CN113845677A - Emulsion film and preparation method thereof - Google Patents
Emulsion film and preparation method thereof Download PDFInfo
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- CN113845677A CN113845677A CN202111177265.5A CN202111177265A CN113845677A CN 113845677 A CN113845677 A CN 113845677A CN 202111177265 A CN202111177265 A CN 202111177265A CN 113845677 A CN113845677 A CN 113845677A
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- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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- 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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/132—Phenols containing keto groups, e.g. benzophenones
Abstract
The invention discloses an emulsion film and a preparation method thereof, and belongs to the technical field of food packaging materials. The invention uses natural soybean oil to stabilize curcumin emulsion, improves the stability of curcumin, compounds natural edible biological macromolecule carboxymethyl chitosan and glycerol as a plasticizer, prepares a film by a solution casting method, and has good mechanical property and moisture and oxygen resistance. The oil body is rich in components which are beneficial to human health, such as polyunsaturated fatty acid, phytosterol, tocopherol, carotenoid, oil body protein and the like, curcumin also provides antioxidant and antibacterial activity, carboxymethyl chitosan has strong film forming property, biocompatibility, degradability, antibacterial property and nontoxicity, and the prepared film can be applied to packaging and fresh-keeping of food, has the effects of delaying product deterioration and prolonging shelf life, and ensures the quality and safety of the food.
Description
Technical Field
The invention relates to an emulsion film and a preparation method thereof, belonging to the technical field of food packaging materials.
Background
Soybean, which is an important oil crop in China, has lipids stored in subcellular structure particles, namely soybean oil bodies, mainly in the form of Triglyceride (TAG). Soy oil bodies are found in the food industry to be as beneficial as pre-emulsified additives or carriers for bioactive ingredients, where they are present as pre-emulsified oils in seeds, as naturally occurring food materials, containing polyunsaturated fatty acids, phospholipids, tocopherols, phytosterols and oil body proteins, among other ingredients beneficial to human health, and also have the potential to carry hydrophobic bioactive or aromatic compounds, as capsules for fat-soluble food ingredients, for applications in the development of food, pharmaceuticals and personal care products, among others. The diameter of a soybean oil body is usually 0.2-0.5 mu m, the structure is that TAG is wrapped by single-layer phospholipid, the surface of the soybean oil body is embedded with some proteins, the hydrophobic structure domain of oleosin is fixed in an oil core, the hydrophilic structure domain is reserved on the surface of the oil body, and the unique structure of the phospholipid layer promotes the oil body to be dispersed in a water phase and generate a natural oil-in-water emulsifying system.
Curcumin is a natural polyphenol of turmeric, chemically named 1, 7-bis (4-hydroxy-3-methoxyphenyl) -1, 6-heptadiene-3, 5-dione, is a clinically approved compound with a variety of biological activities, such as anti-inflammatory, anti-cancer, anti-coagulant, anti-proliferative, anti-diabetic, anti-oxidant, and antibacterial activities. However, curcumin may lose its function during preparation and storage due to heat, light and oxidation due to its low bioavailability, low pH and heat sensitivity, susceptibility to oxidation and chemical degradation, and its use is limited. Thus to improve the stability of curcumin, new strategies are needed to provide this compound and incorporate it into films that can be protected with soy oil body emulsions, while most films simply add curcumin to the film without further treatment.
Carboxymethyl chitosan (CMCS) is an amphoteric polyelectrolyte containing amino and carboxyl groups. In contrast to the insolubility of chitosan in water, CMCS has good water solubility due to its strong film-forming property, biocompatibility, degradabilityAnd has antibacterial and nontoxic effects, and can be widely used in the fields of edible film, medicine, etc., and CMCS is used for treating gas (CO)2And O2) Has selective permeability and good mechanical properties. However, their hydrophilicity results in poor barrier properties to moisture, which limits the use of CMCS.
Disclosure of Invention
The invention aims to provide an emulsion film and a preparation method thereof, and particularly relates to a preparation method of a soy oil stable curcumin emulsion composite carboxymethyl chitosan-based film.
The technical scheme of the invention is as follows:
a method for preparing an emulsion film, which comprises the following steps: firstly adopting soybean oil to stabilize curcumin emulsion, then compounding carboxymethyl chitosan, and finally taking glycerin as a plasticizer to prepare the curcumin emulsion by a solution casting method.
Further defined, the method includes the steps of:
step one, preparing soybean oil body;
step two, dispersing the soybean oil body obtained in the step one in deionized water, adding curcumin, mixing and homogenizing to obtain curcumin emulsion;
dissolving carboxymethyl chitosan in deionized water, filtering, adding glycerol, stirring, adding curcumin emulsion, stirring, mixing, and degassing in an ultrasonic cleaning instrument to obtain a film-forming dispersion, wherein the ultrasonic intensity is 300W, and the ultrasonic treatment time is 3 min;
and step four, preparing the film-forming dispersion obtained in the step three into a film by adopting a solution casting method, drying and cooling the film to room temperature, uncovering the film, and placing the film in a constant temperature and humidity chamber for balancing to obtain the emulsion film.
Further limiting, the specific operation process of the step one is as follows:
(1) soaking soybeans in deionized water at 4 ℃ for 18h, wherein the ratio of the soaked soybeans to the deionized water is 1:9 grinding the mixture in a tissue crusher for 8min after mixing, removing bean dregs from the ground mixture through three layers of absorbent gauze, and collecting filtrate;
(2) mixing sucrose and the filtrate obtained in step (1), stirring in ice water bath for 10min, adjusting pH to 11.0 with 1mol/L NaOH, centrifuging at 25000 × g below 4 deg.C for 30min, and collecting upper layer cream;
(3) dissolving the upper layer cream collected in the step (2) in a sucrose solution with the mass fraction of 20% according to the feed-liquid ratio of 1:8, adjusting the pH value to 11.0 by using 1mol/L NaOH, centrifuging for 30min under the conditions of 25000 Xg at the temperature of below 4 ℃, collecting upper layer purified oil bodies, and repeating the step once;
(4) dissolving the purified oil body obtained in the step (3) in deionized water according to the material-liquid ratio of 1:8, adjusting the pH value to 11.0, centrifuging for 30min at the temperature of below 4 ℃ and under the condition of 25000 Xg, and collecting the upper layer substance to obtain the soybean oil body.
Further limiting, the feed-liquid ratio of the soybeans to the deionized water in the step (1) is 1: 5.
Further limiting, the feed-liquid ratio of the sucrose to the filtrate in the step (2) is 1: 4.
Further limiting, the specific operation process of the step two is as follows:
dispersing the soybean oil body obtained in the step one in deionized water, so that the mass concentration of the soybean oil body in the water phase is 5-15%, the mass concentration of curcumin in the oil phase is 0.06-0.10%, and the mass ratio of the oil phase to the water phase is (1-2): (8-9), homogenizing and mixing for 3min by a homogenizer at the speed of 5000rpm, and finally homogenizing and circulating for 2 times by a high-pressure homogenizer under the pressure of 30-50MPa to obtain the curcumin emulsion.
Further limiting, the specific operation process of the step three is as follows:
dissolving carboxymethyl chitosan in deionized water, stirring for 30min, filtering with 0.22 μm syringe filter, adding glycerol into the filtrate, stirring for 2 hr, adding curcumin emulsion obtained in step two, and mixing at 5000rpm for 3 min.
Further limiting, the mass concentration of the carboxymethyl chitosan in the filtrate is 3-5%.
More specifically, the addition amount of the glycerol is 30% of the mass of the carboxymethyl chitosan, and the addition amount of the curcumin emulsion is 40-60% of the mass of the carboxymethyl chitosan.
Further limiting, the specific operation process of the step four is as follows:
pouring 20mL of film-forming dispersion into a silica gel plate with the size of 8.0 multiplied by 8.0cm, preparing a film by adopting a solution casting method, drying in an oven at the temperature of 40-60 ℃ for 10-15h, cooling to room temperature, uncovering the film, and placing in a constant temperature and humidity box for balancing for 12 h.
The invention has the following beneficial effects: the invention uses natural soybean oil to stabilize curcumin emulsion, improves the stability of curcumin, compounds natural edible biological macromolecule carboxymethyl chitosan and glycerol as a plasticizer, prepares a film by a solution casting method, has good mechanical property and moisture and oxygen resistance, delays the deterioration of products and ensures the quality and safety of food. In addition, the invention also has the following advantages:
(1) the prepared curcumin emulsion composite carboxymethyl chitosan-based film with stable soybean oil body has the film thickness of 172.3 mu m, the tensile strength of 2.44Mpa, the elongation at break of 53.22 percent and the water vapor permeability of 1.25 multiplied by 10-11(g·m-1·s-1·Pa-1) Oxygen permeability of 1.36X 10-3(g·m-1·s-1·Pa-1) The waterproof performance is good, the oxidation resistance is strong, and the antibacterial performance is certain;
(2) the invention takes soybean oil body as a natural emulsifier, the unique structure and specific components (phospholipid and protein) of the soybean oil body can form a protective coating by absorbing oleosin and phospholipid on the interface of liquid drops, used for stabilizing curcumin emulsion, and also has the advantages of improving the stability by enhancing the electrostatic repulsion force between droplets with the same surface charge, avoiding using some micromolecule surfactants such as Tween 80 and the like, simultaneously, the emulsion is added into the carboxymethyl chitosan film-forming solution to develop an emulsion film, the defects of poor water resistance, poor oxidation resistance and the like of a pure carboxymethyl chitosan film are overcome, the characteristics of a lipid compound and a hydrocolloid compound are linked to provide effective and controllable barrier characteristics, the preparation method of the film is simple, easy to operate, biodegradable, biocompatible, low in cost and free of pollution, and can be applied to packaging and fresh-keeping of food;
(3) the oil body is rich in components which are beneficial to human health, such as polyunsaturated fatty acid, phytosterol, tocopherol, carotenoid, oil body protein and the like, curcumin also provides antioxidant and antibacterial activity, carboxymethyl chitosan has strong film forming property, biocompatibility, degradability, antibacterial property and nontoxicity, and the prepared film can be applied to packaging and fresh-keeping of food, has the effects of delaying product deterioration and prolonging shelf life, and ensures the quality and safety of the food.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Example 1:
(1) soaking soybeans in deionized water at a feed-to-liquid ratio of 1:5(w/v) at 4 ℃ for 18 h. Grinding the soaked soybeans in a tissue crusher for 8min, wherein the material-liquid ratio of the soybeans to deionized water is 1:9 (w/v). Removing bean dregs from the pulverized mixture by passing through three layers of absorbent gauze, and collecting the filtrate. Sucrose was mixed with the filtrate at a 1:4(w/v) feed-to-liquid ratio and stirred in an ice-water bath for 10min, adjusted to pH 7.0 with 1M NaOH, and centrifuged at 25000 Xg for 30min at 4 ℃ to collect the upper cream layer rich in soybean oil bodies.
(2) For further purification of soybean oil bodies, the upper layer collected in step (1) was dissolved in a 20% (w/w) sucrose solution at a feed-to-liquid ratio of 1:8(w/v) and the pH was adjusted to 7.0 again, and then centrifuged at 25000 Xg for 30min at 4 ℃ to collect the upper layer soybean oil bodies, and this step (2) was repeated once.
(3) And (3) dissolving the purified oil body collected in the step (2) in deionized water according to the feed-liquid ratio of 1:8(w/v), adjusting the pH value to 7.0, centrifuging at 25000 Xg for 30min at 4 ℃, and taking the supernatant to obtain the soybean oil body.
(4) And (3) uniformly dispersing the soybean oil body extracted in the step (3) in deionized water, wherein the concentration of the soybean oil body in a water phase reaches 10% (w/w), curcumin is dissolved in the soybean oil through magnetic stirring, the concentration of the curcumin in an oil phase reaches 0.10% (w/w), the mixing ratio of the oil phase and the water phase is 2:8(w/w), homogenizing and mixing are carried out for 3min by a homogenizer at the speed of 5000rpm, and the emulsion is homogenized and circulated for 2 times under the homogenizing pressure of 40MPa by a high-pressure homogenizer, so that the curcumin emulsion with stable soybean oil body is obtained.
(5) Dissolving carboxymethyl chitosan in deionized water, stirring for 30min, wherein the concentration of the carboxymethyl chitosan is 5% (w/w), filtering by using a 0.22-micron syringe filter, adding 30% (w/w) of pure glycerol (based on the mass of the carboxymethyl chitosan) as a plasticizer, stirring for 2h, then adding 60% (w/w, based on the mass of the carboxymethyl chitosan) curcumin emulsion into the carboxymethyl chitosan film-forming solution, and mixing for 3min at the speed of 5000 rpm.
(6) The prepared film-forming dispersion was degassed by treatment at 300W for 5min in an ultrasonic cleaner. 20mL of the film-forming dispersion was poured into a silica gel plate (8.0X 8.0cm), and a film was prepared by a solution casting method. Drying in a 50 ℃ oven for 10h to form a film, cooling to room temperature, uncovering the film, and placing in a constant temperature and humidity box for balancing for 12 h.
Example 2:
(1) soaking soybeans in deionized water at a feed-to-liquid ratio of 1:5(w/v) at 4 ℃ for 18 h. Grinding the soaked soybeans in a tissue crusher for 8min, wherein the material-liquid ratio of the soybeans to deionized water is 1:9 (w/v). Removing bean dregs from the pulverized mixture by passing through three layers of absorbent gauze, and collecting the filtrate. Sucrose was mixed with the filtrate at a 1:4(w/v) feed-to-liquid ratio and stirred in an ice-water bath for 10min, adjusted to pH 9.0 with 1M NaOH, and centrifuged at 25000 Xg for 30min at 4 ℃ to collect the upper cream layer rich in soybean oil bodies.
(2) For further purification of soybean oil bodies, the upper layer collected in step (1) was dissolved in a 20% (w/w) sucrose solution at a feed-to-liquid ratio of 1:8(w/v) and the pH was adjusted to 9.0 again, and then centrifuged at 25000 Xg for 30min at 4 ℃ to collect the upper layer soybean oil bodies, and this step (2) was repeated once.
(3) And (3) dissolving the purified oil body collected in the step (2) in deionized water according to the feed-liquid ratio of 1:8(w/v), adjusting the pH value to 9.0, centrifuging at 25000 Xg for 30min at 4 ℃, and taking the supernatant to obtain the soybean oil body.
(4) And (3) uniformly dispersing the soybean oil body extracted in the step (3) in deionized water, wherein the concentration of the soybean oil body in a water phase reaches 15% (w/w), curcumin is dissolved in the soybean oil through magnetic stirring, the concentration of the curcumin in an oil phase reaches 0.10% (w/w), the mixing ratio of the oil phase and the water phase is 1:9(w/w), homogenizing and mixing are carried out for 3min by a homogenizer at the speed of 5000rpm, and the emulsion is homogenized and circulated for 2 times by a high-pressure homogenizer at the homogenizing pressure of 30MPa, so that the curcumin emulsion with stable soybean oil body is obtained.
(5) Dissolving carboxymethyl chitosan in deionized water, stirring for 30min, wherein the concentration of the carboxymethyl chitosan is 3% (w/w), filtering by using a 0.22-micron syringe filter, adding 30% (w/w) of pure glycerol (based on the mass of the carboxymethyl chitosan) as a plasticizer, stirring for 2h, then adding 40% (w/w, based on the mass of the carboxymethyl chitosan) curcumin emulsion into the carboxymethyl chitosan film-forming solution, and mixing for 3min at the speed of 5000 rpm.
(6) The prepared film-forming dispersion was degassed by treatment at 300W for 5min in an ultrasonic cleaner. 20mL of the film-forming dispersion was poured into a silica gel plate (8.0X 8.0cm), and a film was prepared by a solution casting method. Drying in a 40 ℃ oven for 15h to form a film, cooling to room temperature, uncovering the film, and placing in a constant temperature and humidity box for balancing for 12 h.
Example 3:
(1) soaking soybeans in deionized water at a feed-to-liquid ratio of 1:5(w/v) at 4 ℃ for 18 h. Grinding the soaked soybeans in a tissue crusher for 8min, wherein the material-liquid ratio of the soybeans to deionized water is 1:9 (w/v). Removing bean dregs from the pulverized mixture by passing through three layers of absorbent gauze, and collecting the filtrate. Sucrose was mixed with the filtrate at a 1:4(w/v) feed-to-liquid ratio and stirred in an ice-water bath for 10min, adjusted to pH 11.0 with 1M NaOH, and centrifuged at 25000 Xg for 30min at 4 ℃ to collect the upper cream layer rich in soybean oil bodies.
(2) For further purification of soybean oil bodies, the upper layer collected in step (1) was dissolved in a 20% (w/w) sucrose solution at a feed-to-liquid ratio of 1:8(w/v) and the pH was adjusted to 11.0 again, and then centrifuged at 25000 Xg for 30min at 4 ℃ to collect the upper layer soybean oil bodies, and this step (2) was repeated once.
(3) And (3) dissolving the purified oil body collected in the step (2) in deionized water according to the feed-liquid ratio of 1:8(w/v), adjusting the pH value to 11.0, centrifuging at 25000 Xg for 30min at 4 ℃, and taking the supernatant to obtain the soybean oil body.
(4) And (3) uniformly dispersing the soybean oil body extracted in the step (3) in deionized water, wherein the concentration of the soybean oil body in a water phase reaches 10% (w/w), curcumin is dissolved in the soybean oil through magnetic stirring, the concentration of the curcumin in an oil phase reaches 0.06% (w/w), the mixing ratio of the oil phase and the water phase is 2:8(w/w), homogenizing and mixing are carried out for 3min by a homogenizer at the speed of 5000rpm, and the emulsion is homogenized and circulated for 2 times under the homogenizing pressure of 50MPa by a high-pressure homogenizer, so that the curcumin emulsion with stable soybean oil body is obtained.
(5) Dissolving carboxymethyl chitosan in deionized water, stirring for 30min, wherein the concentration of the carboxymethyl chitosan is 5% (w/w), filtering by using a 0.22-micron syringe filter, adding 30% (w/w) of pure glycerol (based on the mass of the carboxymethyl chitosan) as a plasticizer, stirring for 2h, then adding 40% (w/w, based on the mass of the carboxymethyl chitosan) curcumin emulsion into the carboxymethyl chitosan film-forming solution, and mixing for 3min at the speed of 5000 rpm.
(6) The prepared film-forming dispersion was degassed by treatment at 300W for 5min in an ultrasonic cleaner. 20mL of the film-forming dispersion was poured into a silica gel plate (8.0X 8.0cm), and a film was prepared by a solution casting method. Drying in a 60 ℃ oven for 10h to form a film, cooling to room temperature, uncovering the film, and placing in a constant temperature and humidity box for balancing for 12 h.
Example 4:
(1) soaking soybeans in deionized water at a feed-to-liquid ratio of 1:5(w/v) at 4 ℃ for 18 h. Grinding the soaked soybeans in a tissue crusher for 8min, wherein the material-liquid ratio of the soybeans to deionized water is 1:9 (w/v). Removing bean dregs from the pulverized mixture by passing through three layers of absorbent gauze, and collecting the filtrate. Sucrose was mixed with the filtrate at a 1:4(w/v) feed-to-liquid ratio and stirred in an ice-water bath for 10min, adjusted to pH 11.0 with 1M NaOH, and centrifuged at 25000 Xg for 30min at 4 ℃ to collect the upper cream layer rich in soybean oil bodies.
(2) For further purification of soybean oil bodies, the upper layer collected in step (1) was dissolved in a 20% (w/w) sucrose solution at a feed-to-liquid ratio of 1:8(w/v) and the pH was adjusted to 11.0 again, and then centrifuged at 25000 Xg for 30min at 4 ℃ to collect the upper layer soybean oil bodies, and this step (2) was repeated once.
(3) And (3) dissolving the purified oil body collected in the step (2) in deionized water according to the feed-liquid ratio of 1:8(w/v), adjusting the pH value to 11.0, centrifuging at 25000 Xg for 30min at 4 ℃, and taking the supernatant to obtain the soybean oil body.
(4) And (3) uniformly dispersing the soybean oil body extracted in the step (3) in deionized water, wherein the concentration of the soybean oil body in a water phase reaches 5% (w/w), curcumin is dissolved in the soybean oil through magnetic stirring, the concentration of the curcumin in an oil phase reaches 0.10% (w/w), the mixing ratio of the oil phase and the water phase is 1:9(w/w), homogenizing and mixing are carried out for 3min by a homogenizer at the speed of 5000rpm, and the emulsion is homogenized and circulated for 2 times under the homogenizing pressure of 40MPa by a high-pressure homogenizer, so that the curcumin emulsion with stable soybean oil body is obtained.
(5) Dissolving carboxymethyl chitosan in deionized water, stirring for 30min, wherein the concentration of the carboxymethyl chitosan is 4% (w/w), filtering by using a 0.22-micron syringe filter, adding 30% (w/w) of pure glycerol (based on the mass of the carboxymethyl chitosan) as a plasticizer, stirring for 2h, then adding 60% (w/w, based on the mass of the carboxymethyl chitosan) curcumin emulsion into the carboxymethyl chitosan film-forming solution, and mixing for 3min at the speed of 5000 rpm.
(6) The prepared film-forming dispersion was degassed by treatment at 300W for 5min in an ultrasonic cleaner. 20mL of the film-forming dispersion was poured into a silica gel plate (8.0X 8.0cm), and a film was prepared by a solution casting method. Drying in a 50 ℃ oven for 10h to form a film, cooling to room temperature, uncovering the film, and placing in a constant temperature and humidity box for balancing for 12 h.
Comparative example 1:
the comparative example differs from example 1 in that: adding curcumin only into carboxymethyl chitosan film-forming solution
The method specifically comprises the following steps: dissolving carboxymethyl chitosan in deionized water, stirring for 30min, filtering with 0.22 μm syringe filter, adding pure glycerol as plasticizer, stirring for 2h, adding curcumin into carboxymethyl chitosan film-forming solution, mixing at 5000rpm for 3min, and degassing by treating the prepared film-forming dispersion in an ultrasonic cleaner at 300W for 5 min. 20mL of the film-forming dispersion was poured into a silica gel plate (8.0X 8.0cm), and a film was prepared by a solution casting method. Drying in a 60 ℃ oven for 10h to form a film, cooling to room temperature, uncovering the film, and placing in a constant temperature and humidity box for balancing for 12 h. The proportion of carboxymethyl chitosan, plasticizer and curcumin in the film forming dispersion in this comparative example was guaranteed to be the same as in example 1.
Comparative example 2:
the comparative example differs from example 1 in that: only adding soybean oil into carboxymethyl chitosan film-forming liquid
The method specifically comprises the following steps: dissolving carboxymethyl chitosan in deionized water, stirring for 30min, filtering with 0.22 μm syringe filter, adding pure glycerol as plasticizer, stirring for 2h, adding soybean oil into carboxymethyl chitosan film-forming solution, mixing at 5000rpm for 3min, and degassing by treating the prepared film-forming dispersion in an ultrasonic cleaner at 300W for 5 min. 20mL of the film-forming dispersion was poured into a silica gel plate (8.0X 8.0cm), and a film was prepared by a solution casting method. Drying in a 60 ℃ oven for 10h to form a film, cooling to room temperature, uncovering the film, and placing in a constant temperature and humidity box for balancing for 12 h. The proportion of carboxymethyl chitosan, plasticizer and soybean oil in the film-forming dispersion in this comparative example was the same as in example 1.
Comparative example 3:
the comparative example differs from example 1 in that: soy protein isolate was used in place of soy oil bodies and the remaining operating steps and parameters were the same as in example 1.
The films obtained in the above examples and comparative examples were subjected to conventional physicochemical indexes, oxidation resistance and antibacterial activity tests, and the test results are shown in the following tables:
table 1 shows the comparison of the physical and chemical indexes of the examples and the control group
As can be seen from Table 1, the products obtained in examples 1 to 4 have good mechanical properties and moisture and oxygen barrier properties, which are superior to those of comparative example 1. Control 1 shows that the incorporation of the emulsion increases the thickness of the dried film, and due to the presence of the oil phase, the film reduces the hydroxyl bonding between the polysaccharide and the water molecules, reduces the diffusion of the water molecules through the film, increases the barrier properties thereof, and thus forms a more water-resistant film, and the compatibility of the film matrix with the oil phase results in a dense structure, making it more difficult for nonpolar oxygen molecules to enter the film. In example 2 and example 4, the thickness of the film is small due to the small addition amount of carboxymethyl chitosan group and the low concentration of water-phase soybean oil body, the mechanical property and the water vapor permeability of the film are influenced by the thickness, and the film shows low mechanical property and high water vapor permeability. In the control group 2, only the carboxymethyl chitosan group was added to the soybean oil body, and the decrease in the oil content resulted in higher water vapor permeability and oxygen permeability. The control group 3 shows that the effect of the soy oil body for stabilizing the curcumin emulsion is better than that of the soy protein isolate, so that the oil phase is better present in the film, and the phase separation in the system is avoided.
Table 2 compares the antioxidant results of each example with the control group.
As can be seen from table 2, examples 1 to 4 have better antioxidant ability than control 2, compared with controls 1 and 3, the addition of curcumin improved the antioxidant activity of the film, and the soybean oil body improved the stability of the curcumin emulsion, and is a novel carrier for lipophilic bioactive molecules.
Table 3 shows the results of the zone of inhibition test for each example and the control group.
| Experimental group (antibacterial ring) | Staphylococcus aureus | Bacillus subtilis | Escherichia coli |
| Example 1(mm) | 11.77±0.64 | 11.40±0.57 | 9.50±0.55 |
| Example 2(mm) | 8.39±0.67 | 7.57±0.64 | 7.12±0.73 |
| Example 3(mm) | 9.71±0.71 | 8.77±0.63 | 8.49±0.54 |
| Example 4(mm) | 9.26±0.66 | 8.29±0.63 | 7.63±0.62 |
| Control group 1(mm) | 7.22±0.43 | 6.22±0.69 | 5.91±0.79 |
| Control group 2(mm) | 5.58±0.58 | 4.79±0.30 | 4.60±0.45 |
| Control group 3(mm) | 8.39±0.43 | 7.57±0.24 | 7.29±0.28 |
As can be seen from Table 3, the products obtained in examples 1 to 4 had a larger zone of inhibition and a better effect of inhibition than those of the control groups 1 to 3. In the absence of curcumin, the antibacterial activity of the membrane is low in the control group 2, and the antibacterial activity of curcumin is derived from the capability of decomposing cell membranes, so that the membrane can release cytoplasm, destroy organelles and infect the life activities of cells, and the antibacterial property of the membrane is improved. And because of the protection of the soybean oil body, the film prepared by the curcumin-loaded soybean oil body emulsion has higher antibacterial activity. In general, the antibacterial activity of the film against gram-positive bacteria (staphylococcus aureus, bacillus subtilis) is stronger than that of gram-negative bacteria (escherichia coli), and because the cell structure of gram-negative bacteria is more complex than that of gram-positive bacteria, the existence of the outer film provides an additional permeation barrier with stronger resistance, thereby being more beneficial to protecting the film from the external environment.
Claims (10)
1. A method for preparing an emulsion film is characterized by comprising the following steps: firstly adopting soybean oil to stabilize curcumin emulsion, then compounding carboxymethyl chitosan, and finally taking glycerin as a plasticizer to prepare the curcumin emulsion by a solution casting method.
2. The method of claim 1, comprising the steps of:
step one, preparing soybean oil body;
step two, dispersing the soybean oil body obtained in the step one in deionized water to be used as a water phase, dissolving curcumin in the soybean oil to be used as an oil phase, mixing the oil phase and the water phase, and then homogenizing to obtain curcumin emulsion;
dissolving carboxymethyl chitosan in deionized water, filtering, adding glycerol, stirring, adding curcumin emulsion, stirring, mixing, and degassing in an ultrasonic cleaning instrument to obtain a film-forming dispersion, wherein the ultrasonic intensity is 300W, and the ultrasonic treatment time is 3 min;
and step four, preparing the film-forming dispersion obtained in the step three into a film by adopting a solution casting method, drying and cooling the film to room temperature, uncovering the film, and placing the film in a constant temperature and humidity chamber for balancing to obtain the emulsion film.
3. The method for preparing an emulsion film according to claim 1, wherein the specific operation process of the first step is as follows:
(1) soaking soybeans in deionized water at 4 ℃ for 18h, wherein the ratio of the soaked soybeans to the deionized water is 1:9 grinding the mixture in a tissue crusher for 8min after mixing, removing bean dregs from the ground mixture through three layers of absorbent gauze, and collecting filtrate;
(2) mixing sucrose and the filtrate obtained in step (1), stirring in ice water bath for 10min, adjusting pH to 7.0-11.0 with 1mol/L NaOH, centrifuging at 25000 Xg below 4 deg.C for 30min, and collecting upper layer cream;
(3) dissolving the upper layer cream collected in the step (2) in a sucrose solution with the mass fraction of 20% according to the feed-liquid ratio of 1:8, adjusting the pH value to 7.0-11.0 by using 1mol/L NaOH, centrifuging for 30min under the conditions of 25000 Xg and below 4 ℃, collecting upper layer purified oil bodies, and repeating the step once;
(4) dissolving the purified oil body obtained in the step (3) in deionized water according to the feed-liquid ratio of 1:8, adjusting the pH value to 7.0-11.0, centrifuging for 30min at the temperature of below 4 ℃ and under the condition of 25000 Xg, and collecting the upper layer substance to obtain the soybean oil body.
4. The method for preparing an emulsion film according to claim 3, wherein the ratio of the soybean to the deionized water in the step (1) is 1: 5.
5. The method for preparing an emulsion film according to claim 3, wherein the ratio of sucrose to filtrate in step (2) is 1: 4.
6. The method for preparing an emulsion film according to claim 1, wherein the specific operation process of the second step is as follows:
dispersing the soybean oil body obtained in the step one in deionized water, so that the mass concentration of the soybean oil body in the water phase is 5-15%, the mass concentration of curcumin in the oil phase is 0.06-0.10%, and the mass ratio of the oil phase to the water phase is (1-2): (8-9), homogenizing and mixing for 3min by a homogenizer at the speed of 5000rpm, and finally homogenizing and circulating for 2 times by a high-pressure homogenizer under the pressure of 30-50MPa to obtain the curcumin emulsion.
7. The method for preparing an emulsion film according to claim 1, wherein the specific operation process of the third step is as follows:
dissolving carboxymethyl chitosan in deionized water, stirring for 30min, filtering with 0.22 μm syringe filter, adding glycerol into the filtrate, stirring for 2 hr, adding curcumin emulsion obtained in step two, and mixing at 5000rpm for 3 min.
8. The method of claim 7, wherein the carboxymethyl chitosan is present in the filtrate in a concentration of 3 to 5% by mass.
9. The method for preparing an emulsion film according to claim 7, wherein the glycerol is added in an amount of 30% by mass of the carboxymethyl chitosan, and the curcumin emulsion is added in an amount of 40-60% by mass of the carboxymethyl chitosan.
10. The method for preparing an emulsion film according to claim 1, wherein the specific operation process of the fourth step is as follows:
pouring 20mL of film-forming dispersion into a silica gel plate with the size of 8.0 multiplied by 8.0cm, preparing a film by adopting a solution casting method, drying in an oven at the temperature of 40-60 ℃ for 10-15h, cooling to room temperature, uncovering the film, and placing in a constant temperature and humidity box for balancing for 12 h.
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| CN108728235A (en) * | 2018-06-20 | 2018-11-02 | 东北农业大学 | A kind of extracting method of the soybean grease body with high oxidative stability |
| CN109349360A (en) * | 2018-09-29 | 2019-02-19 | 东北农业大学 | A kind of preparation method of high stability functional latex |
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