CN111471307A - Preparation method of degradable collagen packaging material - Google Patents
Preparation method of degradable collagen packaging material Download PDFInfo
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- CN111471307A CN111471307A CN202010195419.2A CN202010195419A CN111471307A CN 111471307 A CN111471307 A CN 111471307A CN 202010195419 A CN202010195419 A CN 202010195419A CN 111471307 A CN111471307 A CN 111471307A
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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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/78—Connective tissue peptides, e.g. collagen, elastin, laminin, fibronectin, vitronectin, cold insoluble globulin [CIG]
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
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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
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
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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
- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/02—Starch; Degradation products thereof, e.g. dextrin
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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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
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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
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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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- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
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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
The invention discloses a preparation method of an easily degradable packaging material of a fish scale collagen matrix, belonging to the technical field of food packaging and processing. The material is prepared by taking fish scale collagen prepared by extracting collagen from freshwater fish scales as a matrix and adding wheat starch, a pomegranate flower extract, essential oil, glycerol and sodium alginate. The invention can reduce the environmental pollution caused by waste fish scales and improve the high-value utilization of the fish scales. The invention has simple process, and the prepared packaging material has higher tensile strength, excellent toughness and plasticity, better antibacterial and antioxidant effects, is degradable in natural environment and has no pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of food packaging and processing, and particularly relates to a method for preparing an easily degradable food packaging material of a fish scale collagen matrix with good mechanical properties and excellent antibacterial and antioxidant properties.
Background
Compared with the environmental pollution problem caused by non-degradable food packaging materials, the degradable food packaging materials are receiving wide attention. The packaging material taking protein as a matrix has good plasticity and biocompatibility, but has the defects of low mechanical strength, poor water resistance, weak antibacterial activity and the like. Therefore, the packaging material with protein matrix usually needs to be added with other base materials, plasticizers, bacteriostats and the like to improve the mechanical properties and improve the oxidation resistance and bacteriostasis performance of the material.
The fish scale collagen is a good source of protein packaging materials, and researches show that the edible film prepared by taking the fish phosphorus collagen as the base material has better air permeability and certain mechanical property, and is applied to the research of food preservation as a potential plastic film substitute. The fish scale collagen is produced by using the fish scales, so that the environmental pollution is reduced, and the high-valued utilization value of the fish scales can be improved. However, the fish scale collagen packaging material still has the problems of poor antibacterial activity, low oxidation resistance and the like, so that the structure of the material is improved by adding the pomegranate flower extract, the essential oil and the like, the generation of a collagen gel network is promoted, and the material and the wheat starch substrate form a composite packaging material with good mechanical property, so that the antibacterial and fresh-keeping capacity of the material is improved. The glycerol and the sodium alginate can enter protein molecules to further improve the forming performance, the mechanical performance and the surface performance of the material. Therefore, the easily degradable food packaging material of the fish scale collagen matrix has wide development and application prospects from the aspects of technical effects, market requirements, environmental protection, economy and the like.
Disclosure of Invention
The invention provides a preparation method of a fish scale collagen matrix easily-degradable food packaging material, aiming at solving the problem of environmental pollution caused by difficulty in degradation of plastic serving as a packaging material and improving the utilization rate of fish scales of freshwater fish.
The fish scale collagen matrix food packaging material comprises the following components in parts by weight: 10-20 parts of freshwater fish scale collagen, 0.4-4 parts of wheat starch, 0.1-2 parts of pomegranate flower extract coarse powder, 0.1-1 part of essential oil, 0.2-1 part of glycerol, 0.1-1 part of sodium alginate and 500 parts of deionized water.
Further taking the collagen of the scale of the freshwater fish prepared from the collagen extracted from the scale of the freshwater fish as a base material, adding wheat starch and the pomegranate flower extract powder extracted from the pomegranate flower, and then adding essential oil, glycerol and sodium alginate.
The preparation method of the easily degradable food packaging material of the fish scale collagen matrix comprises the following steps: (1) extracting scale collagen powder of freshwater fish:
① pretreating fish scales by cleaning and decalcifying fresh water fish scales;
② extracting collagen, namely washing the pretreated fish scales, freeze-drying, regulating the pH to 1.5 by using 1M hydrochloric acid according to the feed-liquid ratio of 1:25g/ml and the addition of pepsin of 4%, performing ultrasonic treatment at the ultrasonic power of 350W for 30min, leaching at 25 ℃ for 4h, and performing suction filtration to obtain a fish scale collagen solution;
③ concentrating the fish scale collagen protein solution to 10-15% of the original volume by a rotary evaporator.
④ freeze drying, namely, using a freeze dryer to dry, pre-freezing the fish scale protein powder for 24 hours at the temperature of minus 80 ℃, setting all parameters of the freeze dryer as initial temperature of minus 60 ℃, then starting vacuumizing after 4 hours, increasing the temperature at 5 ℃/h until the temperature rises to 30 ℃, and keeping the temperature at the temperature for 4 hours to obtain the fish scale protein powder.
(3) Preparation of pomegranate flower extract:
① pretreating by washing fresh flos Granati with deionized water for 3 times, oven drying at 35 deg.C, and pulverizing into flos Granati powder;
② dynamic high-pressure microjet treatment, mixing flos Granati powder with 70% ethanol at a mass-volume ratio of 1:10-15, treating with high-pressure homogenizer at 40Mpa for 2 times (each time for 15-30 s), and dynamic high-pressure microjet for 2 times, ③ hot water extracting with water bath heating method at 65 deg.C for 1-2 hr to obtain flos Granati extract solution;
④ centrifuging, and centrifuging to obtain supernatant.
⑤ concentrating, concentrating the centrifuged flos Granati extract solution to 5-10% of the original volume by rotary evaporator;
⑥ freeze drying, namely, pre-freezing the pomegranate flower extract for 24h at-80 ℃, setting the parameters of the freeze dryer as initial temperature-60 ℃, starting to vacuumize after 4h, increasing the temperature at 5 ℃/h until the temperature rises to 30 ℃, and keeping the temperature constant for 4h at the temperature to obtain coarse powder of the pomegranate flower extract;
(3) preparing materials: respectively weighing 10-20 parts of freshwater fish scale collagen, 0.4-4 parts of wheat starch, 0.1-2 parts of coarse powder of a pomegranate flower extract, 0.1-1 part of essential oil, 0.2-1 part of glycerol, 0.1-1 part of sodium alginate and 500 parts of deionized water.
(4) Compounding: dissolving freshwater fish scale collagen and wheat starch in deionized water, stirring at 50-60 deg.C for 5-10min in a magnetic stirrer, and adding flos Granati extract coarse powder, essential oil, glycerol, and sodium alginate to obtain mixed solution. Treating the mixed solution for 2 times at 40MPa of a high-pressure homogenizer for 15-30s each time, treating the mixed solution for 2 times at 30-60MPa by dynamic high-pressure microjet, then carrying out water bath in a magnetic water bath kettle for 20-40min at the rotation speed of 600-1000rpm/min and the temperature of 55-65 ℃, and then filtering out bubbles by using a vacuum pump to obtain a forming solution;
(5) and (3) film forming, namely pouring 50-100m of L forming liquid into a die with the thickness of 15 × 10 × 5cm for hot press forming, taking out, cooling and cutting edges to obtain the fish scale gelatin protein packaging material.
Further, in the step (1), the scale of the freshwater fish is selected from one or a mixture of grass carp, black carp, silver carp, bighead carp, carp and crucian carp.
Further, the fish scale pretreatment in the step (1) is specifically that fresh freshwater fish scales are soaked in deionized water, washed for 3 times, drained, added with 10% citric acid with a solid-to-liquid ratio of 1:20-25(g/m L), treated on a magnetic stirrer for 50-80min at a rotation speed of 800-.
Further, in the step (2) ②, the dynamic high-pressure microjet pressure is 120 Mpa.
Further, the rotation speed of the centrifugal machine during the centrifugation in the step (2) ④ is 5000rpm/min, the temperature is-4 ℃, and the time is 15-20 min.
Further, in the step (3), the essential oil is one or a mixture of more of clove, tea tree, chrysanthemum, lemon, grapefruit and sweet orange essential oil.
Further, the dynamic high-pressure microjet pressure in the step (4) is 30-60 Mpa.
The tensile strength of the fish scale collagen food packaging material is 12.34-21.15 MPa; the elongation at break is 21.43-38.10%.
The key points of the invention are as follows: mixing freshwater fish scale collagen with wheat starch, pomegranate flower extract and essential oil in proportion, and adding glycerol and sodium alginate for improving mechanical property and surface property to prepare the packaging material with antibacterial property, antioxidant property and good mechanical property. Blending wheat starch, essential oil and pomegranate flower extract causes the intermolecular acting force (such as hydrogen bonds, disulfide bonds and the like) and conformation (such as the increase of an ordered structure) of the collagen to be changed, thereby changing the mechanical property and the barrier property of the collagen matrix material. By comparing evaluation indexes such as color, texture, TVB-N value, TBARs value and colony count of the cold fresh fish, the fish scale collagen matrix material can effectively prolong the retention time of color, toughness and hardness of the fish, delay the increase of the TVB-N value and the TBARs value and inhibit the total number of bacteria, thereby prolonging the shelf life of the cold fresh fish, and thus proving that the fish scale collagen matrix packaging material has good oxidation resistance and antibacterial performance.
The invention has the advantages that:
(1) the fish scale collagen matrix packaging material prepared by the invention is a biological material, can be completely degraded and has no pollution to the environment.
(2) The pomegranate flower extract and the essential oil contained in the fish scale collagen matrix packaging material prepared by the invention can effectively prolong the retention time of color, toughness and hardness of fish products; the antioxidant has antioxidant capacity, and can delay the increase of TVB-N value and TBARs value of meat products; has good antibacterial ability, and can effectively inhibit the growth and reproduction of microorganisms in food and prolong the shelf life of food.
(3) The fish scale collagen matrix packaging material prepared by the invention has better plasticity and barrier property.
(4) The preparation method disclosed by the invention is simple in preparation process, simple and convenient to operate, has a good development prospect, and has important significance for protecting the environment and improving the high-value utilization of the fish scales.
Detailed Description
Example 1
The present invention will be further described with reference to specific embodiments.
The preparation method of the fish scale collagen matrix degradable packaging material comprises the following steps:
(1) extracting scale protein of freshwater fish:
① preprocessing fish scale, washing 200g of fresh water fish scale with deionized water for 3 times, draining, adding 10% citric acid with a solid-to-liquid ratio of 1:20(g/m L), processing on a magnetic stirrer for 60min at a rotation speed of 800rpm/min, washing with deionized water for 3 times, and freeze-drying to obtain decalcified fish scale.
② extracting collagen, weighing 150g of decalcified fish scales, regulating the material-liquid ratio to be 1:25g/M L and the addition amount of pepsin to be 4%, regulating the pH to be 1.5 by using 1M hydrochloric acid, performing ultrasonic treatment at the ultrasonic power of 350W for 30min, leaching at the temperature of 25 ℃ for 4h, and performing suction filtration to obtain the fish scale collagen solution.
③ concentrating, concentrating the fish scale collagen protein solution by a rotary evaporator at 60 deg.C to obtain 10% protein concentrate.
④ freeze drying, namely, using a freeze dryer to dry, pre-freezing the fish scale collagen powder for 24 hours at the temperature of minus 80 ℃, setting all parameters of the freeze dryer as initial temperature of minus 60 ℃, then starting vacuumizing after 4 hours, increasing the temperature at 5 ℃/h until the temperature rises to 30 ℃, and keeping the temperature at the temperature for 4 hours to obtain the fish scale collagen powder.
(2) Preparation of pomegranate flower extract:
① pretreating by washing fresh flos Granati with deionized water for 3 times, oven drying at 35 deg.C, and pulverizing into flos Granati powder;
② dynamic high-pressure microjet treatment, mixing flos Granati powder with 70% ethanol at a mass-volume ratio of 1:10, treating with high-pressure homogenizer at 40Mpa for 2 times (20 s each time), and treating with dynamic high-pressure microjet at 120Mpa for 2 times.
③ hot water extraction, wherein the hot water extraction is carried out by heating in water bath at 65 deg.C for 1.5h to obtain flos Granati extract solution;
④ centrifuging at 5000rpm/min and-4 deg.C for 15min to obtain supernatant, and concentrating ⑤ by concentrating the centrifuged flos Granati extract solution with rotary evaporator at 50 deg.C to 5% of the original volume;
⑥ freeze drying, namely, pre-freezing the pomegranate flower extract for 24h at-80 ℃, setting the parameters of the freeze dryer as initial temperature-60 ℃, starting to vacuumize after 6h, increasing the temperature at 5 ℃/h until the temperature rises to 30 ℃, and keeping the temperature constant for 4h at the temperature to obtain coarse powder of the pomegranate flower extract;
(3) weighing 5g of freshwater fish scale collagen, 1.4g of wheat starch, 0.8g of coarse powder of pomegranate flower extract, 0.2g of clove essential oil, 0.8g of glycerol, 0.4g of sodium alginate and 200m L of deionized water.
(4) Dissolving freshwater fish scale collagen and wheat starch in 200m L deionized water, stirring for 5min at 55 ℃ on a magnetic stirrer at the rotation speed of 800rpm/min, continuously adding 0.8g coarse powder of the pomegranate flower extract, 0.2g essential oil, 0.8g glycerol and 0.4g sodium alginate to obtain a mixed solution, treating the mixed solution for 2 times at 40MPa of a high-pressure homogenizer for 20s each time, treating the mixed solution for 2 times at 40MPa by dynamic high-pressure microjet, then bathing the treated mixed solution in a magnetic water bath kettle for 20min at the rotation speed of 800rpm/min and the temperature of 55 ℃, and then filtering out bubbles by using a vacuum pump to obtain a molding solution;
(5) and (3) molding, namely pouring 50m of L molding liquid into a mold of 15 × 10 × 5cm for hot press molding, taking out, cooling and cutting edges to obtain the fish scale gelatin protein packaging material.
The test shows that the tensile strength of the packaging material is 15.75MPa, the elongation at break is 26.84 percent, the light transmittance is 43.85 percent, and the water vapor transmission rate is 0.76 g.Pa-1·s-1·m-1×10-10。
Example 2
This example differs from example 1 in that: the ingredients are not added with three substances of wheat starch, pomegranate flower extract and clove essential oil, and the rest is the same as the example 1.
The method specifically comprises the following steps:
(1) extracting scale protein of freshwater fish:
① preprocessing fish scale, washing 200g of fresh water fish scale with deionized water for 3 times, draining, adding 10% citric acid with a solid-to-liquid ratio of 1:20(g/m L), processing on a magnetic stirrer for 60min at a rotation speed of 800rpm/min, washing with deionized water for 3 times, and freeze-drying to obtain decalcified fish scale.
② extracting collagen, weighing 150g of decalcified fish scales, adjusting the material-liquid ratio to 1:25g/ml, adding 4% of pepsin, adjusting the pH to 1.5 with 1M hydrochloric acid, performing ultrasonic treatment at the ultrasonic power of 350W for 30min, leaching at 25 ℃ for 4h, and performing suction filtration to obtain the fish scale collagen solution.
③ concentrating, concentrating the fish scale collagen protein solution by a rotary evaporator at 60 deg.C to obtain 10% protein concentrate.
④ freeze drying, namely, using a freeze dryer to dry, pre-freezing the fish scale collagen powder for 24 hours at the temperature of minus 80 ℃, setting all parameters of the freeze dryer as initial temperature of minus 60 ℃, then starting vacuumizing after 4 hours, increasing the temperature at 5 ℃/h until the temperature rises to 30 ℃, and keeping the temperature at the temperature for 4 hours to obtain the fish scale collagen powder.
(2) The ingredients are 5g of freshwater fish scale collagen, 0.8g of glycerol, 0.4g of sodium alginate and 200m L of deionized water.
(3) Dissolving freshwater fish scale collagen and wheat starch in 200m L deionized water, stirring for 5min at 55 ℃ on a magnetic stirrer at the rotation speed of 800rpm/min, adding 0.8g of glycerol and 0.4g of sodium alginate to obtain a mixed solution, treating the mixed solution for 2 times at 40MPa of a high-pressure homogenizer for 20s each time, treating for 2 times at 40MPa by dynamic high-pressure microjet, then carrying out water bath for 20min in a magnetic water bath kettle at the rotation speed of 800rpm/min and the temperature of 55 ℃, and then filtering out bubbles by using a vacuum pump to obtain a molding solution;
(4) and (3) molding, namely pouring 50m of L molding liquid into a mold of 15 × 10 × 5cm for hot press molding, taking out, cooling and cutting edges to obtain the fish scale gelatin protein packaging material.
Example 3
This example differs from example 1 in that: only fish scale collagen is adopted to directly prepare the packaging material.
The method specifically comprises the following steps:
(1) extracting scale protein of freshwater fish:
① preprocessing fish scale, washing 200g of fresh water fish scale with deionized water for 3 times, draining, adding 10% citric acid with a solid-to-liquid ratio of 1:20(g/m L), processing on a magnetic stirrer for 60min at a rotation speed of 800rpm/min, washing with deionized water for 3 times, and freeze-drying to obtain decalcified fish scale.
② extracting collagen, weighing 150g of decalcified fish scales, adjusting the material-liquid ratio to 1:25g/ml, adding 4% of pepsin, adjusting the pH to 1.5 with 1M hydrochloric acid, performing ultrasonic treatment at the ultrasonic power of 350W for 30min, leaching at 25 ℃ for 4h, and performing suction filtration to obtain the fish scale collagen solution.
③ concentrating, concentrating the fish scale collagen protein solution by a rotary evaporator at 60 deg.C to obtain 10% protein concentrate.
④ freeze drying, namely, using a freeze dryer to dry, pre-freezing the fish scale collagen powder for 24 hours at the temperature of minus 80 ℃, setting all parameters of the freeze dryer as initial temperature of minus 60 ℃, then starting vacuumizing after 4 hours, increasing the temperature at 5 ℃/h until the temperature rises to 30 ℃, and keeping the temperature at the temperature for 4 hours to obtain the fish scale collagen powder.
(2) Dissolving freshwater fish scale collagen and wheat starch in 200m L deionized water, stirring for 5min at 55 ℃ on a magnetic stirrer at the rotating speed of 800rpm/min, treating the mixed solution for 2 times at 40Mpa of a high-pressure homogenizer for 20s each time, treating the mixed solution for 2 times at 40Mpa by dynamic high-pressure microjet, then bathing in a magnetic water bath kettle for 20min at the rotating speed of 800rpm/min and the temperature of 55 ℃, and then filtering out bubbles by using a vacuum pump to obtain a molding solution.
(3) And (3) molding, namely pouring 50m of L molding liquid into a mold of 15 × 10 × 5cm for hot press molding, taking out, cooling and cutting edges to obtain the fish scale gelatin protein packaging material.
Comparative example 1
A commercially available common food packaging bag was used, and cut into the same size of 15 × 10 × 5 cm.
Blank example 1
The fish meat is preserved without any packaging material.
Packaging 100g of fresh fish meat of the same variety (grass carp) (taking out the meat within 10min after killing the fish) in each bag by using the packaging materials prepared in the examples 1-3 and the comparative example 1; examples 1 to 3 and comparative example 1 and blank example 1 were each charged with 10 parts. The mixture is sealed and preserved at the same temperature of 4 ℃, and the color and texture are firstly observed at 0h, 2d, 4d, 6d and 8d respectively. The TVB-N value, TBARs value and colony count were again determined and reported in tables 1, 2, 3 and 4, respectively.
The TVB-N value is determined by the following process:
1. weighing 1-5 g of sample (accurate to 0.001g) in a 250m L conical flask with a plug, adding 100m L of distilled water, shaking uniformly for 30min, and standing to obtain a supernatant as a sample solution.
2. A20 m L2% boric acid solution was placed in a 150m L conical flask, and 2 drops of the mixed indicator were added to immerse the end of the condenser tube of the semimicro distillation apparatus in the solution.
3. Adding several drops of methyl red indicator and several drops of sulfuric acid into the water of steam generator of distillation equipment, and making said solution be orange red, otherwise adding sulfuric acid.
4. Accurately transferring 10m L sample liquid into a reaction chamber of a distillation device, washing a sample inlet with a small amount of distilled water, plugging an inlet glass plug, adding 10m L% magnesium oxide solution, carefully lifting the glass plug to flow into the reaction chamber, plugging the glass plug, adding water at the inlet to seal, preventing air leakage, distilling for 10min, separating the tail end of a condensation tube from an absorption liquid level, distilling for 1min, washing the tail end of the condensation tube with distilled water, and enabling washing liquid to flow into absorption liquid.
5. Immediately after ammonia absorption, the solution was titrated with 0.01 mol/L HCl standard solution, and the solution turned from blue-green to grey-red as the end point.
And (3) calculation of measurement results:
1. the calculation is shown in the following formula:
X1＝[(V1-V2)xC1x14/(M1xV’/V)]x100
in the formula: x1: the content of volatile basic nitrogen of the sample is mg/100 g;
v1, volume of hydrochloric acid standard solution required for titrating the sample, m L;
v2, volume of hydrochloric acid standard solution required for blank titration, m L;
c1, hydrochloric acid standard solution concentration, mol/L;
m1: sample weight, g;
v' is the volume for distilling the sample decomposition liquid, m L;
v is the total volume of the sample solution, m L;
mass of nitrogen equivalent to 1.00m L hydrochloric acid standard titration solution [ c (hcl) 1.000 mol/L ], mg.
2. Repeatability:
two replicates of each sample were taken and measured, the arithmetic mean of which was the result. The relative deviation was allowed to be 5% 2, (the filtrate was measured by the semimicronitrogen method, 3 replicates per treatment, 3 replicates per sample, and the results are expressed in milligrams of N contained per 100g of fish meat sample).
The TBARs value is determined by using a tissue thiobarbituric acid reactant (TBARS) colorimetric quantitative detection kit and recorded.
The total number of colonies is determined in GB4789.2-2016 (national food safety Standard food microbiology test for Total number of colonies).
Color standard: the grading standard is that the fish has inherent color and pattern of the fresh fish, the pattern is obvious, the pattern is fuzzy and has no pattern.
TABLE 1
| 0h | 2d | 4d | 6d | 8d | |
| Example 1 | Obvious pattern | Obvious pattern | Obvious pattern | Obvious pattern | Obvious pattern |
| Example 2 | Obvious pattern | Obvious pattern | Obvious pattern | Fuzzy pattern | Without pattern |
| Example 3 | Obvious pattern | Obvious pattern | Fuzzy pattern | Without pattern | Without pattern |
| Comparative example 1 | Obvious pattern | Obvious pattern | Fuzzy pattern | Without pattern | Without pattern |
| Blank example 1 | Obvious pattern | Obvious pattern | Fuzzy pattern | Without pattern | Without pattern |
TVB-N value:
TABLE 2
TBARs value
TABLE 3
Total number of colonies: TABLE 4
Claims (9)
1. An easily degradable food packaging material of a fish scale collagen matrix is characterized by comprising the following components in parts by weight: 10-20 parts of freshwater fish scale collagen, 0.4-4 parts of wheat starch, 0.1-2 parts of pomegranate flower extract coarse powder, 0.1-1 part of essential oil, 0.2-1 part of glycerol, 0.1-1 part of sodium alginate and 500 parts of deionized water.
2. A method for preparing the easily degradable food packaging material of the fish scale collagen matrix as claimed in claim 1, wherein the method comprises the following steps: taking scale collagen prepared from collagen extracted from freshwater fish scale as base material, adding wheat starch and flos Granati extract powder, and adding essential oil, glycerol and sodium alginate.
3. The method for preparing the easily degradable food packaging material with the fish scale collagen matrix as claimed in claim 2, wherein the preparation method comprises the following steps:
(1) extracting scale collagen of freshwater fish:
① pretreating fish scales by cleaning and decalcifying fresh water fish scales;
② extracting collagen, cleaning pretreated fish scales, drying, adjusting the material-liquid ratio to be 1:25g/ml and the pepsin addition amount to be 4%, adjusting the pH to be 1.5 by using 1M hydrochloric acid, performing ultrasonic treatment at the ultrasonic power of 350W for 30min, leaching at 25 ℃ for 4h, and performing suction filtration to obtain a fish scale collagen solution;
③ concentrating, concentrating the fish scale collagen solution to 10-15% of the original volume by a rotary evaporator;
④ freeze drying, namely, drying by using a freeze dryer, pre-freezing for 24h at-80 ℃, setting all parameters of the freeze dryer as initial temperature-60 ℃, starting vacuumizing after 4h, increasing the temperature by 5 ℃/h until the temperature rises to 30 ℃, and keeping the temperature constant for 4h at the temperature to obtain fish scale collagen powder;
(2) preparation of pomegranate flower extract:
① pretreating by washing fresh flos Granati with deionized water for 3 times, oven drying at 35 deg.C, and pulverizing into flos Granati powder;
② dynamic high-pressure microjet treatment, mixing flos Granati powder with 70% ethanol at a mass volume ratio of 1:10-15, treating with high-pressure homogenizer at 40Mpa for 2 times, each time for 15-30s, and treating with dynamic high-pressure microjet for 2 times;
③ hot water extraction, wherein the hot water extraction is carried out by heating in water bath at 65 deg.C for 1-2h to obtain flos Granati extract solution;
④ centrifuging, centrifuging the flos Granati extract solution to obtain supernatant;
⑤ concentrating, concentrating the centrifuged flos Granati extract solution to 5-10% of the original volume by rotary evaporator;
⑥ freeze drying, namely, pre-freezing the pomegranate flower extract for 24h at-80 ℃, setting the parameters of the freeze dryer as initial temperature-60 ℃, starting to vacuumize after 4h, increasing the temperature at 5 ℃/h until the temperature rises to 30 ℃, and keeping the temperature constant for 4h at the temperature to obtain coarse powder of the pomegranate flower extract;
(3) preparing materials: respectively weighing 10-20 parts of freshwater fish scale collagen, 0.4-4 parts of wheat starch, 0.1-2 parts of coarse powder of a pomegranate flower extract, 0.1-1 part of essential oil, 0.2-1 part of glycerol, 0.1-1 part of sodium alginate and 500 parts of deionized water;
(4) compounding: dissolving freshwater fish scale collagen and wheat starch in deionized water, stirring for 5-10min at 50-60 ℃ on a magnetic stirrer, continuously adding coarse powder of a pomegranate flower extract, essential oil, glycerol and sodium alginate to obtain a mixed solution, treating the mixed solution for 2 times at 40Mpa of a high-pressure homogenizer for 15-30s each time, treating for 2 times by dynamic high-pressure microjet, carrying out water bath for 20-40min in a magnetic water bath kettle at the rotation speed of 600 and 1000rpm/min and the temperature of 55-65 ℃, and then filtering out bubbles by using a vacuum pump to obtain a molding liquid;
(5) and (3) molding, namely pouring 50-100m of L molding liquid into a mold of 15 × 10 × 5cm for hot press molding, taking out, cooling and cutting edges to obtain the fish scale gelatin protein packaging material.
4. The method for preparing a fish scale collagen matrix degradable food packaging material as claimed in claim 3, wherein the freshwater fish scale in step (1) is selected from one or more of grass carp, black carp, silver carp, bighead carp, carp and crucian carp.
5. The method for preparing the easily degradable food packaging material with the scale collagen matrix as claimed in claim 3, wherein the fish scale pretreatment in step (1) comprises the steps of soaking fresh freshwater fish scales in deionized water, washing with water for 3 times, draining, adding 10% citric acid with a solid-to-liquid ratio of 1:20-25(g/m L), treating on a magnetic stirrer for 50-80min at a rotation speed of 800-1000rpm/min, and washing for 3 times to obtain the decalcified fish scales.
6. The method for preparing a fish scale collagen matrix degradable food packaging material as claimed in claim 3, wherein the dynamic high pressure microjet pressure of step (2), step ② is 120 MPa.
7. The method for preparing a fish scale collagen matrix degradable food packaging material as claimed in claim 3, wherein the centrifuge rotation speed in the step (2) ④ is 5000rpm/min, the temperature is-4 ℃, and the time is 15-20 min.
8. The method for preparing a fish scale collagen matrix-based degradable food packaging material as claimed in claim 3, wherein the essential oil in step (3) is one or more of clove, tea tree, chrysanthemum, lemon, grapefruit and sweet orange essential oil.
9. The method for preparing a fish scale collagen matrix degradable food packaging material as claimed in claim 3, wherein the dynamic high pressure microjet pressure in step (4) is 30-60 MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111387477A (en) * | 2020-05-06 | 2020-07-10 | 江西师范大学 | Microcapsule embedding technology for improving digestion stability of lotus leaf flavone |
| CN113899647A (en) * | 2021-09-27 | 2022-01-07 | 山东海奥斯生物科技有限公司 | Method for detecting content of microcrystalline cellulose in collagen casing |
| CN114276658A (en) * | 2021-12-07 | 2022-04-05 | 杭州人民环保科技有限公司 | Degradable material, preparation method thereof and paper cup |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101301319A (en) * | 2008-07-09 | 2008-11-12 | 中国科学院新疆理化技术研究所 | Preparation of granada flower polyphenol and uses thereof |
| CN104356412A (en) * | 2014-11-10 | 2015-02-18 | 江西师范大学 | Preparation method of fish scale gelatin starch antioxidant edible composite film |
| CN105687093A (en) * | 2016-03-30 | 2016-06-22 | 甘肃乡草坊土特产品有限公司 | Anti-aging natural pomegranate skin-care product and preparation method thereof |
| CN107739515A (en) * | 2017-10-19 | 2018-02-27 | 张永华 | A kind of isinglass antibacterial oxidation-resistant film and preparation method thereof |
| CN109777126A (en) * | 2019-03-20 | 2019-05-21 | 江南大学 | A kind of fish scale collagen/mesona polysaccharide blend film and preparation method thereof |
| CN109769920A (en) * | 2019-03-20 | 2019-05-21 | 江南大学 | A kind of fish scale albumen-mesona glue-asparagus powder nutrition edible film and preparation method thereof |
| CN110607075A (en) * | 2019-05-20 | 2019-12-24 | 北京化工大学 | Preparation method of edible fish gelatin antioxidant film containing guava leaf extract |
-
2020
- 2020-03-19 CN CN202010195419.2A patent/CN111471307A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101301319A (en) * | 2008-07-09 | 2008-11-12 | 中国科学院新疆理化技术研究所 | Preparation of granada flower polyphenol and uses thereof |
| CN104356412A (en) * | 2014-11-10 | 2015-02-18 | 江西师范大学 | Preparation method of fish scale gelatin starch antioxidant edible composite film |
| CN105687093A (en) * | 2016-03-30 | 2016-06-22 | 甘肃乡草坊土特产品有限公司 | Anti-aging natural pomegranate skin-care product and preparation method thereof |
| CN107739515A (en) * | 2017-10-19 | 2018-02-27 | 张永华 | A kind of isinglass antibacterial oxidation-resistant film and preparation method thereof |
| CN109777126A (en) * | 2019-03-20 | 2019-05-21 | 江南大学 | A kind of fish scale collagen/mesona polysaccharide blend film and preparation method thereof |
| CN109769920A (en) * | 2019-03-20 | 2019-05-21 | 江南大学 | A kind of fish scale albumen-mesona glue-asparagus powder nutrition edible film and preparation method thereof |
| CN110607075A (en) * | 2019-05-20 | 2019-12-24 | 北京化工大学 | Preparation method of edible fish gelatin antioxidant film containing guava leaf extract |
Non-Patent Citations (5)
| Title |
|---|
| 张德权主编: "《羊肉加工与质量控制》", 31 August 2016, 中国轻工业出版社 * |
| 张立华等: ""石榴不同部位提取物抗油脂氧化及抑菌活性的比较"", 《中国粮油学报》 * |
| 张立华等: "石榴不同部位提取物抗油脂氧化及抑菌活性的比较", 《中国粮油学报》 * |
| 张露等: ""动态高压微射流预处理对甘薯叶多酚提取物抗氧化性的影响机制初探"", 《食品与发酵工业》 * |
| 邵东旭等: ""鱼鳞胶原蛋白复合抗菌膜对罗非鱼肉的保鲜效果"", 《包装工程》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111387477A (en) * | 2020-05-06 | 2020-07-10 | 江西师范大学 | Microcapsule embedding technology for improving digestion stability of lotus leaf flavone |
| CN113899647A (en) * | 2021-09-27 | 2022-01-07 | 山东海奥斯生物科技有限公司 | Method for detecting content of microcrystalline cellulose in collagen casing |
| CN114276658A (en) * | 2021-12-07 | 2022-04-05 | 杭州人民环保科技有限公司 | Degradable material, preparation method thereof and paper cup |
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