CN111333889A - Edible lipid-protein double-layer active membrane and preparation method thereof - Google Patents

Edible lipid-protein double-layer active membrane and preparation method thereof Download PDF

Info

Publication number
CN111333889A
CN111333889A CN202010230316.5A CN202010230316A CN111333889A CN 111333889 A CN111333889 A CN 111333889A CN 202010230316 A CN202010230316 A CN 202010230316A CN 111333889 A CN111333889 A CN 111333889A
Authority
CN
China
Prior art keywords
film
solution
soluble protein
lipid
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202010230316.5A
Other languages
Chinese (zh)
Other versions
CN111333889B (en
Inventor
肖杰
蔡济洋
陈霞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
South China Agricultural University
Original Assignee
South China Agricultural University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by South China Agricultural University filed Critical South China Agricultural University
Priority to CN202010230316.5A priority Critical patent/CN111333889B/en
Publication of CN111333889A publication Critical patent/CN111333889A/en
Application granted granted Critical
Publication of CN111333889B publication Critical patent/CN111333889B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D7/00—Producing flat articles, e.g. films or sheets
    • B29D7/01—Films or sheets
    • 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
    • B65D65/463—Edible 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
    • C08J2389/00—Characterised by the use of proteins; Derivatives thereof
    • 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
    • C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2471/02—Polyalkylene oxides
    • 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
    • C08J2489/00—Characterised by the use of proteins; Derivatives thereof
    • 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
    • C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
    • 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
    • C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
    • C08J2491/06—Waxes
    • 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
    • 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
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/005—Stabilisers against oxidation, heat, light, ozone
    • 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
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/0058—Biocides
    • 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
    • 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
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
    • 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
    • C08K5/13—Phenols; Phenolates
    • C08K5/134—Phenols containing ester groups
    • C08K5/1345—Carboxylic esters of phenolcarboxylic acids
    • 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
    • C08K5/1535—Five-membered rings
    • 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
    • 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

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Preparation And Processing Of Foods (AREA)

Abstract

The invention discloses a lipid-protein edible double-layer active membrane and a preparation method thereof. The method comprises the following steps: respectively dissolving prolamin and water soluble protein in acetic acid-water solution, adding hydrophobic active substance into prolamin and/or adding hydrophilic active substance into water soluble protein to respectively obtain prolamin solution and water soluble protein solution; uniformly mixing the alcohol soluble protein solution and the water soluble protein solution, and adding a plasticizer; mixing the film forming solution with solid lipid, heating to above lipid melting point, homogenizing by high speed shearing to form emulsion, and casting to form film. The preparation process is simple, and the protein-lipid double-layer active membrane can be prepared by one-time tape casting, so that the drying time can be reduced, and the production efficiency can be improved. The active membrane has good one-way water-blocking effect and mechanical property, and can realize the regulation of the release rate of active substances by regulating the proportion of the alcohol soluble protein and the water soluble protein and the mass percentage of lipid.

Description

Edible lipid-protein double-layer active membrane and preparation method thereof
Technical Field
The invention belongs to the technical field of active packaging materials. More particularly, relates to a lipid-protein edible double-layer active membrane and a preparation method thereof.
Background
Non-degradable plastic packaging causes environmental pollution, and films composed of biodegradable materials, such as proteins, polysaccharides and lipids, are gaining increasing popularity from researchers. The biodegradable film can form an active package by loading natural antioxidant and antibacterial active substances, and control the adverse reactions of microbial growth, grease oxidation and the like in food, thereby effectively prolonging the shelf life of the food. However, the film formed of proteins and polysaccharides has poor water-blocking effect, and is greatly limited in application to food having high water activity.
Researchers have added lipids to prepare lipid-polysaccharide or protein composite membranes to enhance the water resistance of the membranes. The preparation method of lipid-polysaccharide or protein composite membranes is generally divided into two methods: the first method is that after the polysaccharide film or the protein film is formed by casting, the melted lipid is cast on the surface of the polysaccharide film or the protein film; the second method is to add lipid into the film-forming solution of polysaccharide or protein to prepare emulsion, and then to cast. Chinese patent CN109608670A discloses a preparation method of a vegetable protein/Arabic gum/lipid emulsified edible composite membrane, which comprises the steps of adding lipid into a membrane forming solution of vegetable protein/Arabic gum, forming a membrane by utilizing a protein/polysaccharide covalent complex, forming an emulsion by shearing and high-pressure homogenization, and finally forming an emulsion membrane by tape casting. Chinese patent CN104861187B discloses a preparation method of a tara gum edible film with hydrophobic property, which comprises the steps of heating and dissolving tara gum, adding glycerol, sorbitol and oleic acid into tara gum solution, homogenizing, and then carrying out tape casting to obtain the tara gum edible film with hydrophobic property. However, the film prepared by the first method has a good water blocking effect, but needs two casting processes, so that the production efficiency is reduced, and the lipid layer formed on the surface has poor compatibility and adhesion with the polysaccharide/protein film, so that the lipid layer is easy to fall off and crack; the second method has poor water-blocking effect because the lipid is uniformly distributed in the membrane matrix and cannot form a continuous lipid water-blocking layer on the surface. Chinese patent CN106905564B also discloses a functional edible film and a preparation method thereof, solid lipid is melted at high temperature, and active substances are added to obtain an oil phase; uniformly dispersing an emulsifier in hot water to obtain a water phase; and adding the water phase into the oil phase to prepare solid lipid nanoparticles loaded with active substances, taking starch as a main film forming substance, homogenizing, and carrying out tape casting to obtain the functional edible film with oxidation resistance and broad-spectrum antibacterial activity. However, edible films using Solid Lipid Nanoparticles (SLNs) also suffer from several disadvantages: the transparency is low, and the thickness and uniformity of the film are difficult to control; the air permeability is poor, and anaerobic respiration of fruits and vegetables can be caused; the mechanical property is low, and cracks or holes are easy to generate during film preparation.
Therefore, how to reduce the flow casting process of lipid-polysaccharide/protein, improve the production efficiency, form an effective water-resisting layer and load various hydrophilic and hydrophobic active compounds to prepare the biodegradable active film has important significance for the development of the active packaging field in China and the reduction of plastic pollution.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a lipid-protein edible double-layer active membrane. The method has simple preparation process, can form the protein-lipid double-layer membrane by one-time tape casting, has good one-way water-blocking effect and mechanical property, can load hydrophilic and hydrophobic active substances simultaneously, and can realize the regulation of the release rate of the active substances by regulating the proportion of the alcohol soluble protein and the water soluble protein and the concentration of the lipid. When the active film is applied to food preservation, the intelligent regulation and control of antioxidant and bacteriostatic effects can be expected to be realized.
Another object of the present invention is to provide an edible lipid-protein bilayer active membrane prepared using the above method.
It is still another object of the present invention to provide a packaging article comprising or produced from the above edible lipid-protein bilayer active film.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a lipid-protein edible double-layer active membrane comprises the following steps:
s1, preparing a film forming solution: respectively dissolving prolamin and water soluble protein in acetic acid-water solution, and after completely dissolving, adding hydrophobic active substance into prolamin and/or adding hydrophilic active substance into water soluble protein to respectively obtain prolamin solution and water soluble protein solution; uniformly mixing the alcohol soluble protein solution and the water soluble protein solution, adding a plasticizer, and stirring to obtain a film forming solution;
s2, mixing the film forming solution obtained in the step S1 with solid lipid, heating to a temperature above the melting point of the lipid, and carrying out high-speed shearing and homogenization to form emulsion;
and S3, pouring the emulsion obtained in the step S2 into a trough of a casting machine while the emulsion is hot, gradually forming a film in the casting machine, and finishing rolling at the other end.
The edible lipid-protein double-layer active film can be formed by one-step casting through a casting machine, the casting process is saved, the drying time is reduced, the film can be formed only by 0.5-2.5 hours, and the production efficiency is improved. The prepared edible film has good one-way water-blocking effect and mechanical property, good transparency and easy regulation of the thickness and air permeability of the film, thereby realizing intelligent regulation of degree-resisting oxidation and bacteriostasis effects.
In some preferred embodiments, in step S1, the total mass concentration of the prolamin protein and the water-soluble protein is 16-27 wt%, wherein the mass ratio of the prolamin protein to the water-soluble protein is 1: 0.4 to 2.7. More preferably, the total mass concentration of the prolamin and the water-soluble protein is 18-22 wt%, wherein the mass ratio of the prolamin to the water-soluble protein is 1: 0.5 to 2.0. The edible film prepared from the prolamin and the water-soluble protein in the dosage range has good film forming property, and has good mechanical strength and transparency. The prepared film forming solution has proper viscosity, and ensures that the lipid can be demulsified and floated to form a double-layer film in the casting process.
In some preferred embodiments, the solid lipid accounts for 10-60% (w/w) of the solid content by mass. More preferably, the solid lipid accounts for 20-50% (w/w) of the solid content by mass. The lipid with the dosage range can be demulsified and floated to form a water-resistant lipid layer in the film forming process, and the formed film is not easy to crack and has good optical performance.
In some preferred embodiments, the sum of the mass of the hydrophobic active matter and the mass of the hydrophilic active matter accounts for 5-18% of the mass of the solid content; the mass ratio of the hydrophobic active substance to the hydrophilic active substance is 1: 1 to 3.
In some preferred embodiments, in step S2, the heating temperature of the film forming solution is 50-90 ℃, the high-speed shearing speed is 6000-20000 rpm, and the homogenizing time is 1-3 min. More preferably, the film-forming solution is heated at 70 deg.C with a high shear rate of 10000rpm for a homogenization time of 2 min. The heating temperature of the film forming solution is 50-90 ℃, and the heating temperature is higher than the melting temperature of lipid, so that the one-step forming of subsequent curtain coating film forming is ensured. If the high-speed shearing speed is more than 20000rpm, the homogenization time is too long, the particle size of the formed emulsion is too small, and the demulsification and floating of lipid in the casting process are not facilitated; and the high-speed shearing speed is less than 6000rpm, the homogenizing time is shorter than 1min, emulsion can be destabilized before casting, a film prepared by casting is rough and uneven, the lipid distributed on the surface is not uniform, the high-speed shearing speed is 6000-20000 rpm, and the homogenizing time is 1-3 min, so that the demulsification and the floating of the lipid in the casting process are facilitated to form a double-layer film, and the film prepared by casting is smooth and flat, and the lipid distributed on the surface is uniform.
In some preferred embodiments, in step S3, the casting temperature of the casting machine is controlled to be 50 to 100 ℃, more preferably 70 to 80 ℃. The casting speed is 0.01 to 0.1m/min, and more preferably 0.03 to 0.05 m/min. The height of the casting machine is set to be 0.2-2 mm, and more preferably 0.6-0.8 mm. The casting temperature is controlled to be above the melting point of the lipid, the casting temperature is controlled to be 50-100 ℃, demulsification and floating of the lipid to form a double-layer film are facilitated by properly increasing the casting temperature, and the mechanical property of the film is reduced if the temperature is higher than 100 ℃. The height of the knife is set to be 0.2-2 mm, so that a relatively continuous lipid layer is formed.
In some preferred embodiments, the prolamin is selected from one or a mixture of two or more of wheat gliadin, zein, avenin, or kafirin;
the water soluble protein is one or a mixture of more than two of gelatin, soybean protein, whey protein or casein; suitable prolamines and water-soluble proteins that can be used according to the present invention include, but are not limited to, these species;
the solid lipid is wax which is solid at normal temperature, and the melting point of the wax is more than 30 ℃;
the hydrophobic active is volatile plant essential oil;
the hydrophilic active comprises an antioxidant and a preservative;
the plasticizer is one or more of glycerol, water, oleic acid or polyethylene glycol; and step S1, controlling the concentration of the plasticizer accounting for 5-20% (v/w) of the solid content.
In some preferred embodiments, the solid lipid is selected from paraffin, beeswax, palm wax, candelilla wax or a mixture of two or more of wood wax;
the plant essential oil is selected from one or more of fructus Citri Sarcodactylis essential oil, flos Caryophylli essential oil, thyme essential oil, lemon vanilla essential oil, herba Ocimi essential oil, herba Salvia officinalis essential oil, herba Rosmarini officinalis essential oil, herba Menthae essential oil, Oregano essential oil, cortex Cinnamomi essential oil, tea tree essential oil, herba Cymbopogonis Citrari essential oil, flos Rosae Multiflorae essential oil or flos Rosae Rugosae essential oil;
the antioxidant is one or more of polyphenol antioxidant, vitamin C, rosmarinic acid and bamboo leaf antioxidant; suitable hydrophobic and hydrophilic actives that may be used in accordance with the present invention include, but are not limited to, these species;
the preservative is selected from potassium sorbate, sodium benzoate, or a combination thereof.
More preferably, the prolamin is zein and the water soluble protein is gelatin (preferably gelatin a, i.e., type a gelatin).
In some preferred embodiments, the plasticizer is one or more of glycerol, water, oleic acid or polyethylene glycol; the concentration of the plasticizer in the solid content in step S1 is 5 to 20% (v/w), and more preferably 8 to 20% (v/w).
In some preferred embodiments, the concentration of the acetic acid-water solution is 70% to 85%, more preferably 80%.
Accordingly, the edible lipid-protein bilayer active membrane prepared by the preparation method is also within the protection scope of the invention.
The invention also provides a packaging product, which comprises the edible lipid-protein double-layer active film prepared by the preparation method or is produced by the edible lipid-protein double-layer active film prepared by the preparation method.
The invention also relates to a packaging product comprising or produced from the edible film.
Compared with the prior art, the invention has the following beneficial effects:
(1) the edible lipid-protein double-layer active film avoids the traditional two-time tape casting preparation process of the lipid-protein double-layer film, can be formed by one-time tape casting through a tape casting machine by utilizing the characteristic that lipid can float at high temperature, saves tape casting procedures, reduces drying time, can form a film only in 0.5-2.5 hours, and improves production efficiency.
(2) The lipid-protein edible double-layer active membrane prepared by the invention can form a continuous lipid water-blocking layer on the surface, and the lipid layer and the protein membrane matrix have good compatibility and adhesion and are not easy to fall off and crack.
(3) The edible film prepared by the invention has good one-way water-blocking effect and mechanical property, is biodegradable and has good transparency.
(4) The edible film prepared by the invention can load hydrophobic and hydrophilic active substances at the same time, and can realize the regulation of the release rate of the active substances by regulating the proportion of the alcohol soluble protein and the water soluble protein and the concentration of the solid lipid. When the edible film is applied to food preservation, the thickness, air permeability and one-way water blocking rate of the film are easy to regulate, and intelligent regulation of antioxidation effect and bacteriostasis effect is expected to be realized, so that the edible film is applied to preservation of foods with different water activities.
Drawings
Fig. 1 is a flow chart illustrating a preparation process of a lipid-protein edible bilayer active membrane according to the present invention.
FIG. 2 is a cross-sectional microscopic view of various examples and comparative examples.
Fig. 3 is a surface contact angle of various examples and comparative examples.
Fig. 4 shows the water vapor transmission rate of various examples and comparative examples.
Figure 5 is a graph of the dissolution curves of essential oils and tea polyphenols for different examples and comparative examples.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. The present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents and are intended to be included in the scope of the present invention.
Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1
A lipid-protein edible double-layer active membrane is prepared by the following steps, wherein the preparation process is shown in figure 1:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the oregano essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding tea polyphenols into gelatin solution, and magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 20 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 2; controlling the mass percent of oregano essential oil accounting for the solid content to be 7.5 percent, and the mass percent of tea polyphenol accounting for the solid content to be 7.5 percent; controlling the concentration of plasticizer glycerol in the solid content to be 8% (v/w);
(2) high-speed homogenization: mixing the film forming solution with paraffin, and controlling the mass percentage of the paraffin in the solid content to be 20% (w/w); heating to 70 deg.C, homogenizing with high speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Example 2
A lipid-protein edible double-layer active membrane is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the oregano essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding tea polyphenols into gelatin solution, and magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 20 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 2; controlling the mass percent of oregano essential oil accounting for the solid content to be 7.5 percent, and the mass percent of tea polyphenol accounting for the solid content to be 7.5 percent; controlling the concentration of plasticizer glycerol in the solid content to be 8% (v/w);
(2) high-speed homogenization: mixing the film forming solution with paraffin, and controlling the mass percent of the paraffin accounting for the solid content to be 50% (w/w); heating to 70 deg.C, homogenizing with high speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Example 3
A lipid-protein edible double-layer active membrane is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the oregano essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding tea polyphenols into gelatin solution, and magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 20 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 1; controlling the mass percent of oregano essential oil accounting for the solid content to be 7.5 percent, and the mass percent of tea polyphenol accounting for the solid content to be 7.5 percent; controlling the concentration of plasticizer glycerol in the solid content to be 8% (v/w);
(2) high-speed homogenization: mixing the film forming solution with paraffin, and controlling the mass percentage of the paraffin in the solid content to be 20% (w/w); heating to 70 deg.C, homogenizing with high speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Example 4
A lipid-protein edible double-layer active membrane is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the oregano essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding tea polyphenols into gelatin solution, and magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 20 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 1; controlling the mass percent of oregano essential oil accounting for the solid content to be 7.5 percent, and the mass percent of tea polyphenol accounting for the solid content to be 7.5 percent; controlling the concentration of plasticizer glycerol in the solid content to be 8% (v/w);
(2) high-speed homogenization: mixing the film forming solution with paraffin, and controlling the mass percentage of the paraffin in the solid content to be 30% (w/w); heating to 70 deg.C, homogenizing with high speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Example 5
A lipid-protein edible double-layer active membrane is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the oregano essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding tea polyphenols into gelatin solution, and magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 20 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 0.5; controlling the mass percent of oregano essential oil accounting for the solid content to be 7.5 percent, and the mass percent of tea polyphenol accounting for the solid content to be 7.5 percent; controlling the concentration of plasticizer glycerol in the solid content to be 8% (v/w);
(2) high-speed homogenization: mixing the film forming solution with paraffin, and controlling the mass percentage of the paraffin in the solid content to be 20% (w/w); heating to 70 deg.C, homogenizing with high speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Example 6
A lipid-protein edible double-layer active membrane is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the oregano essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding tea polyphenols into gelatin solution, and magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 20 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 0.5; controlling the mass percent of oregano essential oil accounting for the solid content to be 7.5 percent, and the mass percent of tea polyphenol accounting for the solid content to be 7.5 percent; controlling the concentration of plasticizer glycerol in the solid content to be 8% (v/w);
(2) high-speed homogenization: mixing the film forming solution with paraffin, and controlling the mass percentage of the paraffin in the solid content to be 30% (w/w); heating to 70 deg.C, homogenizing with high speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Example 7
A lipid-protein edible double-layer active membrane is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the cinnamon essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding vitamin C into gelatin solution, and continuously magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding polyethylene glycol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 20 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 2; controlling the mass percent of cinnamon essential oil accounting for the solid content to be 2.5% (w/w), and the mass percent of vitamin C accounting for the solid content to be 2.5% (w/w); controlling the concentration of the plasticizer polyethylene glycol in the solid content to be 8% (v/w);
(2) high-speed homogenization: mixing the film forming solution with beeswax, heating to 70 deg.C, homogenizing with high speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min; controlling the mass percentage of the beeswax in the solid content to be 20%;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Example 8 Loading of hydrophobic actives alone
A lipid-protein edible double-layer active membrane is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the thyme essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 18 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 0.5; controlling the mass percentage of the thyme essential oil in the solid content to be 15% (w/w), and controlling the concentration of the plasticizer glycerol in the solid content to be 8% (v/w);
(2) high-speed homogenization: mixing the film forming solution with paraffin, heating to 70 ℃, and homogenizing by using a high-speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min; controlling the mass percentage of paraffin accounting for the solid content to be 20%;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Example 9 Loading of hydrophilic actives alone
A lipid-protein edible double-layer active membrane is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring until the potassium sorbate is completely dissolved, adding potassium sorbate into the gelatin A solution, and continuing magnetic stirring for 15min to obtain a water-soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding oleic acid, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 22 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 2; controlling the mass percentage of potassium sorbate in the solid content to be 15% (w/w), and controlling the concentration of the plasticizer oleic acid in the solid content to be 8% (v/w);
(2) high-speed homogenization: mixing the film forming solution with palm wax, heating to 70 ℃, and homogenizing by using a high-speed shearing machine to form emulsion; controlling the shearing speed to be 20000rpm, and controlling the time to be 1 min; controlling the mass percentage of the palm wax in the solid content to be 50%;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.8mm, the casting temperature is 80 ℃, and the casting speed is 0.05 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Example 10
A lipid-protein edible double-layer active membrane is prepared by the following steps:
(1) preparation of film-forming solution: mixing zein and kafirin in a mass ratio of 1: 1 is dissolved in 80 percent acetic acid-water solution, and after the solution is stirred to be completely dissolved, alcohol soluble protein solution is obtained;
gelatin A and whey protein are mixed according to the mass ratio of 1: 1 is dissolved in 80 percent acetic acid-water solution, and water soluble protein solution is obtained after the mixture is stirred to be completely dissolved;
adding oregano essential oil into the alcohol soluble protein solution, and continuing to magnetically stir for 15 min; adding tea polyphenols into water soluble protein solution, and magnetically stirring for 15 min;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the prolamin and the water-soluble protein to be 16 wt%, wherein the mass ratio of the prolamin to the water-soluble protein is 1: 0.4; controlling the mass percentage of the oregano essential oil in the solid content to be 9% (w/w), and the mass percentage of the oregano essential oil in the solid content to be 9% (w/w); controlling the concentration of plasticizer glycerol in the solid content to be 20% (v/w);
(2) high-speed homogenization: mixing the film forming solution with paraffin, heating to 90 ℃, and homogenizing by using a high-speed shearing machine to form emulsion; controlling the shearing speed to be 20000rpm, and controlling the time to be 1 min; controlling the mass percentage of paraffin accounting for the solid content to be 60%;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.2mm, the casting temperature is 100 ℃, and the casting speed is 0.1 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Example 11
A lipid-protein edible double-layer active membrane is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the oregano essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding tea polyphenols into gelatin A solution, and magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding polyethylene glycol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 27 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 2.7; controlling the mass percent of the oregano essential oil accounting for the solid content to be 7.5 percent (w/w), and the mass percent of the tea polyphenol accounting for the solid content to be 7.5 percent (w/w); controlling the concentration of plasticizer glycerol in the solid content to be 8% (v/w);
(2) high-speed homogenization: mixing the film forming solution with paraffin, heating to 50 ℃, and homogenizing by using a high-speed shearing machine to form emulsion; controlling the shearing speed to be 6000rpm and the time to be 3 min; controlling the mass percentage of paraffin accounting for the solid content to be 10 percent;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.2mm, the casting temperature is 50 ℃, and the casting speed is 0.01 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Comparative example 1
Compared with examples 1 and 2, the edible active protein film prepared conventionally is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the oregano essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding tea polyphenols into gelatin solution, and magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 20 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 2; controlling the mass percent of oregano essential oil accounting for the solid content to be 7.5 percent, and the mass percent of tea polyphenol accounting for the solid content to be 7.5 percent; controlling the concentration of plasticizer glycerol in the solid content to be 8% (v/w);
(2) heating: heating the film-forming solution to 70 ℃, and homogenizing by using a high-speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Comparative example 2
Compared with examples 3 and 4, the edible active protein film prepared conventionally is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the oregano essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding tea polyphenols into gelatin solution, and magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 20 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 1; controlling the mass percent of oregano essential oil accounting for the solid content to be 7.5 percent, and the mass percent of tea polyphenol accounting for the solid content to be 7.5 percent; controlling the concentration of plasticizer glycerol in the solid content to be 8% (v/w);
(2) heating: heating the film-forming solution to 70 ℃, and homogenizing by using a high-speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Comparative example 3
Compared with examples 5 and 6, the edible active protein film prepared conventionally is prepared by the following steps:
(1) preparation of film-forming solution: respectively dissolving zein and gelatin A in 80% acetic acid-water solution; after stirring to be completely dissolved, adding the oregano essential oil into the zein solution, and continuing to stir for 15min by magnetic force to obtain the zein solution;
adding tea polyphenols into gelatin solution, and magnetically stirring for 15min to obtain water soluble protein solution;
mixing the alcohol soluble protein solution and the water soluble protein solution, adding glycerol, and continuously stirring for 15 min;
controlling the total mass concentration of the zein and the water-soluble protein gelatin A to be 20 wt%, wherein the mass ratio of the zein to the water-soluble protein gelatin A is 1: 0.5; controlling the mass percent of oregano essential oil accounting for the solid content to be 7.5 percent, and the mass percent of tea polyphenol accounting for the solid content to be 7.5 percent; controlling the concentration of plasticizer glycerol in the solid content to be 8% (v/w);
(2) heating: heating the film-forming solution to 70 ℃, and homogenizing by using a high-speed shearing machine to form emulsion; controlling the shearing rotation speed to 10000rpm and the time to be 2 min;
(3) film laying by a one-step tape casting process: pouring the emulsion into a trough of a casting machine, drying the emulsion in the casting machine to form a film, and then rolling the film at the other end of the casting machine to obtain a lipid-protein edible double-layer active film; the control casting machine parameters are: the height of the knife is 0.6mm, the casting temperature is 70 ℃, and the casting speed is 0.02 m/min;
(4) the prepared edible film is placed in a closed container with the temperature of 25-30 ℃ and the humidity of 45% -55% for storage and to be tested.
Examples of the experiments
1. The cross-sectional microstructure of the products obtained in example 1 and comparative example 1 was observed under the same conditions using an electron scanning microscope, and the test results are shown in FIG. 2.
FIG. 2 is a sectional microstructure of a film with an air surface above the film and a bottom surface below the film. Comparative example 1 and comparative example 2 did not show a layered structure, and a two-layer film structure could not be formed. While examples 1 and 4 show a distinct layered structure, the irregular shape at the air level is paraffin (paraffin layer where red circles are marked), and the underlying matrix is prolamin and glutinin, and during casting film formation, paraffin originally mixed with the protein solution breaks emulsion and floats to form a double-layer film. During the baking process of the film-forming emulsion in a casting machine, the oil-in-water emulsion state of the film-forming emulsion is destroyed (namely demulsification) at high temperature, and paraffin floats upwards, so that a continuous paraffin layer is formed on the air surface. The paraffin layer has one-way water-blocking effect, and has good compatibility and adhesion with protein membrane matrix (prolamin and gelatin protein layer), and is not easy to fall off and crack.
2. The surface contact angle measurements were carried out on the products obtained in examples 1, 2, 3, 4, 5 and 6 and comparative examples 1, 2 and 3 under the same conditions
(1) The contact angle of the film was measured by a dropping method using an SC-100 contact angle measuring Instrument (ShengDing Precision Instrument co., ltd., China). The film is cut into a strip shape, the strip shape is fixed on a glass slide by using double-sided adhesive tape, a drop of Milli-Q water (2 mu L) is dripped on the surface of the film, contact angle images are obtained by photographing in 0s and 60s respectively, contact angle data can be obtained by measuring the images in a computer, and the average value of the contact angle is obtained by selecting 7-10 different positions on the film for measurement and calculation. The contact angles were measured on both the air side and the bottom side of each sample.
(2) As can be seen from fig. 3, the contact angles of the air planes of examples 1, 2, 3, 4, 5, 6 are all increased as compared to comparative examples 1, 2, 3, indicating that the examples can enhance the surface hydrophobicity of the air plane of the film. The contact angles of the air surfaces of examples 1, 2, 3, 4, 5 and 6 were larger than those of the corresponding bottom surfaces, which indicates that the lipids were able to float upward during casting and delaminate on the air surface of the film.
3. Water vapor transmission rate measurements were carried out on the products obtained in examples 1, 2, 3, 4, 5 and 6 and comparative examples 1, 2 and 3 under the same conditions
(1) The water vapor transmission rate was determined according to GB 1037-1988 cup method, test method for Water vapor permeability of Plastic films and sheets. Weighing about 11g of anhydrous calcium chloride by adopting a cup-like method at the temperature of 25 ℃, putting the anhydrous calcium chloride into a weighing bottle, shearing the composite film into a proper size, sealing the opening of the weighing bottle, and fastening by using a rubber ring to ensure the sealing property. The weighing bottle was weighed and placed in a desiccator (containing tertiary water) at a temperature of 25 ℃ plus or minus 1 ℃ and a relative humidity of 100%, and the weight of the weighing bottle was weighed every 12 hours and continuously measured for 5 days. The water vapor transmission rate of the membrane is calculated as follows:
Figure BDA0002429078930000151
wherein △ m is the mass increment/g of the sample in t time, d is the thickness/cm of the film, A is the effective area/cm of the sample for water vapor permeation2T is the time interval/s of each measurement, △ p is the water vapor pressure difference/Pa of the two sides of the membrane, and the saturated vapor pressure of pure water at 25 ℃ is 3167.1 Pa.
(2) As can be seen from fig. 4, the water vapor transmission rate of the films was decreased in examples 1 and 2 as compared to comparative example 1, in examples 3 and 4 as compared to comparative example 2, and in examples 5 and 6 as compared to comparative example 3, which indicates that the present invention can effectively enhance the unidirectional water resistance of the films. The water vapor transmission rate of the air face is lower than that of the corresponding bottom face of examples 1, 2, 3, 4, 5, 6, which again verifies that the lipid floats up to form a water-resistant layer during casting, and the film prepared by the invention has good one-way water resistance.
4. The products obtained in examples 1, 2 and 3 and comparative example were subjected to mechanical property test and transparency value test under the same conditions, and the test results are shown in table 1.
TABLE 1 comparison of mechanical Properties and transparency values of different edible films
Figure BDA0002429078930000161
As can be seen from the data in table 1, although the addition of lipid can reduce the mechanical properties of the membrane, examples 1, 2, 3, 4, 5, and 6 all have relatively good tensile strength and elongation at break, and can withstand a certain mechanical impact in practical applications. And the film has good transparency, so that the acceptability of consumers on the appearance of the film is ensured, and the loss of nutrients in food by light irradiation is reduced.
5. The products obtained in examples 1, 2 and 3 and comparative examples 1, 2 and 3 were subjected to the measurement of the elution release curves of oregano essential oil and tea polyphenol, respectively, under the same conditions.
(1) Determination of the dissolution profile of the essential oil 1g of the membrane was cut into 5 × 5 squares, immersed in 30mL of 80% glycerol-water solution, left to stand, 0.5mL of the solution was taken out at a certain time and extracted with 4mL of n-hexane under vigorous shaking, the absorbance was measured at 276nm with an ultraviolet spectrophotometer using n-hexane as a reference.
(2) According to the national standard GB/8213-2002, a ferrous tartrate colorimetric method is adopted for measuring the concentration of tea polyphenol, a ferrous tartrate solution and a pH 7.5 buffer solution are prepared in advance, a film is formed into a square block of 5 × 5, the square block is immersed into 30mL of purified water, the solution is kept stand, 1mL of the solution is taken out at a certain time point, a 25mL volumetric flask is filled with the solution, 4mL of the solution and 5mL of the solution of the ferrous tartrate are added, the solution is fully mixed, the pH 7.5 buffer solution is used for fixing the volume to a scale line, the solution is fully mixed, a reagent blank solution is used as a reference, an ultraviolet spectrophotometer is used for measuring the absorbance at 540nm, the content of the tea polyphenol is calculated according to the previously measured standard curve, and finally, the release curve of the tea polyphenol release ratio (the content of dissolved tea polyphenol accounts for the percentage of the originally added essential oil content) along with the.
(3) The essential oil is released by water molecules entering the membrane matrix to destroy the structure of the membrane matrix, so that the essential oil is released into the environment, and the tea polyphenol is released by water molecules entering the membrane matrix, dissolved in the water molecules and driven into the environment. Thus, the release of both is related to the water absorption of the film.
As shown in fig. 5, the dissolution rate of essential oil and tea polyphenol is controlled by the lipid concentration, because the distribution of lipid in the membrane is different, the water absorption of the membrane and the release path of essential oil and tea polyphenol in the membrane are changed. And is also regulated by the ratio of prolamin to water soluble protein due to the difference in hydrophobicity of the membrane matrix. Therefore, the release rate of the active substance in the film can be regulated and controlled by regulating the lipid concentration and the proportion of the prolamin and the water-soluble protein, so that the film can be applied to the fresh-keeping of foods with different water activities. For example, when applied to food products having a relatively high water activity (such as fruit), the edible films prepared in examples 5 and 6, etc. can be used; the edible films prepared in examples 1 and 2, etc. may be used when applied to food products with low water activity, such as nuts.
6. The products obtained in example 1 and examples 7, 8, 9, 10 and 11 were subjected to cross-sectional microstructure observation, surface contact angle test, water vapor transmission rate test, mechanical property test and active substance elution release property test under the same conditions. The test method was consistent with the products prepared in experimental examples 1-6 above.
As a result, the products obtained in examples 7, 8, 9, 10 and 11 were found to have good lipid stratification, and the air side of the film had a higher water-blocking effect than the bottom side, indicating that the edible films obtained in examples 7 to 11 had good unidirectional water-blocking performance, and that the edible films had good mechanical properties and transparency. In addition, the release efficiency of either the hydrophilic or hydrophobic active carried by these edible films can be modulated.
The applicant declares that the above detailed description is a preferred embodiment described for the convenience of understanding the present invention, but the present invention is not limited to the above embodiment, i.e. it does not mean that the present invention must be implemented by means of the above embodiment. It will be apparent to those skilled in the art that any modification of the present invention, equivalent substitutions of selected materials and additions of auxiliary components, selection of specific modes and the like, which are within the scope and disclosure of the present invention, are contemplated by the present invention.

Claims (10)

1. A preparation method of a lipid-protein edible double-layer active film is characterized by comprising the following steps:
s1, preparing a film forming solution: dissolving prolamin and water soluble protein in acetic acid-water solution respectively; after complete dissolution, adding a hydrophobic active substance into the alcohol soluble protein and/or adding a hydrophilic active substance into the water soluble protein to respectively obtain an alcohol soluble protein solution and a water soluble protein solution; uniformly mixing the alcohol soluble protein solution and the water soluble protein solution, adding a plasticizer, and stirring to obtain a film forming solution;
s2, mixing the film forming solution obtained in the step S1 with solid lipid, heating to a temperature above the melting point of the lipid, and carrying out high-speed shearing and homogenization to form emulsion;
and S3, pouring the emulsion obtained in the step S2 into a trough of a casting machine while the emulsion is hot, gradually forming a film in the casting machine, and finishing rolling at the other end.
2. The method according to claim 1, wherein in step S1, the total mass concentration of the prolamin and the water-soluble protein is 16-27 wt%, and the mass ratio of the prolamin and the water-soluble protein is 1: 0.4 to 2.7.
3. The method according to claim 2, wherein the solid lipid is contained in an amount of 10 to 60% by mass (w/w) based on the solid content.
4. The preparation method according to claim 3, wherein the mass sum of the hydrophobic active substance and the hydrophilic active substance accounts for 5-18% of the solid content; the mass ratio of the hydrophobic active substance to the hydrophilic active substance is 1: 1 to 3.
5. The method according to claim 1, wherein in step S2, the film forming solution is heated at a temperature of 50-90 ℃, at a high shear rate of 6000-20000 rpm, and for a homogenization time of 1-3 min.
6. The method according to claim 1, wherein in step S3, the casting temperature of the casting machine is controlled to be 50 to 100 ℃, the casting speed is 0.01 to 0.1m/min, and the height of the casting machine is set to be 0.2 to 2 mm.
7. The method according to claim 1, wherein the prolamin is selected from the group consisting of gliadin, zein, avenin, and kafirin;
the water soluble protein is one or a mixture of more than two of gelatin, soybean protein, whey protein or casein;
the solid lipid is wax which is solid at normal temperature, and the melting point of the wax is more than 30 ℃;
the hydrophobic active is volatile plant essential oil;
the hydrophilic active comprises an antioxidant and a preservative;
the plasticizer is one or more of glycerol, water, oleic acid or polyethylene glycol; and step S1, controlling the concentration of the plasticizer accounting for 5-20% (v/w) of the solid content.
8. The preparation method according to claim 7, wherein the solid lipid is selected from paraffin, beeswax, carnauba wax, candelilla wax or wood wax, or a mixture of two or more thereof;
the plant essential oil is selected from one or more of fructus Citri Sarcodactylis essential oil, flos Caryophylli essential oil, thyme essential oil, lemon vanilla essential oil, herba Ocimi essential oil, herba Salvia officinalis essential oil, herba Rosmarini officinalis essential oil, herba Menthae essential oil, Oregano essential oil, cortex Cinnamomi essential oil, tea tree essential oil, herba Cymbopogonis Citrari essential oil, flos Rosae Multiflorae essential oil or flos Rosae Rugosae essential oil;
the antioxidant is one or more of polyphenol antioxidant, vitamin C, rosmarinic acid and bamboo leaf antioxidant;
the preservative is selected from potassium sorbate, sodium benzoate, or a combination thereof.
9. A lipid-protein edible double-layer active membrane prepared by the preparation method of any one of claims 1 to 8.
10. A packaging product comprising or produced from the edible lipid-protein bilayer active film prepared by the preparation method of any one of claims 1 to 8.
CN202010230316.5A 2020-03-27 2020-03-27 Edible lipid-protein double-layer active membrane and preparation method thereof Active CN111333889B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010230316.5A CN111333889B (en) 2020-03-27 2020-03-27 Edible lipid-protein double-layer active membrane and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010230316.5A CN111333889B (en) 2020-03-27 2020-03-27 Edible lipid-protein double-layer active membrane and preparation method thereof

Publications (2)

Publication Number Publication Date
CN111333889A true CN111333889A (en) 2020-06-26
CN111333889B CN111333889B (en) 2021-05-25

Family

ID=71178565

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010230316.5A Active CN111333889B (en) 2020-03-27 2020-03-27 Edible lipid-protein double-layer active membrane and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111333889B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112704112A (en) * 2020-12-25 2021-04-27 东北农业大学 Preparation method of edible coating liquid for bacteriostasis and fresh-keeping of eggs
CN113480784A (en) * 2021-06-04 2021-10-08 南京中医药大学 Preparation method of chitosan-alcohol soluble protein-essential oil-polyphenol edible emulsion liquid film
CN113907124A (en) * 2020-12-30 2022-01-11 吉林农业大学 Corn filament polyphenol-whey protein composite membrane and application thereof
CN115029005A (en) * 2022-06-27 2022-09-09 重庆师范大学 Chitosan/lactalbumin composite edible preservative film and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140230690A1 (en) * 2011-09-23 2014-08-21 Centro Regional De Productividad E Innovacion Del Cauca Crepic Biodegradable packaging obtained from cassava flour and fique fiber and their manufacture process
CN106905564A (en) * 2017-01-18 2017-06-30 华南理工大学 A kind of feature edible film and preparation method thereof
WO2019068155A1 (en) * 2017-10-08 2019-04-11 De Paula Lima Roseane Composition for manufacturing edible, recyclable, biodegradable containers for storing liquids and foods
CN110202860A (en) * 2019-05-31 2019-09-06 华南农业大学 A kind of active composite membrane of gradient slow-release and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140230690A1 (en) * 2011-09-23 2014-08-21 Centro Regional De Productividad E Innovacion Del Cauca Crepic Biodegradable packaging obtained from cassava flour and fique fiber and their manufacture process
CN106905564A (en) * 2017-01-18 2017-06-30 华南理工大学 A kind of feature edible film and preparation method thereof
WO2019068155A1 (en) * 2017-10-08 2019-04-11 De Paula Lima Roseane Composition for manufacturing edible, recyclable, biodegradable containers for storing liquids and foods
CN110202860A (en) * 2019-05-31 2019-09-06 华南农业大学 A kind of active composite membrane of gradient slow-release and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
SEUNG YONG CHO等: "Edible oxygen barrier bilayer film pouches from corn zein and soy protein isolate", 《FOOD SCIENCE AND TECHNOLOGY》 *
郭新华: "以大豆分离蛋白为基质的可食性食品包装薄膜制备及性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112704112A (en) * 2020-12-25 2021-04-27 东北农业大学 Preparation method of edible coating liquid for bacteriostasis and fresh-keeping of eggs
CN113907124A (en) * 2020-12-30 2022-01-11 吉林农业大学 Corn filament polyphenol-whey protein composite membrane and application thereof
CN113480784A (en) * 2021-06-04 2021-10-08 南京中医药大学 Preparation method of chitosan-alcohol soluble protein-essential oil-polyphenol edible emulsion liquid film
CN115029005A (en) * 2022-06-27 2022-09-09 重庆师范大学 Chitosan/lactalbumin composite edible preservative film and preparation method thereof
CN115029005B (en) * 2022-06-27 2023-08-25 重庆师范大学 Chitosan/whey protein composite edible preservative film and preparation method thereof

Also Published As

Publication number Publication date
CN111333889B (en) 2021-05-25

Similar Documents

Publication Publication Date Title
CN111333889B (en) Edible lipid-protein double-layer active membrane and preparation method thereof
Chiumarelli et al. Stability, solubility, mechanical and barrier properties of cassava starch–Carnauba wax edible coatings to preserve fresh-cut apples
Atarés et al. Characterization of sodium caseinate-based edible films incorporated with cinnamon or ginger essential oils
Pérez-Córdoba et al. Physico-chemical, antimicrobial and antioxidant properties of gelatin-chitosan based films loaded with nanoemulsions encapsulating active compounds
Yang et al. Effects of lipids on mechanical and moisture barrier properties of edible gellan film
Sapper et al. Antifungal and functional properties of starch-gellan films containing thyme (Thymus zygis) essential oil
Santos et al. Effect of the addition of carnauba wax on physicochemical properties of chitosan films
Yin et al. Surface modification of sodium caseinate films by zein coatings
Cao et al. Mechanical properties of gelatin films cross-linked, respectively, by ferulic acid and tannin acid
Pereda et al. Caseinate films modified with tung oil
CN105663039B (en) Load dewatering medicament and casein/polysaccharide composite lotion of nutrients and preparation method thereof
US20210186064A1 (en) Edible film with enhanced release efficiency of essential oil and preparation method thereof
Lopez-Polo et al. Humectability and physical properties of hydroxypropyl methylcellulose coatings with liposome-cellulose nanofibers: Food application
CN110202860A (en) A kind of active composite membrane of gradient slow-release and preparation method thereof
CN101150960A (en) Foodstuff particulate lipid composition
Bourtoom et al. Improvement of water barrier property of rice starch-chitosan composite film incorporated with lipids
Ribeiro et al. Edible films prepared with different biopolymers, containing polyphenols extracted from elderberry (Sambucus Nigra L.), to protect food products and to improve food functionality
Lira-Vargas et al. Biopolymeric films based on cactus (Opuntia ficus-indica) mucilage incorporated with gelatin and beeswax
CN112961409A (en) Chitosan-based edible film containing cinnamon oil/cellulose nanocrystals and preparation method and application thereof
Syarifuddin et al. Physical, mechanical, and barrier properties of sodium alginate/gelatin emulsion based-films incorporated with canola oil
Uscategui et al. Concentrates of sugarcane juice and whey protein: Study of a new powder product obtained by spray drying of their combinations
Wu et al. Effects of cinnamon essential oil-loaded Pickering emulsion on the structure, properties and application of chayote tuber starch-based composite films
CN116270318A (en) Oil drop containing ammonia-terminal polydimethylsiloxane as well as preparation method and application thereof
Morales et al. Blend of renewable bio-based polymers for oil encapsulation: Control of the emulsion stability and scaffolds of the microcapsule by the gummy exudate of Prosopis nigra
Miele et al. Improving physical properties of sodium caseinate based coating with the optimal formulation: Effect on strawberries’ respiration and transpiration rates

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant