CN115418032A - Preparation method of Carr/BIL membrane - Google Patents
Preparation method of Carr/BIL membrane Download PDFInfo
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- CN115418032A CN115418032A CN202211147504.7A CN202211147504A CN115418032A CN 115418032 A CN115418032 A CN 115418032A CN 202211147504 A CN202211147504 A CN 202211147504A CN 115418032 A CN115418032 A CN 115418032A
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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
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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
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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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
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
- C08K5/3415—Five-membered rings
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- 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
Abstract
A preparation method of Carr/BIL film is an active intelligent food packaging material which takes natural polymer as a substrate and takes pH sensitive dye as a response signal. In the present invention, a color indicating film having oxidation resistance and amine responsiveness was developed by adding Bilirubin (BIL) to a kappa-carrageenan (Carr) matrix. The result shows that the Carr/BIL composite membrane has good DPPH/ABTS free radical scavenging capacity, and can effectively delay the oxidative deterioration of the shrimps in the storage process, thereby playing a role in keeping the packaged shrimps fresh. In addition, the composite membrane shows sensitive color response to ammonia with different concentrations, and quick visual judgment on the freshness of the packaged shrimps is realized through the change of b value.
Description
Technical Field
The invention belongs to the technical field of membrane materials, and relates to a preparation method of a Carr/BIL membrane.
Background
In recent years, "white pollution" caused by non-degradability of synthetic polymer-based food packaging films has become an environmental problem to be solved. The development of environment-friendly packaging materials, such as polysaccharide, starch and protein, by utilizing natural biodegradable polymers is a research trend of the packaging materials. Among various natural biopolymers, kappa-carrageenan (Carr) extracted from red seaweed has excellent gel-forming properties, and has become a biodegradable film-forming substrate commonly used in food packaging. However, pure Carr films with a single function have difficulty meeting consumer demand for monitoring food freshness, limiting their further use in food packaging.
Bilirubin (BIL) is a yellow-red tetrapyrrole pigment that has long been recognized as a waste product of hemoglobin catabolism in red blood cells. However, there is increasing evidence that BIL has good antioxidant activity, helping to protect lipids from oxidation and against oxidative stress. In addition, BIL is sensitive to alkalinity, is insoluble in water, but has good solubility under alkaline conditions. This property can be used for the detection of biogenic amines in spoiled foods. Thus, BIL has the potential to serve as a response factor for the activity and intelligence of packaging materials.
Disclosure of Invention
The invention aims to provide a preparation method of Carr/BIL membrane.
In order to achieve the above objects and other related objects, the present invention provides the following technical solutions: a preparation method of Carr/BIL membrane comprises dispersing glycerol in water, stirring to obtain dispersion, adding Carr (kappa-carrageenan) into the dispersion, stirring, mixing to obtain Carr solution; then adding BIL (bilirubin) suspension into Carr solution, and stirring and mixing uniformly to obtain a film forming solution; finally, spreading the film-forming solution on a bearing plate for drying; and storing the dried sample in a constant temperature and humidity cabinet for 40-60h, wherein the obtained film is a Carr/BIL film.
The preferable technical scheme is as follows: carr is reagent grade, purity of BIL is greater than or equal to 98%, and purity of glycerol is greater than or equal to 99%.
The preferable technical scheme is as follows: carr, ratio of glycerol to water: 1.5-1.7g:0.8-1.1g:55mL.
The preferable technical scheme is as follows: the BIL suspension was added to the Carr solution at a ratio of 0.0025-0.0125% (w/v).
The preferable technical scheme is as follows: the bilirubin suspension was added to the Carr solution at a rate of 0.0075% (w/v).
Due to the application of the technical scheme, compared with the prior art, the invention has the advantages that:
1. the invention uses an anti-oxidation and amine response color indication film based on Carr and BIL as an intelligent packaging film for detection, the detection result is basically consistent with the result of a standard volatile basic nitrogen detection method, the color change is easy to be recognized by naked eyes, and the detection process is economic, efficient, rapid and convenient.
2. The addition of BIL obviously improves the antioxidant activity of the film, delays the oxidative deterioration of food and achieves the aim of fresh-keeping.
3. The Carr/BIL film can be used as an intelligent packaging film to simply and accurately monitor the freshness of shrimps. Can be applied to aquatic products supply chain to the new freshness of real-time visual monitoring. It is also expected that a smartphone will be used to capture the tag and assess freshness through more accurate color analysis.
Drawings
FIG. 1 shows (a) DPPH radical scavenging activity and (b) ABTS radical scavenging activity of Carr/BIL membranes. Different letters (a-f) represent significant differences (p < 0.05).
FIG. 2 is a graph of the color response of Carr/BIL membranes to different concentrations of ammonia.
FIG. 3 shows (a) Carr/BIL 0 Membranes and Carr/BIL 0.0075 The color response of the freshness of the prawn under different storage temperature conditions. (b) Carr/BIL 0.0075 B value of the film. (c) the corresponding TVB-N value.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Referring to fig. 1-3, it should be understood that the structures, ratios, sizes, and the like shown in the drawings are only used for understanding and reading the disclosure of the specification, and are not used to limit the practical conditions of the present invention, so they have no technical significance, the following examples are provided for better understanding of the present invention, and are not intended to limit the present invention.
Example 1: preparation method of Carr/BIL film
The utility model provides an anti-oxidation and amine response color indication membrane based on Carr and BIL, includes and uses Carr as the base material, uses BIL as the color indicator, disperses BIL suspension in the Carr matrix, forms anti-oxidation and amine response color indication membrane, the color indicator be the BIL of yellowish red, the Carr membrane by Carr, pure water and glycerine, prepare through the curtain coating method.
Specifically, the preparation method of the anti-oxidation and amine response color indication membrane comprises the steps of dispersing a suspension of BIL into Carr solution, casting the membrane forming solution into a culture dish, drying, and placing in a constant temperature and humidity incubator for two days.
Specifically, the preparation method of the Carr film comprises the following steps:
dispersing glycerol in the water solution, magnetically stirring, adding Carr, continuously stirring, pouring the film-forming solution into a culture dish, drying, and storing in a constant-temperature constant-humidity incubator.
Specifically, the proportion of the BIL suspension added is as follows: 0%, 0.0025%, 0.005%, 0.0075%, 0.01% and 0.0125%.
Specifically, the amount of Carr added was 1.62g, the volume of pure water was 55mL, the weight of glycerol was 0.96g, and the reaction temperature was 90 ℃.
A process for preparing the antioxidizing and amine-responding color indicating membrane based on Carr and BIL includes dispersing the suspension of BIL in the aqueous solution of Carr, casting the filming liquid in culture dish, drying, and culturing in constant-temp and-humidity incubator for two days.
The optimal addition proportion of BIL is 0.0075%, and the BIL has good antioxidant activity.
BIL is sensitive to alkalinity, is insoluble in water, but has good solubility under alkaline conditions. This property can be used for the detection of biogenic amines in spoiled foods. In daylight, the film containing BIL appears pink to the pigment itself. When biogenic amines are present, the color gradually changes to reflect food freshness.
Table 1 summarizes the color parameters of Carr/BIL films. As the amount of BIL added increased, the L value of Carr/BIL film gradually decreased, while the a, b and Δ E values increased significantly (p < 0.05). This is consistent with the change in the macroscopic photograph of the film, indicating that the BIL content has a greater effect on the color properties of the Carr/BIL film.
TABLE 1 color parameters of Carr/BIL films
In the embodiment, ammonia water is used as model biogenic amine to study the capability of the prepared antioxidant colorimetric film for detecting biogenic amine. Namely, discloses the application of an antioxidant and amine response color indicating film based on Carr and BIL in the detection of biogenic amine.
First, a series of ammonia solutions of known concentration were prepared by diluting commercially available aqueous ammonia with deionized water. Thereafter, the ammonia solution was added to a 24-well plate (1 mL per well), and the prepared film was immediately placed on top of the 24-well plate. Color changes were recorded with a camera and a colorimeter.
As shown in fig. 2, the color of the five membranes gradually changed from pink to yellow as the ammonia concentration increased. When BIL was added in an amount of 0.0075%, the color reaction of Carr/BIL film to ammonia was most easily recognized by naked eyes. In order to reflect the change of color more accurately, a colorimeter is usedColor parameters of Carr/BIL films were measured. As shown in tables 2-5, the b values of Carr/BIL films are closely related to the ammonia concentration. b significantly increases with increasing ammonia concentration (p)<0.05 Indicating that the film color became more yellow. This is consistent with the color change observed with the naked eye. The Δ Ε value represents the change in color compared to the original color. The Δ E values in Table 5 reflect Carr/BIL 0.0025～0.0125 The responsiveness of the membrane to ammonia. After a combination of macroscopic color changes and color parameter changes, carr/BIL was selected 0.0075 The membrane is used for monitoring biogenic amine of aquatic products.
TABLE 2 change in L values of Carr/BIL membranes reacted with different concentrations of ammonia
TABLE 3 a change of values of Carr/BIL membranes with different concentrations of ammonia
TABLE 4 variation in b of Carr/BIL membranes reacted with different concentrations of ammonia
TABLE 5. Delta. E change in Carr/BIL membranes reacted with different concentrations of ammonia
The antioxidant capacity of the Carr/BIL antioxidant intelligent food packaging film is also analyzed, and the antioxidant activity of the Carr/BIL antioxidant intelligent food packaging film is evaluated through DPPH and ABTS free radical scavenging capacity. As in a and 1 of FIG. 1b is shown in Carr/BIL 0.0025～0.0125 The antioxidant activity of the membrane is obviously higher than that of Carr/BIL 0 Film (p)<0.05). In addition, carr/BIL membranes were BIL dose-dependent on DPPH and ABTS clearance activity. Carr/BIL when BIL was added at a level of 0.0125% 0.0125 The DPPH and ABTS free radical scavenging activity of the membrane is respectively improved to Carr/BIL 0 2.4 times and 5.6 times of the membrane. Therefore, the introduction of BIL obviously improves the antioxidant activity of Carr/BIL film, thereby delaying the oxidative deterioration of food and achieving the purpose of prolonging the shelf life.
This example shows the actual detection of biogenic amines produced by Carr/BIL antioxidant smart food packaging films during shrimp storage. The detection of the biogenic amine is carried out by taking commercial fresh shrimps as real samples. The Carr/BIL antioxidant intelligent food packaging film is prepared by the preparation method of the example 1, and the two materials are in the optimal proportion.
First, fresh shrimps were wrapped with Carr/BIL antioxidant smart food packaging films, and then placed at different temperatures (-20 deg.C, 4 deg.C, and 25 deg.C) for 1-5 days. With Carr/BIL 0 As a control group. During this time, the color change of the Carr/BIL film in daylight was recorded by a camera to analyze the freshness of the sample. In addition, total volatile basic nitrogen (TVB-N) in the shrimp meat samples was determined using a fully automated kjeldahl azotometer, all measurements were repeated three times, and the results are shown in fig. 3 c.
In a of FIG. 3, 25 ℃ to 0day means that the shrimp are stored at 25 ℃ for 0day, i.e., the sample in the initial state, 25 ℃ to 1day means that the shrimp are stored at 25 ℃ for 1day, and the rest is analogized.
As shown in a of FIG. 3, carr/BIL 0 The film lacks amine sensitivity and no color change occurs during storage at 25 ℃. In contrast, carr/BIL 0.0075 The film showed a clear color difference from pink to orange during storage. It can be seen that under daylight illumination, light pink represents freshness, dark pink represents deterioration, and orange represents severe deterioration. After being stored for 1day at 25 ℃, the original pink color of the Carr/BIL antioxidant intelligent food packaging film is changed into yellow, which indicates that the shrimps are deteriorated. The color of the film is not obviously changed when the shrimps are stored for 3 days at 4 ℃, which indicates that the shrimps are still fresh,can be eaten. However, when the shrimp were stored for 5 days, the color of the film turned yellow, indicating that the shrimp had deteriorated. However, when the shrimp were stored at-20 ℃ for 5 days, there was little apparent change in the surface color of the Carr/BIL antioxidant smart food packaging film, indicating that the shrimp were still fresh. The change in colour was observed with the naked eye and is well reflected by the b values in b of figure 3 (from 7.5 to 12.3).
And comparing the detection result of the Carr/BIL antioxidant intelligent food packaging film with the detection result of the standard TVB-N method to verify the detection accuracy. According to the standard, when the TVB-N content is less than 120mg/100g, the raw shrimp are fresh. When the TVB-N content is in the range of 12-25mg/100g, the shrimp are already slightly decomposed, but still edible. When the TVB-N content exceeds 25mg/100g, the shrimp deteriorate and are inedible.
Accordingly, the TVB-N level of the shrimp significantly increased from 4.7mg/100g (fresh) to 481mg/100g (c of FIG. 3), indicating that the shrimp had severely deteriorated. Furthermore, it is worth mentioning that Carr/BIL 0.0075 The TVB-N content of the prawn subjected to membrane treatment for 5 days is obviously lower than that of Carr/BIL 0 Film treatment (p)<0.05 Indicating that the antioxidant capacity of the membrane can delay the deterioration of seafood. The film, which was stored at 4 ℃ for 5 days, had a slightly darker yellowness, increasing the b value to 9.2, which is consistent with a slight increase in the TVB-N value. After 5 days at-20 ℃, the color of the film did not change significantly, with a b value of about 8.3, which corresponds to a weaker change in TVB-N. The above data indicate that Carr/BIL was prepared 0.0075 The membrane has antioxidant activity, and can delay oxidative deterioration of marine products. In addition, the film can also be used as a smart label to monitor the quality of aquatic products.
The above experimental results show that the color change of the Carr/BIL antioxidant intelligent food packaging film is consistent with the result of the standard TVB-N method. Therefore, the Carr/BIL antioxidant intelligent food packaging film can simply and accurately monitor the freshness of shrimps. With this functionality, the intelligent package can be easily applied to the seafood supply chain to enable real-time and visual monitoring of freshness. In the future, it is also expected to use smartphones to capture tags and assess freshness through more accurate color analysis.
Example 2: preparation method of Carr/BIL film
A preparation method and application of Carr/BIL membrane, disperse glycerin into water, after stiring, pour Carr into above-mentioned dispersion, stir and mix, get Carr solution; then adding the BIL suspension into Carr solution, and uniformly stirring and mixing to obtain a film forming solution; finally, spreading the film-forming solution on a bearing plate for drying; the dried sample is stored in a constant temperature and humidity box for 40 hours, and the obtained film is a Carr/BIL film.
The preferred embodiment is: carr is reagent grade, purity of BIL is greater than or equal to 98%, and purity of glycerol is greater than or equal to 99%.
The preferred embodiment is: carr, ratio of glycerol to water: 1.5g:0.8g:55mL.
The preferred embodiment is: the BIL suspension was added to the Carr solution at a ratio of 0.0025% (w/v). I.e. a concentration of BIL of 0.0025% (w/v).
Example 3: preparation method of Carr/BIL membrane
A preparation method and application of Carr/BIL membrane, disperse glycerin into water, after stiring, pour Carr into above-mentioned dispersion, stir and mix, get Carr solution; then adding the BIL suspension into the Carr solution, and stirring and mixing uniformly to obtain a film forming solution; finally, spreading the film-forming solution on a bearing plate for drying; the dried sample is stored for 60h in a constant temperature and humidity cabinet, and the obtained film is a Carr/BIL film.
The preferred embodiment is: carr is reagent grade, purity of BIL is greater than or equal to 98%, and purity of glycerol is greater than or equal to 99%.
The preferred embodiment is: carr, ratio of glycerol to water: 1.7g:1.1g:55mL.
The preferred embodiment is: the BIL suspension was added to the Carr solution at a ratio of 0.0125% (w/v). I.e. a concentration of BIL of 0.0125% (w/v).
The foregoing is illustrative of the preferred embodiment of the present invention and is not to be construed as limiting thereof in any way, and any modifications or variations thereof that fall within the spirit of the invention are intended to be included within the scope thereof.
Claims (5)
1. A preparation method of Carr/BIL membrane is characterized by comprising the following steps: dispersing glycerol into water, uniformly stirring to obtain a dispersion liquid, pouring Carr into the dispersion liquid, and uniformly stirring, mixing and uniformly mixing to obtain a Carr solution; then adding the BIL suspension into Carr solution, and uniformly stirring and mixing to obtain a film forming solution; finally, spreading the film-forming solution on a bearing plate for drying; the dried sample is stored in a constant temperature and humidity cabinet for 40-60h, and the obtained film is Carr/BIL film.
2. The preparation method and application of Carr/BIL film as claimed in claim 1, wherein: carr is reagent grade, purity of BIL is greater than or equal to 98%, and purity of glycerol is greater than or equal to 99%.
3. The method of producing Carr/BIL film according to claim 1, wherein: carr, ratio of glycerol to water: 1.5-1.7g:0.8-1.1g:55 And (mL).
4. The method of producing Carr/BIL film according to claim 1, wherein: the BIL suspension was added to the Carr solution at a ratio of 0.0025-0.0125% (w/v).
5. The method of producing Carr/BIL film according to claim 1, wherein: the BIL suspension was added to the Carr solution at a ratio of 0.0075% (w/v).
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