 days, 4 days respectively, and example 3 shows relatively more apparent fresh-keeping effect, and it can be seen that this kind of water absorption antibacterial degradable preservative film can prolong fresh water fish 2-5 days. And compared with the blank control PE group, the fresh water fish shelf lives of the control PE group and the control PE group are respectively prolonged by 0.5 day. The four components of MCC+gamma-PGA+epsilon-PL+glycerol have more remarkable fresh-keeping effect than the four components of MCC+epsilon-PL+glycerol and the four components of MCC+gamma-PGA+glycerol.
It can be seen that the fresh-water fish meat wrapped by the water-absorbing antibacterial degradable preservative film helps to inhibit the growth of microorganisms in the fish meat, and the antibacterial effect of the embodiment 3 is superior to that of other embodiment groups. TVB-N and TVC are one of classical methods for evaluating the shelf life of aquatic products, wherein the shelf life prolonging effect of each group of fillets obtained by the TVC is short, and the shelf life prolonging effect of each group of fillets obtained by the TVB-N is long. The treatments of examples 1 and 4 did not significantly differ in shelf life extension effects on fresh water fish preservation.
The invention uses gamma-PGA as water absorbent to prepare fresh-keeping adsorption film of fresh water fish lixivium, while the leached blood component in cold fresh meat belongs to complex electrolyte solution, and the main factor affecting adsorption is NaCl, so the salt resistance of the water absorbent is an important investigation index, and physiological saline is usually adopted to simulate blood and urine as test solution of salt resistance of the water absorbent. The test adopts simulated blood (mass fraction) as follows: 88.14% deionized water, 10.00% glycerol, 1.00% NaCl, na 2 CO 3 0.40% CMC (carboxymethyl cellulose) 0.46%. The specific operation steps are as follows: weighing 0.1g of preservative film sample, putting the preservative film sample into a filter bag, putting the filter bag into a beaker, adding enough simulated blood to enable the preservative film to fully absorb water and swell, taking out the preservative film at a certain time interval at 4 ℃, filtering out redundant simulated blood through the filter bag until no liquid drops drop out within 30min, collecting and measuring the filtered liquid quantity, measuring the adsorption multiplying power of the filtered liquid quantity, and observing the relation curve of the adsorption multiplying power and time to obtain the adsorption power curve of the preservative film.
Adsorption ratio (g/g) = (mass of added test liquid-mass of filtered test liquid)/absolute dry mass of preservative film
The adsorption power curves of the preservative films prepared in each group of examples are shown in fig. 5, and the preservative film (PE) group is used as a blank control group. As the adsorption time is prolonged, the adsorption rate of the preservative film is rapidly increased within the first 40min, the adsorption rate of the simulated blood in the embodiment 3 is increased to be about 136g/g, and the adsorption rate of the simulated blood in the embodiment 1 is increased to be minimum to be about 90 g/g. Wherein, the 5 groups of examples are respectively compared with the blank control PE group, and the preservative film prepared in the example 3 has the best adsorption effect on simulated blood, and reaches 163g/g. The adsorption multiplying power increases gradually with the time, and reaches saturation. The adsorption effect of comparative tests 1 and 2 on simulated blood was up to 95g/g and 89g/g. Because the juice leaching rate in the freshwater fish meat is very slow, the gamma-PGA as the adsorption core material for preparing the preservative film can completely and effectively adsorb the exuded blood of the freshwater fish meat.
The degradation of the films prepared in each group of examples was tested by taking the weight loss ratio of the samples as a reference for the degradation study and selecting the indoor conditions. Setting indoor conditions as constant temperature and humidity box, testing at humidity of 60+ -2% and temperature of 30+ -1deg.C, selecting square sample film of 10cm×10cm, burying in soil, periodically taking out, placing the sample in container, removing residual soil and residual leaf which may affect test result with distilled water, completely cleaning, wiping with filter paper, drying in oven at 65deg.C on glass plate, and oven drying to constant weight (W) 1 ) The mass of the initial sample dried to constant weight is W 0 。
The weight loss ratio of the film is calculated as follows:
weight loss ratio I (%) = (W) 0 －W 1 )/W 0 And (5) carrying out parallel treatment for 3 times to obtain an average value, namely the calculated weight loss rate. The change of the weight loss rate of the preservative films prepared by each group of examples in the indoor soil-buried degradation test is shown in fig. 6, and the preservative film (PE) group is used as a blank control group. Along with the prolongation of the soil burying time of the preservative films prepared and obtained in five groups of examples, the weight loss rate shows the trend of increasing faster and then steadily increasing, and compared with the maximum weight change of the preservative films prepared and obtained in example 3, the weight loss rate is as high as87% and 60 days after the end of the degradation test, the preservative film is mostly completely degraded, and the change of the weight loss rate of five groups of examples after 35 days is gradually flattened, so that the biodegradability of the preservative film is better. The weight loss rate of the comparative test reaches 43% and 45% at maximum.
By combining the evaluation, the preservative film prepared by the invention has outstanding effect on fresh water fish preservation, and has obvious progress compared with the conventional PE preservative film. The preservative film prepared in the embodiment 3 has the most remarkable preservative effect on fresh water fish, can prolong the shelf life of the fresh water fish by about 5-11 days, has the adsorption multiplying power of 163g/g for simulated blood, can effectively adsorb exuded blood of the fresh water fish, has the highest weight loss rate of 87% in an indoor soil-buried degradation test, and can be degraded to be complete for the most part.
The invention provides a water-absorbing antibacterial degradable fresh-water fish preservative film, a method for preparing the same and a method for preparing the same, and particularly the method for realizing the technical scheme is a plurality of methods and paths, the above is only a preferred embodiment of the invention, and it should be pointed out that a plurality of improvements and modifications can be made by a person skilled in the art without departing from the principle of the invention, and the improvements and modifications are also regarded as the protection scope of the invention. The components not explicitly described in this embodiment can be implemented by using the prior art.
Claims (6)
1. The fresh water fish preservative film is characterized by comprising the following components in percentage by weight:
an aqueous suspension of microcrystalline cellulose and a method for producing the same,
an aqueous suspension of gamma-polyglutamic acid,
epsilon-polylysine, and
a plasticizer;
wherein the mass ratio of the microcrystalline cellulose aqueous suspension to the gamma-polyglutamic acid aqueous suspension is 2:1;
the addition amount of the epsilon-polylysine is 1-5wt% of the total mass of the microcrystalline cellulose aqueous suspension and the gamma-polyglutamic acid aqueous suspension;
the addition amount of the plasticizer is 1-2wt% of the total mass of the microcrystalline cellulose aqueous suspension and the gamma-polyglutamic acid aqueous suspension;
the concentration of the microcrystalline cellulose aqueous suspension is 6-10wt%;
the concentration of the gamma-polyglutamic acid aqueous suspension is 5-15wt%, wherein the molecular weight of gamma-polyglutamic acid is 50-100 Da;
the plasticizer is any one of glycerol, xylitol, sorbitol and ethylene glycol.
2. The method for preparing the water-absorbing antibacterial degradable fresh-water fish preservative film, which is characterized by comprising the following steps:
(1) Preparing microcrystalline cellulose aqueous suspension and gamma-polyglutamic acid aqueous suspension respectively;
(2) Mixing and stirring the microcrystalline cellulose aqueous suspension prepared in the step (1) and the gamma-polyglutamic acid aqueous suspension to obtain microcrystalline cellulose-gamma-polyglutamic acid mixed solution;
(3) Sequentially adding epsilon-polylysine and a plasticizer into the microcrystalline cellulose-gamma-polyglutamic acid mixed solution obtained in the step (2), homogenizing, uniformly stirring at the temperature of 40-60 ℃ in a water bath, naturally cooling, and degassing to obtain a membrane solution;
(4) And (3) uniformly pouring the film liquid obtained in the step (3) into a mold disc, standing for film formation, and then drying to obtain the film.
3. The method for preparing the water-absorbing antibacterial degradable fresh water fish preservative film according to claim 2, wherein in the step (2), the magnetic stirrer is adopted for stirring for 30-60 min at the rotating speed of 600-1200 r/mm.
4. The method for preparing the water-absorbing antibacterial degradable fresh water fish preservative film according to claim 2, which is characterized in that in the step (3), a high-speed dispersing machine is adopted for homogenizing for 5-10min at 15000-20000 rpm; the stirring speed in the water bath is 600-800 r/min, and the stirring time is 15-30min; the degassing is carried out by adopting ultrasonic, the frequency of the ultrasonic degassing is 35-45HZ, and the time of the ultrasonic degassing is 20-30 min.
5. The method for preparing the fresh-water fish preservative film with water absorption, bacteriostasis and degradability according to claim 2, which is characterized in that in the step (4), the film liquid is poured into a mold disc and kept stand for film forming time of 18-24 hours; the temperature of the drying is 35-40 ℃ and the time is controlled to be 20-24 hours.
6. The method for fresh-keeping fresh water fish by adopting the fresh-keeping film for water-absorbing and bacteria-inhibiting degradable fresh water fish according to claim 1 is characterized in that the fresh water fish is killed, eviscerated, washed by deionized water, sliced, wrapped by the fresh-keeping film for water-absorbing and bacteria-inhibiting degradable fresh water fish and then put into a refrigerator for refrigeration at the temperature of 4+/-1 ℃.
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| CN104544472A (en) * | 2014-12-26 | 2015-04-29 | 山东省药学科学院 | Shrimp preservative containing pulullan polysaccharide |
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