CN113186613A - Nanofiber indicating film for intelligently detecting marine fish spoilage and application thereof - Google Patents
Nanofiber indicating film for intelligently detecting marine fish spoilage and application thereof Download PDFInfo
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Images
Classifications
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- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
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- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/06—Dyes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
The invention provides a nanofiber indicating membrane for intelligently detecting marine fish spoilage and application thereof, and relates to the technical field of nano materials. The invention uses anthocyanin and curcumin as double-color-changing agents, combines gelatin and nano chitin to prepare spinning solution, and then processes and shapes the spinning solution by using an electrostatic spinning technology to obtain the nano fiber indicating membrane. The nanofiber indicating film disclosed by the invention has higher color development capability and stability, and can be used for rapidly detecting the putrefaction and deterioration conditions of the marine fishes.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a nanofiber indicating membrane for intelligently detecting marine fish spoilage and application thereof.
Background
The fresh seawater fish meat has fresh and tender texture and delicious taste, is rich in protein, polyunsaturated fatty acid, mineral substances, trace elements and other nutrient elements, and is popular with consumers at home and abroad. However, fresh marine fishes are very easily polluted by microorganisms during storage, processing and sale to generate alkaline gases such as volatile amines, and the like, so that the fresh marine fishes are putrefy and deteriorated and have low quality. Therefore, how to realize the rapid detection of the freshness of the fish meat is particularly important.
At present, the method for detecting the deterioration of marine fishes mainly utilizes large-scale detection equipment, has a long detection period and cannot be used in actual life. The food freshness indicating intelligent film taking the food-borne natural pigment and the macromolecular compound as the matrixes becomes a research hotspot because the film can monitor the volatile ammonia generated by the food spoilage bacteria at any time. Anthocyanin, as a natural gas-sensitive pigment, can react with putrefactive gases (volatile amines) to generate obvious color change, and is an ideal freshness indicator. However, anthocyanins are unstable and are susceptible to factors such as temperature, light, oxygen, etc. In addition, anthocyanins are relatively stable at pH 3-7, red or pink, which may result in an indicator film that does not develop accurately as the volatile amine content changes. Therefore, how to construct an anthocyanin-based indicator film and make the anthocyanin-based indicator film quickly and accurately respond to a volatile amine reaction is a problem to be solved at present.
Chinese patent CN202010579557.0 discloses a beet red element-based convenient poultry and fish and shrimp freshness intelligent indicating film and a preparation method thereof. The betanin in the intelligent indicating film responds to the putrefaction of fresh poultry meat and fishes and shrimps to generate biogenic amine, and the color of the intelligent indicating film is gradually changed from red/pink into yellow or even colorless; and comparing the reacted intelligent indicating film with a standard colorimetric card, calculating the content of the biogenic amine in the sample, and judging the freshness of the biogenic amine.
A pH-sensitive freshness detection intelligent label, a preparation method and application thereof are disclosed in the patent No. CN 201911165467.0. According to the technology, bromocresol purple/methyl red is used as a color developing agent, polyvinyl alcohol/methyl cellulose is used as a film forming base material, and the pH sensitive freshness detection intelligent label is prepared and used for accurately monitoring and detecting the freshness of food materials such as livestock, poultry and aquatic products in real time so as to ensure the quality safety of the food. The invention has the advantages of simple and easy operation, low cost and the like, but the used pH indicator belongs to artificially synthesized pigments, has certain toxicity and is not good for human health. The invention provides an improvement measure aiming at the problem, prepares an intelligent indicating film taking natural pigment as an indicator, is safe and non-toxic, and can show very obvious color change from pink, blue to dark green according to the freshness of the marine fish.
An electrospun nanofiber membrane for indicating freshness of food and a preparation method thereof are disclosed in patent No. CN 201810985483.3. The technology comprises the steps of firstly preparing the anthocyanin lipidosome by an ethanol injection method, secondly modifying chitosan on the surface of the anthocyanin lipidosome, and finally preparing the freshness indication electrospinning nanofiber membrane by utilizing an electrostatic spinning technology. The food freshness monitoring device is used for monitoring the freshness of food in the process of transporting and storing the food. The invention has the advantages of strong gas adsorption, obvious color development and the like, but has the defects of complex operation, low safety of the intelligent indicating membrane caused by using more organic solvents in the preparation process and the like.
Disclosure of Invention
In order to solve the technical problems, the invention provides a nanofiber indicating membrane for intelligently detecting the putrefaction and deterioration of marine fishes. The nanofiber indicating membrane provided by the invention is constructed by using anthocyanin and curcumin as double-color-changing agents and combining an electrostatic spinning technology, has the advantages of large specific surface, strong adsorbability and the like, and effectively improves the color development capability and stability of the indicating membrane.
The nanofiber indicating membrane for intelligently detecting the spoilage of the marine fishes comprises the following steps:
(1) sequentially adding gelatin, nano chitin, anthocyanin and curcumin into an acetic acid aqueous solution with the mass concentration of 80%, and stirring at constant temperature to prepare a spinning solution, wherein the adding amounts of the gelatin, the nano chitin and the pigment respectively account for 7.2%, 1.2% and 4% of the mass of the acetic acid aqueous solution; the mass ratio of the curcumin to the anthocyanin is 2: 8. 5: 5. 8: 2;
(2) spinning the spinning solution into a nanofiber indicating membrane by adopting an electrostatic spinning machine, wherein the receiving material is aluminum foil paper;
(3) and after spinning is finished, taking off the aluminum foil paper and cutting to obtain the nanofiber indicating membrane.
Preferably, the nano chitin in the step (1) is chitin nanofiber.
Preferably, the constant-temperature stirring in the step (1) adopts the temperature of 40-50 ℃ and the stirring time of 20-30 h.
More preferably, the constant temperature stirring in the step (1) is carried out at 42 ℃ for 24 h.
Preferably, the parameters of the electrostatic spinning machine for spinning in the step (2) are as follows:
the test temperature is 25 ℃, the relative humidity is 50%, the injection speed is 0.1mm/h, the distance from the spinning needle to the receiving device is 10cm, and the voltage is set to be 25 kv.
The invention also aims to provide an application of the nanofiber indicating film in detecting the spoilage of the seawater fish, and particularly the nanofiber indicating film is cut into a size of 1cm multiplied by 1cm, then is attached to a tray cap containing the public fish without contacting with the public fish, and the food spoilage is monitored by observing the color change of the film.
Compared with the prior art, the invention has the following beneficial effects:
the electrostatic spinning technology is characterized in that the spinning solution is stretched, refined and split by utilizing liquid drops under the action of electrostatic repulsion of a high-voltage electrostatic field, a solvent is volatilized quickly, so that a uniform nanofiber membrane can be formed, the formed fiber membrane is compact in structure, high in porosity and large in specific surface area, and compared with membranes prepared by other methods, the adsorption of the membranes on gas is good, the color change is more sensitive and accurate, and the freshness of food can be monitored in real time. The invention utilizes anthocyanin and curcumin as double-color-changing agents and combines an electrostatic spinning technology to process a nanofiber indicating membrane, thereby improving the color development effect and stability.
The nanofiber indicating film comprises chitin and gelatin. The nano chitin has high mechanical strength, can be used as a material reinforcing agent, and can also enhance the antibacterial activity of the indicating film. In addition, the nano chitin and the polyphenol have strong interaction, so that the nano chitin can be used as a fixed carrier of natural polyphenol pigment, the release rate of the natural pigment in a membrane is controlled, and the stability of the natural pigment is improved.
According to the invention, gelatin and nano chitin are mixed, strong hydrogen bonds and ionic bonds can be generated between the gelatin and the nano chitin, and the indication film can improve the barrier property and block partial O under the action of the hydrogen bonds and the ionic bonds2And CO2To enter. In addition, the chitin molecule has an amphiphilic structure, and a hydrogen bond and an ionic bond generated between the chitin molecule and the amphiphilic structure can seal a hydrophilic head group of the chitin to expose a hydrophobic tail part, so that the hydrophobic property of the indicating membrane is improved, and the water solubility is reduced.
The invention utilizes the electrostatic spinning technology to electrically spin the indicating membrane, enhances the adsorbability of the indicating membrane, uses double indicators for color development, is more sensitive to pH, has more obvious color change, and can timely monitor whether the seawater fish is deteriorated.
Drawings
FIG. 1 shows the results of the nanofiber indicating film of example 1 before and after the putrefaction of a turtle;
fig. 2 is an electron microscope image of the nanofiber indicating films prepared in example 1, example 2 and example 3, from left to right.
Detailed Description
The indicating film for intelligently monitoring food deterioration prepared by the invention is based on the following principle: the strong hydrogen bond and electrostatic interaction exist between the nano chitin and the gelatin, so that the gelatin chitin forms a more compact gel network structure, the gel strength and the gel capacity of the gelatin are further enhanced, and the mechanical property and the adsorbability of a finally formed film are improved. The anthocyanin and the curcumin are natural pigments, the addition of the natural pigments has no obvious influence on the water content, the water solubility, the air permeability and the thickness of the indicating membrane, and the two natural pigments can enhance the color reaction of the indicating membrane and are more sensitive to pH. And then, by using an electrostatic spinning technology, the spinning solution is stretched and split by liquid drops under the action of electrostatic repulsion of a high-voltage electrostatic field, so that a uniform nanofiber membrane can be formed, the membrane observed under an electron microscope has a very compact pore structure, and the special structure enables the indicating membrane to have very good adsorbability on gas. If the food changes in quality, volatile ammonia or methylamine exists in the air, and the pH of the air changes, the indicating film can react in color according to the change of the pH, so that the purpose of monitoring the food deterioration is achieved.
The present invention will be further described with reference to the following examples.
Example 1
A nanofiber indicating membrane for intelligently detecting marine fish spoilage is prepared by the following steps:
(1) sequentially adding gelatin, nano chitin, anthocyanin and curcumin into an acetic acid aqueous solution with the mass concentration of 80%, and stirring for 24 hours at the constant temperature of 42 ℃ to prepare a spinning solution, wherein the addition amounts of the gelatin and the nano chitin respectively account for 7.2% and 1.2% of the mass of the acetic acid aqueous solution; the mass ratio of the curcumin to the anthocyanin is 2: 8;
(2) spinning the spinning solution into a nanofiber indicating membrane by adopting an electrostatic spinning machine, wherein the receiving material is aluminum foil paper, and the parameters of spinning by the electrostatic spinning machine are as follows:
the testing temperature is 25 ℃, the relative humidity is 50%, the injection speed is 0.1mm/h, the distance from the spinning needle head to the receiving device is 10cm, and the voltage is set to be 25 kv;
(3) and after spinning is finished, taking off the aluminum foil paper and cutting to obtain the nanofiber indicating membrane.
Example 2
A nanofiber indicating membrane for intelligently detecting marine fish spoilage is prepared by the following steps:
(1) sequentially adding gelatin, nano chitin, anthocyanin and curcumin into an acetic acid aqueous solution with the mass concentration of 80%, and stirring for 24 hours at the constant temperature of 42 ℃ to prepare a spinning solution, wherein the adding amounts of the gelatin, the nano chitin and the pigment respectively account for 7.2%, 1.2% and 4% of the mass of the acetic acid aqueous solution; the mass ratio of the curcumin to the anthocyanin is 5: 5;
(2) spinning the spinning solution into a nanofiber indicating membrane by adopting an electrostatic spinning machine, wherein the receiving material is aluminum foil paper, and the parameters of spinning by the electrostatic spinning machine are as follows:
the testing temperature is 25 ℃, the relative humidity is 50%, the injection speed is 0.1mm/h, the distance from the spinning needle head to the receiving device is 10cm, and the voltage is set to be 25 kv;
(3) and after spinning is finished, taking off the aluminum foil paper and cutting to obtain the nanofiber indicating membrane.
Example 3
A nanofiber indicating membrane for intelligently detecting marine fish spoilage is prepared by the following steps:
(1) sequentially adding gelatin, nano chitin, anthocyanin and curcumin into an acetic acid aqueous solution with the mass concentration of 80%, and stirring for 24 hours at the constant temperature of 42 ℃ to prepare a spinning solution, wherein the adding amounts of the gelatin, the nano chitin and the pigment respectively account for 7.2%, 1.2% and 4% of the mass of the acetic acid aqueous solution; the mass ratio of the curcumin to the anthocyanin is 8: 2;
(2) spinning the spinning solution into a nanofiber indicating membrane by adopting an electrostatic spinning machine, wherein the receiving material is aluminum foil paper, and the parameters of spinning by the electrostatic spinning machine are as follows:
the testing temperature is 25 ℃, the relative humidity is 50%, the injection speed is 0.1mm/h, the distance from the spinning needle head to the receiving device is 10cm, and the voltage is set to be 25 kv;
(3) and after spinning is finished, taking off the aluminum foil paper and cutting to obtain the nanofiber indicating membrane.
Comparative example 1
A nanofiber indicating membrane for intelligently detecting marine fish spoilage is prepared by the following steps:
(1) sequentially adding gelatin, nano chitin and anthocyanin into an acetic acid aqueous solution with the mass concentration of 80%, and stirring for 24 hours at the constant temperature of 42 ℃ to prepare a spinning solution, wherein the adding amounts of the gelatin, the nano chitin and the anthocyanin respectively account for 7.2%, 1.2% and 4% of the mass of the acetic acid aqueous solution;
(2) spinning the spinning solution into a nanofiber indicating membrane by adopting an electrostatic spinning machine, wherein the receiving material is aluminum foil paper, and the parameters of spinning by the electrostatic spinning machine are as follows:
the testing temperature is 25 ℃, the relative humidity is 50%, the injection speed is 0.1mm/h, the distance from the spinning needle head to the receiving device is 10cm, and the voltage is set to be 25 kv;
(3) and after spinning is finished, taking off the aluminum foil paper and cutting to obtain the nanofiber indicating membrane.
Comparative example 2
A nanofiber indicating membrane for intelligently detecting marine fish spoilage is prepared by the following steps:
(1) sequentially adding gelatin, nano chitin and curcumin into an acetic acid aqueous solution with the mass concentration of 80%, and stirring for 24 hours at the constant temperature of 42 ℃ to obtain a spinning solution, wherein the adding amounts of the gelatin, the nano chitin and the curcumin respectively account for 7.2%, 1.2% and 4% of the mass of the acetic acid aqueous solution;
(2) spinning the spinning solution into a nanofiber indicating membrane by adopting an electrostatic spinning machine, wherein the receiving material is aluminum foil paper, and the parameters of spinning by the electrostatic spinning machine are as follows:
the testing temperature is 25 ℃, the relative humidity is 50%, the injection speed is 0.1mm/h, the distance from the spinning needle head to the receiving device is 10cm, and the voltage is set to be 25 kv;
(3) and after spinning is finished, taking off the aluminum foil paper and cutting to obtain the nanofiber indicating membrane.
The nanofiber indicating films prepared in examples 1 to 3 and comparative examples 1 to 2 were cut into a size of 1cm x 1cm, and then attached to a tray cap containing a kombu without contacting the fish, thereby monitoring the deterioration of foods by observing the color change of the films.
The nanofiber indicating film prepared in comparative example 1 has a good indicating ability but is poor in stability.
The nanofiber indicating membrane prepared in comparative example 2 has good stability but poor indicating capability, and cannot timely and accurately indicate the quality change of the marine fish.
The nanofiber indicating films prepared in examples 1-3 have obvious color change reaction and high stability. As shown in fig. 1.
Very dense network structures can be observed in the scanning electron microscope of the films produced by examples 1 to 3 of FIG. 2 (where A is1Film from example 1, A2Film from example 2, A3The film made in example 3).
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A nanofiber indicating membrane for intelligently detecting marine fish spoilage is characterized by comprising the following steps:
(1) sequentially adding gelatin, nano chitin, anthocyanin and curcumin into an acetic acid aqueous solution with the mass concentration of 80%, and stirring at constant temperature to prepare a spinning solution, wherein the adding amounts of the gelatin, the nano chitin and the pigment respectively account for 7.2%, 1.2% and 4% of the mass of the acetic acid aqueous solution; the mass ratio of the curcumin to the anthocyanin is 2: 8. 5: 5. 8: 2;
(2) spinning the spinning solution into a nanofiber indicating membrane by adopting an electrostatic spinning machine, wherein the receiving material is aluminum foil paper;
(3) and after spinning is finished, taking off the aluminum foil paper and cutting to obtain the nanofiber indicating membrane.
2. The nanofiber indicator film for intelligently detecting marine fish spoilage according to claim 1, wherein the nano chitin is chitin nanofiber.
3. The nanofiber indicating membrane for intelligently detecting marine fish spoilage according to claim 1, wherein constant-temperature stirring in the step (1) is carried out at a temperature of 40-50 ℃ for 20-30 h.
4. The nanofiber indicating membrane for intelligently detecting marine fish spoilage according to claim 3, wherein the constant-temperature stirring in the step (1) is carried out at 42 ℃ for 24 hours.
5. The nanofiber indicating membrane for intelligently detecting marine fish spoilage according to claim 1, wherein parameters of spinning performed by an electrostatic spinning machine in the step (2) are as follows:
the test temperature is 25 ℃, the relative humidity is 50%, the injection speed is 0.1mm/h, the distance from the spinning needle to the receiving device is 10cm, and the voltage is set to be 25 kv.
6. Use of a nanofiber indicator film for detecting spoilage of marine fishes, wherein the nanofiber indicator film of any one of claims 1-5 is cut into a size of 1cm x 1cm, and then is attached to a tray cap containing a pacifier without contacting the pacifier, and the food spoilage is monitored by observing the color change of the film.
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