CN112831069A - Pectin-alginic acid composite preservative film and preparation and application thereof - Google Patents
Pectin-alginic acid composite preservative film and preparation and application thereof Download PDFInfo
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- CN112831069A CN112831069A CN201911156350.6A CN201911156350A CN112831069A CN 112831069 A CN112831069 A CN 112831069A CN 201911156350 A CN201911156350 A CN 201911156350A CN 112831069 A CN112831069 A CN 112831069A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
- C08J2305/04—Alginic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08J2305/06—Pectin; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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Abstract
The invention relates to a preparation method and application of a food biological preservative film taking pectin, alginic acid, chitosan and other natural polysaccharide materials as base materials. The method is characterized in that pectin and alginic acid are used as raw materials, and chitosan is crosslinked by an electrostatic complexation method to prepare the composite hydrogel biological preservative film. The method has simple preparation process and green and environment-friendly process; the obtained composite gel film has good water vapor transmission rate and light transmission, good mechanical tension and tensile tension performance, high biological safety, water solubility, degradability and other characteristics, is convenient to use, is easy to remove and has no residue; can effectively prolong the fresh-keeping time of the fruits and reduce the loss of water and nutrition of the fruits in the transportation and storage processes.
Description
Technical Field
The invention relates to a preparation method and application of a food biological preservative film taking pectin, alginic acid, chitosan and other natural polysaccharide materials as base materials. The method is characterized in that pectin and alginic acid are used as raw materials, and chitosan is crosslinked by an electrostatic complexation method to prepare the composite hydrogel biological preservative film. The method has simple preparation process and green and environment-friendly process; the obtained composite gel film has good water vapor transmission rate and light transmission, good mechanical tension and tensile tension performance and high biological safety, can effectively improve the fresh-keeping time of fruits, and reduces the loss of water and nutrition in the transportation process of fruits, meat and other foods. The high-molecular preservative film has the characteristics of water solubility, degradability, convenient use, simple removal, no residue and the like.
Background
Pectin is a heteropolysaccharide widely existing in cell walls of terrestrial higher plants, alginic acid is a natural polysaccharide derived from brown algae, and both polysaccharides have good biocompatibility and can form gel with low-valence cations through electrostatic complexation, so that the pectin is commonly used as an additive such as a thickening agent, a stabilizer, an emulsifier, a suspending agent and the like in the fields of biological medicines, foods, cosmetics and the like. In addition, pectin can also be used as a carrier material for targeting preparations, gene vectors and the like in the field of biomedicine. In recent years, pectin and alginic acid have good water retention due to their film-forming and gel-forming properties, and are widely used in food processing, packaging, fresh-keeping, and the like.
Due to the source, molecular characteristics and other reasons, the pectin has good water retention property and mechanical property after being crosslinked with low-valent cations, but due to the irregular spatial distribution of branched chain structures in molecules, the formed gel film has poor toughness and is easy to break and break. If other water-soluble polysaccharide substances such as alginic acid and the like are introduced, the toughness of the pectin film can be improved, and the mechanical property of the film can be improved. In addition, through blending with pectin, the problems of large porosity, poor water resistance, poor membrane mechanical property and the like of the alginic acid gel are further improved. In addition, the pectin material has good emulsifying property and stability, and is beneficial to loading of the fresh-keeping active component rosemary. Therefore, the two materials can play a complementary and synergistic effect.
Chitosan is a polycationic polysaccharide extracted from shells of crustaceans (shrimp, crab, etc.) and is a linear block copolymer with different deacetylation degree. As the degree of deacetylation increases, the molecular chain of chitosan contains-NH2Increase of-CO in molecular chain with pectin and alginic acidThe more OH binding sites, the more gel formation is favored. In addition, the electropositivity of the chitosan is easy for the interaction of bacteria with negative electricity on the surface, and the metabolism of the bacteria is influenced so as to inhibit the growth of the bacteria.
Based on the method, the composite gel biological preservative film is prepared through the electrostatic complexation of the pectin alginic acid compound and the chitosan, and the composite film has good water retention property, film forming property and mechanical property; the rosemary and the chitosan play a synergistic role, so that the barrier and antibacterial properties of the preservative film are improved. The biological membrane has the advantages of simple preparation, safety, no toxicity, controllable degradation and the like.
Disclosure of Invention
The invention relates to a preparation method and application of a food biological preservative film taking pectin, alginic acid, chitosan and other natural polysaccharide materials as base materials. The method is characterized in that pectin and alginic acid are used as raw materials, and chitosan is crosslinked by an electrostatic complexation method to prepare the composite hydrogel biological preservative film. The method has simple preparation process and green and environment-friendly process; the obtained composite gel film has good water vapor transmission rate and light transmission, good mechanical tension and tensile tension performance and high biological safety, can effectively improve the fresh-keeping time of fruits, and reduces the loss of water and nutrition in the transportation process of the fruits. The high-molecular preservative film has the characteristics of water solubility, degradability and the like, is convenient to use and simple to remove, and has no residue.
In order to realize the aim, the invention discloses a preparation method of a composite hydrogel biological preservative film taking pectin, alginic acid and chitosan as basic materials, which is characterized by comprising the following steps: the method sequentially comprises the following steps:
(1) weighing pectin and alginic acid powder respectively, dissolving in water, swelling, and stirring to dissolve completely; the mass concentration of the pectin is 0.2-4% (preferably 2%, 4% times), the molecular weight (Mw) is 5-20 kD (20kD is optimal, 15-18 kD is optimal), the esterification Degree (DE) is 18-40% (28% is optimal, 35% times), and the pectin is derived from one or more than two cell wall extracts of higher plants such as apples, oranges, dragon fruits, ginkgo biloba sarcotesta, grapefruit and the like; the mass concentration of alginic acid is 0.5-3%, and the content of a G (a-L-guluronic acid) structural unit is 25-55%;
(2) uniformly mixing the pectin solution prepared in the step (1) and alginic acid solution according to the volume ratio of 10: 1-1: 10(v/v), standing for more than 0.5 hour, and degassing to obtain mixed membrane liquid;
(3) and (3) adding a plasticizer into the mixed membrane liquid prepared in the step (2), and dropwise adding rosemary essential oil under the stirring condition of 100-500 rpm. After completely mixing, uniformly coating 1-2 mL of the mixture on a horizontal plate (10cm multiplied by 10cm), naturally salivating to be horizontally laid, standing for 5-20 min and drying;
(4) placing the glass plate obtained in the step (3) in a chitosan solution, crosslinking into a gel film, and drying at room temperature (20-25 ℃); the mass concentration of the chitosan is 0.2-1.5%, the Mw is 2.5-10 kDa, and the degree of deacetylation is more than or equal to 90%;
(5) and (4) uncovering the dried gel film prepared in the step (4).
The plasticizer in the step (3) is one or more than two of sorbitol, mannitol, glycerol, glycol, polyethylene glycol and ethyl succinate, and the volume concentration is 0.5-5%.
The volume concentration of the rosemary essential oil in the step (3) is 0.05-1.5%.
The crosslinking film-forming temperature in the step (4) is 25-37 ℃.
The polysaccharide biomembrane can be used for wrapping or covering, fresh-keeping and storing one or more than two kinds of foods of fruits, vegetables, aquatic products, meat and the like.
The invention has the following advantages:
1. the pectin and the alginic acid are used for preparing the composite biological membrane with ideal mechanical strength and ductility through complementary action;
2. the pectin and the alginic acid form hydrogel through electrostatic complexation, the process is green, no organic solvent is used, the three components are complementary through advantages, and the biological membrane has good water retention and antibacterial performance.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art and researchers in further understanding the present invention, but do not constitute any limitation to the present invention. Any modification made by anyone within the scope of the claims of the present invention is still within the scope of the claims of the present invention.
Example 1
(1) 1.5G of citrus pectin powder (Mw 2kDa, DE 28%) and 1.5G of alginic acid (G content 42%) were dissolved in 100ml of deionized water, respectively, and after sufficient swelling, they were stirred until completely dissolved.
(2) Respectively taking 5mL of pectin and alginic acid solution, and mixing the pectin and the alginic acid solution according to the weight ratio of 1:1 volume ratio was mixed completely.
(3) 2% glycerol was added to the mixture, 1mL rosemary was added dropwise under magnetic stirring at 300rpm, and the mixture was stirred until complete mixing. Standing, degassing, spreading 3mL of the solution on a glass plate, naturally salivating to horizontal spreading, and standing for 10 min.
(4) Slowly soaking the glass plate in 1% chitosan solution (Mw is 30kDa, degree of deacetylation is 95%), crosslinking for 8min, taking out, drying in a fume hood at room temperature, and removing the membrane.
(5) The biological membrane sterilized by ultraviolet radiation is cut into the size of 6mm in diameter, and sterile filter paper sheets and a PE membrane are used for comparison. The antibacterial activity of the biofilm against escherichia coli was determined in vitro by the antibacterial circle method (thesis of the university of tianjin science, ran by zuo ran, preparation and performance study of Chinese herbal medicine antibacterial membranes, 2017), and each experiment was repeated three times. After culturing for 24 hours, determining the inhibition zone, wherein the diameter of the inhibition zone of the composite hydrogel biological membrane is 2.84mm +/-0.31 mm, and no inhibition zone is generated in a control group, which shows that the biological membrane has good in-vitro antibacterial activity.
Example 2
(1) 2.5G of apple pectin powder (molecular weight 10kDa, DE ═ 35%) and 1.0G of alginic acid (G content 55%) were dissolved in 100ml of deionized water, respectively, and after sufficient swelling, they were stirred until completely dissolved.
(2) 5mL of pectin and alginic acid solution are respectively taken and mixed completely according to the volume ratio of 1: 3.
(3) 1.5% mannitol was added to the mixture, 1.5mL rosemary was added dropwise under magnetic stirring at 500rpm, and the mixture was stirred until complete mixing. Standing, degassing, spreading 3mL of the solution on a glass plate, naturally salivating to horizontal spreading, and standing for 5 min.
(4) Slowly soaking the glass plate in 0.5% chitosan solution (Mw is 85kDa, degree of deacetylation is more than 90%), crosslinking for 10min, taking out, drying in a fume hood at room temperature, and removing the membrane.
(5) And measuring the film thickness by using a micrometer, randomly selecting 5 sites on the same film, wherein the film thickness is uniform, and the average film thickness is 0.0258 +/-0.0019 mm.
Example 3
(1) 2.0G of citrus pectin powder (molecular weight 20kDa, DE ═ 30%) and 1.8G of alginic acid (G content 28%) were dissolved in 100ml of deionized water, respectively, and after sufficient swelling, they were stirred until completely dissolved.
(2) 5mL of pectin and alginic acid solution are respectively taken, and the weight ratio of the pectin to the alginic acid is 2: 1 volume ratio was mixed completely.
(3) 0.8% ethylene glycol was added to the mixture, 0.5mL of rosemary was added dropwise under magnetic stirring at 500rpm, and the mixture was stirred until complete mixing. Standing, degassing, spreading 3mL of the solution on a glass plate, naturally salivating to horizontal spreading, and standing for 5 min.
(4) Slowly soaking the glass plate in 1.5% chitosan solution (Mw is 60kDa, degree of deacetylation is more than 90%), crosslinking for 10min, taking out, drying in a fume hood at room temperature, and removing the membrane.
(5) And measuring the film thickness by using a micrometer, randomly selecting 5 sites on the same film, wherein the film thickness is uniform, and the average film thickness is 0.035 +/-0.003 mm.
Example 4
(1) 3.0G of citrus pectin powder (molecular weight 20kDa, DE ═ 20%) and 1.0G of alginic acid (G content 36%) were dissolved in 100ml of deionized water, respectively, and after sufficient swelling, they were stirred until completely dissolved.
(2) 5mL of pectin and 5mL of alginic acid solution are respectively taken and mixed completely according to the volume ratio of 5: 1.
(3) To the mixture was added 3% ethyl succinate, and 2mL rosemary was added dropwise under magnetic stirring at 400rpm, and the mixture was stirred until complete mixing. Standing, degassing, spreading 3mL of the solution on a glass plate, naturally salivating to horizontal spreading, and standing for 10 min.
(4) Slowly soaking the glass plate in 0.8% chitosan solution (Mw 80kDa, deacetylation degree > 95%), crosslinking for 15min, taking out, drying in a fume hood at room temperature, and removing the membrane.
(5) And measuring the film thickness by using a micrometer, randomly selecting 5 sites on the same film, wherein the film thickness is uniform, and the average film thickness is 0.027 +/-0.0025 mm. Measuring light transmittance of the film at 600nm wavelength by spectrophotometry, repeating for three times, and light transmittance is 87.48 + -3.79%
Example 5
The in vitro antioxidant performance of the bio-composite membranes prepared in examples 1-4 was evaluated by the method for determining DPPH free radical scavenging rate (see SEONG S.H., SEOG G.L., YONG C., et al. antioxidant activity of crop extract and pure compounds of Acer ginnala Mix, 2001,25(3): 389-. The results show that 4 samples with the same dosage have good in-vitro oxidation resistance, and the removal rate of DPPH free radicals of the samples in examples 1-4 is 30.74%, 32.16%, 28.53% and 30.6% in sequence. Through statistical analysis, the compositions prepared in examples 1-4 of each distributor have no significant difference in radical scavenging effect.
Example 6
Sodium chloride, magnesium chloride and magnesium nitrate are respectively placed in a glass vessel by a cup-like method, the distance between the glass vessel and a bottle opening is 1cm, a 3 x 3cm sample film of the embodiment 1-4 is covered on the bottle opening, and the bottle opening is fixed and weighed. The reagent bottles were placed in desiccators containing saturated sodium chloride, magnesium nitrate and magnesium chloride at relative humidities of 76% and 34%, respectively, and the weights were recorded after constant weight. The weight was then measured every 12h for 5 consecutive days, with each sample being weighed in triplicate. Alginic acid-chitosan membrane was used as a control. The water vapor transmission rate is calculated by the following equation:
WVP＝(Wa-Wb)/T/S
wherein WVP is the water vapor transmission coefficient (mg. m)-2d-1) Wa is the final weight of the weighing flask, Wb is the initial weight, T is the duration (h), S is the film area (m)2)。
The results showed that the water vapor transmission coefficients of the four films were 0.204, 0.251, 0.218 and 0.237mg · m, respectively, at a Relative Humidity (RH) of 76%-2d-1Each ofThere was no significant difference between the groups, and the water vapor transmission rate of the control group was 0.343mg · m-2d-1The composite biological membrane obviously improves the water retention effect (p) of the alginate gel membrane<0.05), can delay the water loss of fruits, vegetables and other foods and prolong the preservation time; the transmittance of the sample was 0.181, 0.168, 0.173, and 0.187 at 34% RH, respectively, and the control was 0.207, which showed no significant difference between the groups.
Claims (7)
1. A preparation method of a composite hydrogel biological preservative film taking pectin, alginic acid and chitosan as basic materials is characterized in that: the method sequentially comprises the following steps:
(1) weighing pectin and alginic acid powder respectively, dissolving in water, swelling, and stirring to dissolve completely; the mass concentration of the pectin is 0.2-4% (preferably 2%, 4% times), the molecular weight (Mw) is 5-20 kD (20kD is optimal, 15-18 kD is optimal), the esterification Degree (DE) is 18-40% (28% is optimal, 35% times), and the pectin is derived from one or more than two cell wall extracts of higher plants such as apples, oranges, dragon fruits, ginkgo biloba sarcotesta, grapefruit and the like; the mass concentration of alginic acid is 0.5-3%, and the content of a G (a-L-guluronic acid) structural unit is 25-55%;
(2) uniformly mixing the pectin solution prepared in the step (1) and alginic acid solution according to the volume ratio of 10: 1-1: 10(v/v), standing for more than 0.5 hour, and degassing to obtain mixed membrane liquid;
(3) adding rosemary essential oil and a plasticizer into the mixed membrane liquid prepared in the step (2), uniformly coating 1-2 mL of the mixed membrane liquid on a horizontal plate (10cm multiplied by 10cm), naturally salivating to be horizontally laid, standing for 5-20 min, and drying;
(4) placing the glass plate obtained in the step (3) in a chitosan solution, crosslinking into a gel film, and drying at room temperature (20-25 ℃); the mass concentration of the chitosan is 0.2-1.5%, the Mw is 2.5-10 kDa, and the degree of deacetylation is more than or equal to 90%;
(5) and (4) uncovering the dried gel film prepared in the step (4).
2. The method of claim 1, wherein: the plasticizer in the step (3) is one or more than two of sorbitol, mannitol, glycerol, ethylene glycol, polyethylene glycol and ethyl succinate.
3. The production method according to claim 1 or 2, characterized in that: the volume concentration of the plasticizer in the step (3) is 0.5-5%.
4. The method of claim 1, wherein: the volume concentration of the rosemary essential oil in the step (3) is 0.05-1.5%.
5. The method of claim 1, wherein: and (4) the crosslinking film-forming temperature in the step (4) is 25-37 ℃.
6. A pectin-alginic acid composite preservative film prepared by the preparation method of any one of claims 1 to 7.
7. The application of the pectin-alginic acid composite preservative film of claim 8, which is characterized in that: the polysaccharide biomembrane can be used for wrapping or covering, fresh-keeping and storing one or more than two kinds of foods of fruits, vegetables, aquatic products, meat and the like.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114369258A (en) * | 2021-12-22 | 2022-04-19 | 浙江大学台州研究院 | Hydrogel composite material, preparation method and application |
| WO2023123662A1 (en) * | 2021-12-27 | 2023-07-06 | 青岛农业大学 | Preparation method for edible and biodegradable tableware |
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| CN1508175A (en) * | 2002-12-13 | 2004-06-30 | 上海爱普食品工业有限公司 | Method for preparing composite comestible shell polysaccharide membrane |
| US20040137041A1 (en) * | 2003-01-09 | 2004-07-15 | Jakwang Co., Ltd. | Water-soluble natural film and its preparing method |
| CN104877180A (en) * | 2015-05-25 | 2015-09-02 | 苏州市贝克生物科技有限公司 | Water-soluble food packaging film and preparation method thereof |
| CN109294003A (en) * | 2018-09-03 | 2019-02-01 | 太原理工大学 | A kind of chitosan containing ZnO/sodium alginate antimicrobial preservative film and preparation method thereof |
-
2019
- 2019-11-22 CN CN201911156350.6A patent/CN112831069A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1508175A (en) * | 2002-12-13 | 2004-06-30 | 上海爱普食品工业有限公司 | Method for preparing composite comestible shell polysaccharide membrane |
| US20040137041A1 (en) * | 2003-01-09 | 2004-07-15 | Jakwang Co., Ltd. | Water-soluble natural film and its preparing method |
| CN104877180A (en) * | 2015-05-25 | 2015-09-02 | 苏州市贝克生物科技有限公司 | Water-soluble food packaging film and preparation method thereof |
| CN109294003A (en) * | 2018-09-03 | 2019-02-01 | 太原理工大学 | A kind of chitosan containing ZnO/sodium alginate antimicrobial preservative film and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114369258A (en) * | 2021-12-22 | 2022-04-19 | 浙江大学台州研究院 | Hydrogel composite material, preparation method and application |
| CN114369258B (en) * | 2021-12-22 | 2023-07-25 | 浙江大学台州研究院 | Hydrogel composite material, preparation method and application |
| WO2023123662A1 (en) * | 2021-12-27 | 2023-07-06 | 青岛农业大学 | Preparation method for edible and biodegradable tableware |
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Application publication date: 20210525 |