CN111286056B - Preparation method of nano antioxidant film - Google Patents
Preparation method of nano antioxidant film Download PDFInfo
- Publication number
- CN111286056B CN111286056B CN202010204190.4A CN202010204190A CN111286056B CN 111286056 B CN111286056 B CN 111286056B CN 202010204190 A CN202010204190 A CN 202010204190A CN 111286056 B CN111286056 B CN 111286056B
- Authority
- CN
- China
- Prior art keywords
- gelatin
- film
- nano
- glycerol
- preparation
- 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.)
- Active
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003963 antioxidant agent Substances 0.000 title claims description 20
- 230000003078 antioxidant effect Effects 0.000 title description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 80
- 239000008273 gelatin Substances 0.000 claims abstract description 75
- 229920000159 gelatin Polymers 0.000 claims abstract description 75
- 108010010803 Gelatin Proteins 0.000 claims abstract description 73
- 235000019322 gelatine Nutrition 0.000 claims abstract description 72
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 72
- 239000000243 solution Substances 0.000 claims abstract description 52
- 108010025899 gelatin film Proteins 0.000 claims abstract description 42
- 239000007788 liquid Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002131 composite material Substances 0.000 claims abstract description 33
- 239000007864 aqueous solution Substances 0.000 claims abstract description 31
- 229930003799 tocopherol Natural products 0.000 claims abstract description 27
- 239000011732 tocopherol Substances 0.000 claims abstract description 27
- GVJHHUAWPYXKBD-UHFFFAOYSA-N d-alpha-tocopherol Natural products OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229960001295 tocopherol Drugs 0.000 claims abstract description 26
- 235000010384 tocopherol Nutrition 0.000 claims abstract description 26
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000000265 homogenisation Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 229920000136 polysorbate Polymers 0.000 claims abstract description 16
- 230000003064 anti-oxidating effect Effects 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 239000004033 plastic Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 10
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 10
- 229920000053 polysorbate 80 Polymers 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000009423 ventilation Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000000527 sonication Methods 0.000 claims 1
- 239000012528 membrane Substances 0.000 abstract description 12
- 230000035699 permeability Effects 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 9
- 238000007254 oxidation reaction Methods 0.000 abstract description 9
- 235000013305 food Nutrition 0.000 abstract description 8
- 230000004888 barrier function Effects 0.000 abstract description 7
- 238000002604 ultrasonography Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 239000005003 food packaging material Substances 0.000 abstract description 4
- 235000013376 functional food Nutrition 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 235000011187 glycerol Nutrition 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000839 emulsion Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000003921 oil Substances 0.000 description 9
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 235000006708 antioxidants Nutrition 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 5
- 239000000341 volatile oil Substances 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 230000004071 biological effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007760 free radical scavenging Effects 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 230000006916 protein interaction Effects 0.000 description 1
- 230000004850 protein–protein interaction Effects 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000019149 tocopherols Nutrition 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- QUEDXNHFTDJVIY-UHFFFAOYSA-N γ-tocopherol Chemical class OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-UHFFFAOYSA-N 0.000 description 1
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
-
- 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
- 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
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- General Preparation And Processing Of Foods (AREA)
Abstract
本发明提供了一种纳米抗氧化膜的制备方法。技术方案以特定配比的明胶、甘油、生育酚、吐温、去离子水为原料,分别制备明胶‑甘油水性溶液及油性溶液,将二者混合后首先进行均质处理,得到复合明胶膜液,而后联合高压均质和超声对复合明胶膜液进行处理,使膜液同时受到来自高压均质的机械效应和来自超声的空化作用。高压均质产生的剪切力和超声空化作用产生的气泡,使复合明胶液中的油滴形成纳米颗粒,并均匀分散在溶液内部,由此而形成的纳米抗氧化明胶膜具有较高拉伸强度、断裂伸长率和光阻隔性,较低的膜厚和水蒸气透过性,且抗氧化性较高,能作为功能性的食品包装材料应用于食品工业中。
The invention provides a preparation method of a nanometer anti-oxidation film. The technical scheme uses gelatin, glycerol, tocopherol, Tween and deionized water in specific proportions as raw materials to prepare gelatin-glycerol aqueous solution and oily solution respectively, and after mixing the two, first perform homogenization treatment to obtain a composite gelatin film liquid , and then combined high-pressure homogenization and ultrasound to process the composite gelatin membrane liquid, so that the membrane liquid is simultaneously subjected to the mechanical effect from high-pressure homogenization and the cavitation from ultrasound. The shear force generated by high-pressure homogenization and the bubbles generated by ultrasonic cavitation make the oil droplets in the composite gelatin solution form nanoparticles and evenly disperse in the solution. Tensile strength, elongation at break and light barrier properties, low film thickness and water vapor permeability, and high oxidation resistance, can be used as functional food packaging materials in the food industry.
Description
技术领域technical field
本发明涉及明胶膜技术领域,具体涉及一种纳米抗氧化膜的制备方法。The invention relates to the technical field of gelatin films, in particular to a preparation method of a nanometer antioxidant film.
背景技术Background technique
近年来,可食用膜因其具有食用安全性、环境可降解性成为食品包装领域的热点。明胶是一种蛋白来源的生物材料,具有良好的成膜性和生物相容性。纯明胶膜的物理性能差,生物活性低,在拉伸强度、光阻隔性能、膜厚度、水蒸气透过性等方面均不够理想,而且其抗氧化性较差,因此,有必要对其进行改性以适应食品包装领域的工艺要求。In recent years, edible film has become a hot spot in the field of food packaging due to its edible safety and environmental degradability. Gelatin is a protein-derived biomaterial with good film-forming properties and biocompatibility. Pure gelatin films have poor physical properties, low biological activity, and are not ideal in terms of tensile strength, light barrier properties, film thickness, and water vapor permeability, and their oxidation resistance is poor. Modified to suit the process requirements in the food packaging field.
目前,制备抗氧化明胶膜的常用添加剂为精油,精油强烈的气味影响明胶膜在食品领域的应用;同时由于分散在明胶膜中油性成分(精油)颗粒较大,阻碍了蛋白-蛋白之间的相互作用,复合膜的机械性能和生物活性并没有发挥到最佳状态。At present, the commonly used additive for preparing antioxidant gelatin film is essential oil, and the strong odor of essential oil affects the application of gelatin film in the food field; at the same time, due to the large particles of oily components (essential oils) dispersed in the gelatin film, it hinders the protein-protein interaction. The mechanical properties and biological activities of the composite membranes did not reach the optimum state due to the interaction.
发明内容SUMMARY OF THE INVENTION
本发明旨在针对现有技术的技术缺陷,提供一种纳米抗氧化膜的制备方法,以解决现有技术中,常规明胶膜物理性能有待提升的技术问题。The present invention aims to provide a method for preparing a nano-antioxidation film in view of the technical defects of the prior art, so as to solve the technical problem in the prior art that the physical properties of conventional gelatin films need to be improved.
本发明要解决的另一技术问题是,常规明胶膜抗氧化性较差。Another technical problem to be solved by the present invention is that the conventional gelatin film has poor oxidation resistance.
本发明要解决的再一技术问题是,如何在实现明胶膜抗氧化性的同时避免引入精油的突出气味。Another technical problem to be solved by the present invention is how to avoid the introduction of the prominent odor of essential oils while achieving the anti-oxidation property of the gelatin film.
为实现以上技术目的,本发明采用以下技术方案:To achieve the above technical purpose, the present invention adopts the following technical solutions:
一种纳米抗氧化膜的制备方法,包括以下步骤:A preparation method of nano anti-oxidation film, comprising the following steps:
1)以如下重量百分比的成分为配方:明胶8%,甘油1%,生育酚4%,吐温0.8%,去离子水余量;1) formula with the following composition by weight: gelatin 8%, glycerol 1%,
2)取配方量的明胶和水混合,在60℃下溶解90min,期间持续搅拌,直至明胶完全溶解;2) Mix the gelatin of the formula with water, dissolve at 60°C for 90min, and continue stirring during this period until the gelatin is completely dissolved;
3)将步骤2)所得的明胶溶液冷却至室温,向其中加入配方量的甘油,混合均匀,得到明胶-甘油水性溶液;3) cooling the gelatin solution obtained in step 2) to room temperature, adding the glycerol of the formula amount to it, and mixing evenly to obtain a gelatin-glycerol aqueous solution;
4)将配方量的生育酚和吐温混合,利用振荡器充分震荡,得到油性溶液;4) mix the tocopherol and Tween of the formula amount, and fully shake the oscillator to obtain an oily solution;
5)将步骤3)所得的明胶-甘油水性溶液与步骤4)所得的油性溶液混合,用均质机在13000rpm的条件下均质处理3min,得到复合明胶膜液;5) mixing the gelatin-glycerol aqueous solution obtained in step 3) with the oily solution obtained in step 4), and homogenizing for 3 min with a homogenizer under the condition of 13000 rpm to obtain a composite gelatin film liquid;
6)将步骤5)所得的复合明胶膜液(也可称之为明胶乳液)在80~100MPa的高压均质条件下进行混合6) Mix the composite gelatin film liquid (also known as gelatin emulsion) obtained in step 5) under high pressure homogenization conditions of 80-100 MPa
7)将步骤6)混合后的产物在400~600w的条件下超声处理10min,得到成膜前的膜液;7) ultrasonically treating the mixed product in step 6) for 10 minutes under the condition of 400-600w to obtain the film liquid before film formation;
8)用步骤7)所得的成膜前的膜液进行成膜。8) Perform film formation with the film liquid before film formation obtained in step 7).
作为优选,步骤8)中所述的进行成膜,包括:将所述成膜前的膜液倒入平皿中,在室温通风条件下干燥48h;将干燥后的膜放入相对湿度为50%的密闭环境平衡24h,揭下后即得到所述纳米抗氧化膜。Preferably, the film formation described in step 8) includes: pouring the film liquid before film formation into a plate, drying at room temperature for 48 hours under ventilation conditions; placing the dried film in a relative humidity of 50% The airtight environment was equilibrated for 24h, and the nano-antioxidant film was obtained after peeling off.
作为优选,所述平皿为90mm×90mm的塑料平皿,成膜前的膜液向平皿中的倒入量为4mL。Preferably, the plate is a plastic plate of 90mm×90mm, and the amount of the film liquid poured into the plate before film formation is 4mL.
作为优选,所述吐温为吐温80。Preferably, the Tween is Tween 80.
作为优选,步骤1)及步骤2)中所述明胶的冻力为260~270。Preferably, the freezing force of the gelatin in steps 1) and 2) is 260-270.
作为优选,步骤2)中,在所述溶解的过程中,用保鲜膜持续封闭容器的端口(用于防止长时间的加热过程使溶液水分挥发,影响溶液中明胶的浓度)。Preferably, in step 2), during the dissolving process, the port of the container is continuously closed with a plastic wrap (to prevent the long-term heating process from volatilizing the water in the solution and affecting the concentration of gelatin in the solution).
作为优选,步骤6)中高压循环次数为3次。Preferably, the number of high-pressure cycles in step 6) is 3 times.
作为优选,步骤7)所述的超声处理,是利用超声波破碎仪实现的,频率为20kHz,选择6mm的变幅杆,每超声处理2s,停止2s。Preferably, the ultrasonic treatment described in step 7) is realized by using an ultrasonic crusher, the frequency is 20 kHz, the horn of 6 mm is selected, and the ultrasonic treatment is stopped for 2 s every 2 s.
作为优选,所述干燥48h,是在温度25±2℃、相对湿度50±5%的条件下进行的。Preferably, the drying for 48 hours is carried out under the conditions of a temperature of 25±2° C. and a relative humidity of 50±5%.
本发明提供了一种纳米抗氧化膜的制备方法。技术方案以特定配比的明胶、甘油、生育酚、吐温、去离子水为原料,分别制备明胶-甘油水性溶液及油性溶液,将二者混合后首先进行均质处理,得到复合明胶膜液,而后联合高压均质和超声对复合明胶膜液进行处理,使膜液同时受到来自高压均质的机械效应和来自超声的空化作用。高压均质产生的剪切力和超声空化作用产生的气泡,使复合明胶液中的油滴形成纳米颗粒,并均匀分散在溶液内部,由此而形成的纳米抗氧化明胶膜具有较高拉伸强度、断裂伸长率和光阻隔性,较低的膜厚和水蒸气透过性,且抗氧化性较高,能作为功能性的食品包装材料应用于食品工业中。The invention provides a preparation method of a nanometer anti-oxidation film. The technical scheme uses gelatin, glycerol, tocopherol, Tween, and deionized water in specific proportions as raw materials to prepare gelatin-glycerol aqueous solution and oily solution, respectively, after mixing the two, first perform homogenization treatment to obtain composite gelatin film liquid , and then combined high-pressure homogenization and ultrasound to process the composite gelatin membrane fluid, so that the membrane fluid is simultaneously subjected to mechanical effects from high-pressure homogenization and cavitation from ultrasound. The shear force generated by high-pressure homogenization and the bubbles generated by ultrasonic cavitation make the oil droplets in the composite gelatin solution form nanoparticles and evenly disperse in the solution. The nano-antioxidant gelatin film thus formed has high tensile strength Tensile strength, elongation at break and light barrier properties, low film thickness and water vapor permeability, and high oxidation resistance, can be used as functional food packaging materials in the food industry.
为改善纯明胶膜的性能,在明胶膜的制备过程中添加油性成分的生育酚,能增强膜的断裂伸长率和光阻隔性,同时明胶膜的抗氧化性也因生育酚的加入而增强;与此同时,复合膜的物理性能和生物活性受到油性颗粒(生育酚)尺寸和分布的影响,通过高压均质和超声辅助制备纳米级别的复合膜,纳米复合膜的物理性能和生物活性得到进一步增强。In order to improve the performance of pure gelatin film, adding oily tocopherol in the preparation process of gelatin film can enhance the elongation at break and light barrier property of the film, and the antioxidant property of the gelatin film is also enhanced by the addition of tocopherol; At the same time, the physical properties and biological activities of the composite membranes are affected by the size and distribution of oily particles (tocopherols). By preparing nano-scale composite membranes by high pressure homogenization and ultrasonic assistance, the physical properties and biological activities of the nanocomposite membranes are further improved. enhanced.
该方法制备的纳米抗氧化膜没有令人不悦的突出气味,同时具有较好的机械性能、防水性能和光阻隔性能,抗氧化性也比非纳米级别的抗氧化性膜高,能作为一种功能性的食品包装材料应用在食品工业领域。The nano-antioxidant film prepared by the method has no unpleasant and prominent odor, and has good mechanical properties, waterproof performance and light blocking performance, and the anti-oxidation property is also higher than that of the non-nano-level anti-oxidation film, which can be used as a kind of anti-oxidation film. Functional food packaging materials are used in the food industry.
本发明的有益效果集中体现在以下方面:本发明通过高压均质和超声结合制备纳米油滴颗粒,从而对复合明胶膜的形成产生以下几种影响:1.纳米级别的油滴颗粒在明胶膜内部均匀分布,有利于形成较低膜厚的膜;2.纳米级别的油滴颗粒尺寸很小,减少了明胶蛋白-蛋白之间的阻碍作用,使蛋白-蛋白之间的相互作用增强,从而增加了明胶膜的拉伸强度和断裂伸长率;3.纳米级别的油滴颗粒使油滴的散色能力增强,从而增强了膜对光的阻隔能力;4.纳米级别的油滴颗粒使油滴的比表面积增大,使水蒸气分子透过膜的难度增大、生育酚油滴颗粒与氧化物质接触的面积增大,从而使膜的水蒸气透过性降低、抗氧化性增强。本发明可以作为食品包装领域的功能性材料。The beneficial effects of the present invention are embodied in the following aspects: the present invention prepares the nano oil droplet particles through the combination of high pressure homogenization and ultrasound, thereby producing the following effects on the formation of the composite gelatin film: The inside is uniformly distributed, which is conducive to the formation of a lower film thickness; 2. The nano-scale oil droplets are small in size, which reduces the hindrance between gelatin protein and protein, and enhances the interaction between protein and protein. Increase the tensile strength and elongation at break of the gelatin film; 3. Nano-scale oil droplet particles enhance the dispersive ability of oil droplets, thereby enhancing the film's blocking ability to light; 4. Nano-scale oil droplet particles make The increase of the specific surface area of the oil droplets makes it more difficult for water vapor molecules to pass through the membrane, and the contact area between the tocopherol oil droplet particles and oxidizing substances increases, thereby reducing the water vapor permeability of the membrane and enhancing the oxidation resistance. The present invention can be used as a functional material in the field of food packaging.
与普通复合膜的制备方法相比,本发明能大大降低表面活性的使用量,产品安全系数高;与常规抗氧化明胶膜的制备方法相比,本发明使用生育酚作为抗氧化材料,避免了由常规抗氧化剂(精油)的突出气味对明胶膜造成的不良影响;与传统复合明胶膜的产品性能相比,本发明方法制备的纳米抗氧化性明胶膜具有较高的拉伸强度和光阻隔性能,较低的膜厚和水蒸气透过性,抗氧化性较高,提升了复合明胶膜的功能性及其应用价值。Compared with the preparation method of the common composite film, the present invention can greatly reduce the amount of surface activity used, and the product safety factor is high; The adverse effect caused by the prominent odor of conventional antioxidants (essential oils) on the gelatin film; compared with the product properties of the traditional composite gelatin film, the nano-antioxidative gelatin film prepared by the method of the present invention has higher tensile strength and light blocking performance , lower film thickness and water vapor permeability, and higher oxidation resistance, which improves the functionality and application value of the composite gelatin film.
附图说明Description of drawings
图1是本发明具体实施方式中,各实施例及对比例所得复合明胶膜抗氧化性的对比图。FIG. 1 is a comparison diagram of the oxidation resistance of the composite gelatin films obtained by each example and a comparative example in the specific embodiment of the present invention.
具体实施方式Detailed ways
以下将对本发明的具体实施方式进行详细描述。为了避免过多不必要的细节,在以下实施例中对属于公知的结构或功能将不进行详细描述。以下实施例中所使用的近似性语言可用于定量表述,表明在不改变基本功能的情况下可允许数量有一定的变动。除有定义外,以下实施例中所用的技术和科学术语具有与本发明所属领域技术人员普遍理解的相同含义。Specific embodiments of the present invention will be described in detail below. In order to avoid unnecessary details, well-known structures or functions will not be described in detail in the following embodiments. The language of approximation used in the following examples can be used for quantitative expressions, showing that some variation in quantity is permissible without changing the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
一种纳米抗氧化膜的制备方法,包括以下步骤:A preparation method of nano anti-oxidation film, comprising the following steps:
(1)按重量份数选择以下材料:明胶8%,甘油1%,生育酚4%,吐温0.8%,其余为去离子水,总计100%。(1) Select the following materials in parts by weight: gelatin 8%, glycerol 1%,
(2)按重量份数将明胶和水混合,在60℃水溶液中溶解90min,期间不停搅拌,直至明胶完全溶解。(2) Mix gelatin and water in parts by weight, dissolve in an aqueous solution at 60° C. for 90 minutes, and keep stirring until the gelatin is completely dissolved.
(3)将步骤(2)的明胶水溶液冷却至室温,按重量份数加入甘油溶液,混合均匀,得到明胶-甘油水性溶液;(3) cooling the aqueous gelatin solution of step (2) to room temperature, adding glycerol solution in parts by weight, and mixing uniformly to obtain gelatin-glycerol aqueous solution;
(4)按重量份数将生育酚和吐温80进行混合,并用振荡器进行充分震荡,得到油性溶液;(4) tocopherol and Tween 80 are mixed by weight, and fully shaken with a vibrator to obtain an oily solution;
(5)将步骤(3)的水溶液和步骤(4)的油性溶液混合,用均质机在13000rpm的条件下均质3min,得到复合明胶膜液;(5) mixing the aqueous solution of step (3) and the oily solution of step (4), and homogenizing for 3min under the condition of 13000rpm with a homogenizer to obtain a composite gelatin film liquid;
(6)将步骤(5)的明胶乳液在80~100MPa的高压均质条件下进行混合;(6) the gelatin emulsion of step (5) is mixed under the high pressure homogenization condition of 80~100MPa;
(7)将步骤(6)的明胶乳液在400~600w的条件下超声10min,得到成膜前的膜液;(7) ultrasonicating the gelatin emulsion of step (6) under the condition of 400~600w for 10min to obtain the film liquid before film formation;
(8)将4ml膜液倒入90mm*90mm的塑料平皿中,在室温通风条件下干燥48h;(8) Pour 4ml of the film liquid into a 90mm*90mm plastic dish, and dry it for 48h under room temperature ventilation;
(9)将干燥后的膜放入相对湿度为50%的密闭环境平衡24h,揭下后即得到纳米抗氧化膜。(9) The dried film is placed in a closed environment with a relative humidity of 50% for equilibrium for 24 hours, and the nano-antioxidant film is obtained after peeling off.
其中,步骤(1)中的明胶冻力为260-270。Wherein, the gelatin freezing power in step (1) is 260-270.
步骤(2)明胶在60℃水溶液中加热时,要用保鲜膜进行封口,防止长时间的加热过程使溶液水分挥发,影响溶液中明胶的浓度。Step (2) When the gelatin is heated in an aqueous solution at 60° C., it should be sealed with a plastic wrap to prevent the water in the solution from volatilizing during the long-term heating process and affect the concentration of gelatin in the solution.
步骤(6)中的高压循环次数为3次。The number of high pressure cycles in step (6) is 3 times.
步骤(7)中的超声设备选择超声波破碎仪,频率为20kHz,选择6mm的变幅杆,超声2s,停止2s。The ultrasonic device in step (7) is an ultrasonic crusher, the frequency is 20 kHz, the horn of 6 mm is selected, the ultrasonic wave is ultrasonic for 2 s, and the stop is 2 s.
步骤(8)中的干燥条件是在25±2℃,相对湿度为50±5%的条件下进行的。The drying conditions in step (8) are carried out under the conditions of 25±2° C. and relative humidity of 50±5%.
以上方法采用高压均质和超声相结合的方式,对复合明胶膜液进行处理,制备纳米级别抗氧化明胶膜。高压均质和超声联合使明胶膜中油滴形成纳米颗粒,从而制备出纳米级别的抗氧化的明胶膜。一方面,添加了生育酚的明胶膜赋予明胶膜良好的抗氧化性,同时使明胶膜的断裂伸长率增高;另一方面与非纳米级别的抗氧化明胶膜相比,高压均质和超声结合制备的纳米明胶膜具有较高的抗氧化性、拉伸强度和断裂伸长率,较低的水蒸气透过性。该方法制备纳米级别的抗氧化明胶膜具有较好的物理性能好较高的抗氧化性,能作为食品包装领域的功能性包装材料。该方法制备的纳米抗氧化明胶膜具有良好的机械性能、水蒸气透过性和光阻隔性,且膜的抗氧化性能较高,可作为一种功能性的食品包装材料。The above method adopts a combination of high-pressure homogenization and ultrasound to process the composite gelatin film liquid to prepare a nano-level antioxidant gelatin film. The combination of high-pressure homogenization and ultrasonication makes the oil droplets in the gelatin film form nanoparticles, thereby preparing a nano-scale anti-oxidative gelatin film. On the one hand, the gelatin film added with tocopherol endows the gelatin film with good anti-oxidation properties, and at the same time increases the elongation at break of the gelatin film; The nanogelatin films prepared by the combination have higher oxidation resistance, tensile strength and elongation at break, and lower water vapor permeability. The nano-level antioxidant gelatin film prepared by the method has better physical properties and higher oxidation resistance, and can be used as a functional packaging material in the field of food packaging. The nano-antioxidative gelatin film prepared by the method has good mechanical properties, water vapor permeability and light barrier properties, and the film has high antioxidative properties, and can be used as a functional food packaging material.
实施例1Example 1
(1)按重量份数选择以下材料:明胶8%,甘油1%,生育酚4%,吐温0.8%,其余为去离子水,总计100%。(1) Select the following materials in parts by weight: gelatin 8%, glycerol 1%,
(2)按重量份数将明胶和水混合,在60℃水溶液中溶解90min,期间不停搅拌,直至明胶完全溶解。(2) Mix gelatin and water in parts by weight, dissolve in an aqueous solution at 60° C. for 90 minutes, and keep stirring until the gelatin is completely dissolved.
(3)将步骤(2)的明胶水溶液冷却至室温,按重量份数加入甘油溶液,混合均匀,得到明胶-甘油水性溶液;(3) cooling the aqueous gelatin solution of step (2) to room temperature, adding glycerol solution in parts by weight, and mixing uniformly to obtain gelatin-glycerol aqueous solution;
(4)按重量份数将生育酚和吐温80进行混合,并用振荡器进行充分震荡,得到油性溶液;(4) tocopherol and Tween 80 are mixed by weight, and fully shaken with a vibrator to obtain an oily solution;
(5)将步骤(3)的水溶液和步骤(4)的油性溶液混合,用均质机在13000rpm的条件下均质3min,得到复合明胶膜液;(5) mixing the aqueous solution of step (3) and the oily solution of step (4), and homogenizing for 3min under the condition of 13000rpm with a homogenizer to obtain a composite gelatin film liquid;
(6)将步骤(5)的明胶乳液在80MPa的高压均质条件下进行混合;(6) the gelatin emulsion of step (5) is mixed under the high pressure homogenization condition of 80MPa;
(7)将步骤(6)的明胶乳液在400w的条件下超声10min,得到成膜前的膜液;(7) the gelatin emulsion of step (6) is ultrasonicated 10min under the condition of 400w, obtains the film liquid before film formation;
(8)将4ml膜液倒入90mm*90mm的塑料平皿中,在室温通风条件下干燥48h;(8) Pour 4ml of the film liquid into a 90mm*90mm plastic dish, and dry it for 48h under room temperature ventilation;
(9)将干燥后的膜放入相对湿度为50%的密闭环境平衡24h,揭下后即得到纳米抗氧化膜。(9) The dried film is placed in a closed environment with a relative humidity of 50% for equilibrium for 24 hours, and the nano-antioxidant film is obtained after peeling off.
实施例2Example 2
(1)按重量份数选择以下材料:明胶8%,甘油1%,生育酚4%,吐温0.8%,其余为去离子水,总计100%。(1) Select the following materials in parts by weight: gelatin 8%, glycerol 1%,
(2)按重量份数将明胶和水混合,在60℃水溶液中溶解90min,期间不停搅拌,直至明胶完全溶解。(2) Mix gelatin and water in parts by weight, dissolve in an aqueous solution at 60° C. for 90 minutes, and keep stirring until the gelatin is completely dissolved.
(3)将步骤(2)的明胶水溶液冷却至室温,按重量份数加入甘油溶液,混合均匀,得到明胶-甘油水性溶液;(3) cooling the aqueous gelatin solution of step (2) to room temperature, adding glycerol solution in parts by weight, and mixing uniformly to obtain gelatin-glycerol aqueous solution;
(4)按重量份数将生育酚和吐温80进行混合,并用振荡器进行充分震荡,得到油性溶液;(4) tocopherol and Tween 80 are mixed by weight, and fully shaken with a vibrator to obtain an oily solution;
(5)将步骤(3)的水溶液和步骤(4)的油性溶液混合,用均质机在13000rpm的条件下均质3min,得到复合明胶膜液;(5) mixing the aqueous solution of step (3) and the oily solution of step (4), and homogenizing for 3min under the condition of 13000rpm with a homogenizer to obtain a composite gelatin film liquid;
(6)将步骤(5)的明胶乳液在80MPa的高压均质条件下进行混合;(6) the gelatin emulsion of step (5) is mixed under the high pressure homogenization condition of 80MPa;
(7)将步骤(6)的明胶乳液在600w的条件下超声10min,得到成膜前的膜液;(7) the gelatin emulsion of step (6) is ultrasonicated 10min under the condition of 600w, obtains the film liquid before film-forming;
(8)将4ml膜液倒入90mm*90mm的塑料平皿中,在室温通风条件下干燥48h;(8) Pour 4ml of the film liquid into a 90mm*90mm plastic dish, and dry it for 48h under room temperature ventilation;
(9)将干燥后的膜放入相对湿度为50%的密闭环境平衡24h,揭下后即得到纳米抗氧化膜。(9) The dried film is placed in a closed environment with a relative humidity of 50% for equilibrium for 24 hours, and the nano-antioxidant film is obtained after peeling off.
实施例3Example 3
(1)按重量份数选择以下材料:明胶8%,甘油1%,生育酚4%,吐温0.8%,其余为去离子水,总计100%。(1) Select the following materials in parts by weight: gelatin 8%, glycerol 1%,
(2)按重量份数将明胶和水混合,在60℃水溶液中溶解90min,期间不停搅拌,直至明胶完全溶解。(2) Mix gelatin and water in parts by weight, dissolve in an aqueous solution at 60° C. for 90 minutes, and keep stirring until the gelatin is completely dissolved.
(3)将步骤(2)的明胶水溶液冷却至室温,按重量份数加入甘油溶液,混合均匀,得到明胶-甘油水性溶液;(3) cooling the aqueous gelatin solution of step (2) to room temperature, adding glycerol solution in parts by weight, and mixing uniformly to obtain gelatin-glycerol aqueous solution;
(4)按重量份数将生育酚和吐温80进行混合,并用振荡器进行充分震荡,得到油性溶液;(4) tocopherol and Tween 80 are mixed by weight, and fully shaken with a vibrator to obtain an oily solution;
(5)将步骤(3)的水溶液和步骤(4)的油性溶液混合,用均质机在13000rpm的条件下均质3min,得到复合明胶膜液;(5) mixing the aqueous solution of step (3) and the oily solution of step (4), and homogenizing for 3min under the condition of 13000rpm with a homogenizer to obtain a composite gelatin film liquid;
(6)将步骤(5)的明胶乳液在100MPa的高压均质条件下进行混合;(6) the gelatin emulsion of step (5) is mixed under the high pressure homogenization condition of 100MPa;
(7)将步骤(6)的明胶乳液在400w的条件下超声10min,得到成膜前的膜液;(7) the gelatin emulsion of step (6) is ultrasonicated 10min under the condition of 400w, obtains the film liquid before film formation;
(8)将4ml膜液倒入90mm*90mm的塑料平皿中,在室温通风条件下干燥48h;(8) Pour 4ml of the film liquid into a 90mm*90mm plastic dish, and dry it for 48h under room temperature ventilation;
(9)将干燥后的膜放入相对湿度为50%的密闭环境平衡24h,揭下后即得到纳米抗氧化膜。(9) The dried film is placed in a closed environment with a relative humidity of 50% for equilibrium for 24 hours, and the nano-antioxidant film is obtained after peeling off.
实施例4Example 4
(1)按重量份数选择以下材料:明胶8%,甘油1%,生育酚4%,吐温0.8%,其余为去离子水,总计100%。(1) Select the following materials in parts by weight: gelatin 8%, glycerol 1%,
(2)按重量份数将明胶和水混合,在60℃水溶液中溶解90min,期间不停搅拌,直至明胶完全溶解。(2) Mix gelatin and water in parts by weight, dissolve in an aqueous solution at 60° C. for 90 minutes, and keep stirring until the gelatin is completely dissolved.
(3)将步骤(2)的明胶水溶液冷却至室温,按重量份数加入甘油溶液,混合均匀,得到明胶-甘油水性溶液;(3) cooling the aqueous gelatin solution of step (2) to room temperature, adding glycerol solution in parts by weight, and mixing uniformly to obtain gelatin-glycerol aqueous solution;
(4)按重量份数将生育酚和吐温80进行混合,并用振荡器进行充分震荡,得到油性溶液;(4) tocopherol and Tween 80 are mixed by weight, and fully shaken with a vibrator to obtain an oily solution;
(5)将步骤(3)的水溶液和步骤(4)的油性溶液混合,用均质机在13000rpm的条件下均质3min,得到复合明胶膜液;(5) mixing the aqueous solution of step (3) and the oily solution of step (4), and homogenizing for 3min under the condition of 13000rpm with a homogenizer to obtain a composite gelatin film liquid;
(6)将步骤(5)的明胶乳液在100MPa的高压均质条件下进行混合;(6) the gelatin emulsion of step (5) is mixed under the high pressure homogenization condition of 100MPa;
(7)将步骤(6)的明胶乳液在600w的条件下超声10min,得到成膜前的膜液;(7) the gelatin emulsion of step (6) is ultrasonicated 10min under the condition of 600w, obtains the film liquid before film-forming;
(8)将4ml膜液倒入90mm*90mm的塑料平皿中,在室温通风条件下干燥48h;(8) Pour 4ml of the film liquid into a 90mm*90mm plastic dish, and dry it for 48h under room temperature ventilation;
(9)将干燥后的膜放入相对湿度为50%的密闭环境平衡24h,揭下后即得到纳米抗氧化膜。(9) The dried film is placed in a closed environment with a relative humidity of 50% for equilibrium for 24 hours, and the nano-antioxidant film is obtained after peeling off.
对比例1Comparative Example 1
(1)按重量份数选择以下材料:明胶8%,甘油1%,生育酚4%,吐温0.8%,其余为去离子水,总计100%。(1) Select the following materials in parts by weight: gelatin 8%, glycerol 1%,
(2)按重量份数将明胶和水混合,在60℃水溶液中溶解90min,期间不停搅拌,直至明胶完全溶解。(2) Mix gelatin and water in parts by weight, dissolve in an aqueous solution at 60° C. for 90 minutes, and keep stirring until the gelatin is completely dissolved.
(3)将步骤(2)的明胶水溶液冷却至室温,按重量份数加入甘油溶液,混合均匀,得到明胶-甘油水性溶液;(3) cooling the aqueous gelatin solution of step (2) to room temperature, adding glycerol solution in parts by weight, and mixing uniformly to obtain gelatin-glycerol aqueous solution;
(4)按重量份数将生育酚和吐温80进行混合,并用振荡器进行充分震荡,得到油性溶液;(4) tocopherol and Tween 80 are mixed by weight, and fully shaken with a vibrator to obtain an oily solution;
(5)将步骤(3)的水溶液和步骤(4)的油性溶液混合,用均质机在13000rpm的条件下均质3min,得到复合明胶膜液;(5) mixing the aqueous solution of step (3) and the oily solution of step (4), and homogenizing for 3min under the condition of 13000rpm with a homogenizer to obtain a composite gelatin film liquid;
(6)将4ml膜液倒入90mm*90mm的塑料平皿中,在室温通风条件下干燥48h;(6) Pour 4ml of the film liquid into a 90mm*90mm plastic dish, and dry it for 48h under room temperature ventilation;
(7)将干燥后的膜放入相对湿度为50%的密闭环境平衡24h,揭下后即得到复合明胶膜。(7) Put the dried film into a closed environment with a relative humidity of 50% to balance for 24 hours, and remove the film to obtain a composite gelatin film.
对比例2Comparative Example 2
(1)按重量份数选择以下材料:明胶8%,甘油1%,生育酚4%,吐温0.8%,其余为去离子水,总计100%。(1) Select the following materials in parts by weight: gelatin 8%, glycerol 1%,
(2)按重量份数将明胶和水混合,在60℃水溶液中溶解90min,期间不停搅拌,直至明胶完全溶解。(2) Mix gelatin and water in parts by weight, dissolve in an aqueous solution at 60° C. for 90 minutes, and keep stirring until the gelatin is completely dissolved.
(3)将步骤(2)的明胶水溶液冷却至室温,按重量份数加入甘油溶液,混合均匀,得到明胶-甘油水性溶液;(3) cooling the aqueous gelatin solution of step (2) to room temperature, adding glycerol solution in parts by weight, and mixing uniformly to obtain gelatin-glycerol aqueous solution;
(4)按重量份数将生育酚和吐温80进行混合,并用振荡器进行充分震荡,得到油性溶液;(4) tocopherol and Tween 80 are mixed by weight, and fully shaken with a vibrator to obtain an oily solution;
(5)将步骤(3)的水溶液和步骤(4)的油性溶液混合,用均质机在13000rpm的条件下均质3min,得到复合明胶膜液;(5) mixing the aqueous solution of step (3) and the oily solution of step (4), and homogenizing for 3min under the condition of 13000rpm with a homogenizer to obtain a composite gelatin film liquid;
(6)将步骤(5)的明胶乳液在100MPa的高压均质条件下进行混合;(6) the gelatin emulsion of step (5) is mixed under the high pressure homogenization condition of 100MPa;
(7)将4ml膜液倒入90mm*90mm的塑料平皿中,在室温通风条件下干燥48h;(7) Pour 4ml of the film liquid into a 90mm*90mm plastic dish, and dry it for 48h under room temperature ventilation;
(8)将干燥后的膜放入相对湿度为50%的密闭环境平衡24h,揭下后即得到复合明胶膜。(8) Put the dried film into a closed environment with a relative humidity of 50% to balance for 24 hours, and remove the film to obtain a composite gelatin film.
对比例3Comparative Example 3
(1)按重量份数选择以下材料:明胶8%,甘油1%,生育酚4%,吐温0.8%,其余为去离子水,总计100%。(1) Select the following materials in parts by weight: gelatin 8%, glycerol 1%,
(2)按重量份数将明胶和水混合,在60℃水溶液中溶解90min,期间不停搅拌,直至明胶完全溶解。(2) Mix gelatin and water in parts by weight, dissolve in an aqueous solution at 60° C. for 90 minutes, and keep stirring until the gelatin is completely dissolved.
(3)将步骤(2)的明胶水溶液冷却至室温,按重量份数加入甘油溶液,混合均匀,得到明胶-甘油水性溶液;(3) cooling the aqueous gelatin solution of step (2) to room temperature, adding glycerol solution in parts by weight, and mixing uniformly to obtain gelatin-glycerol aqueous solution;
(4)按重量份数将生育酚和吐温80进行混合,并用振荡器进行充分震荡,得到油性溶液;(4) tocopherol and Tween 80 are mixed by weight, and fully shaken with a vibrator to obtain an oily solution;
(5)将步骤(3)的水溶液和步骤(4)的油性溶液混合,用均质机在13000rpm的条件下均质3min,得到复合明胶膜液;(5) mixing the aqueous solution of step (3) and the oily solution of step (4), and homogenizing for 3min under the condition of 13000rpm with a homogenizer to obtain a composite gelatin film liquid;
(6)将步骤(6)的明胶乳液在600w的条件下超声10min,得到成膜前的膜液;(6) the gelatin emulsion of step (6) is ultrasonicated 10min under the condition of 600w, obtains the film liquid before film-forming;
(7)将4ml膜液倒入90mm*90mm的塑料平皿中,在室温通风条件下干燥48h;(7) Pour 4ml of the film liquid into a 90mm*90mm plastic dish, and dry it for 48h under room temperature ventilation;
(8)将干燥后的膜放入相对湿度为50%的密闭环境平衡24h,揭下后即得到复合明胶膜。(8) Put the dried film into a closed environment with a relative humidity of 50% to balance for 24 hours, and remove the film to obtain a composite gelatin film.
实施例5Example 5
将按照实施例1~4制得的纳米抗氧化膜和对比例1-3制得的普通复合明胶膜进行膜厚、水蒸气透过率、拉伸强度、断裂拉伸率、水溶解性和透光性的检测。Film thickness, water vapor transmission rate, tensile strength, elongation at break, water solubility and Transmittance detection.
检测方法如下:The detection method is as follows:
一、纳米明胶膜厚度的测量1. Measurement of Nanogelatin Film Thickness
用电子螺旋测微器测量膜的厚度,测量结果如表1所示。The thickness of the film was measured with an electronic helical micrometer, and the measurement results are shown in Table 1.
二、纳米明胶膜机械性能的测试2. Testing of mechanical properties of nano-gelatin films
用质构仪对复合明胶膜对拉伸强度(TS)和断裂伸长率(EAB)进行测试。将膜剪裁成20mm宽和50mm长的条状,将膜固定在仪器手柄的两端,调整手柄两端的间距为30mm,测试速度为1mm/s,促发力为20.0g。测试结构如表1所示。The composite gelatin films were tested for tensile strength (TS) and elongation at break (EAB) with a texture analyzer. Cut the film into strips with a width of 20mm and a length of 50mm, fix the film on both ends of the instrument handle, adjust the distance between the two ends of the handle to 30mm, the test speed is 1mm/s, and the activating force is 20.0g. The test structure is shown in Table 1.
TS(MPa)=Fmax/ATS(MPa)= Fmax /A
EAB(%)=(L0/ΔL)×100%EAB(%)=(L 0 /ΔL)×100%
其中,Fmax是将条状膜样品分离需要的最大负载(N),A是样品膜的切面面积(m2),L0是膜的初始拉伸长度,ΔL是膜断裂后的拉伸长度,L0=30mm。where Fmax is the maximum load (N) required to separate the strip film sample, A is the cut surface area (m 2 ) of the sample film, L 0 is the initial stretch length of the film, and ΔL is the stretch length after film breakage , L 0 =30mm.
三、纳米明胶膜水蒸气透过性的测试3. Test of water vapor permeability of nano-gelatin film
在直径为40mm,深为25mm的玻璃杯中装入干燥的CaCl2,用膜对玻璃杯进行密封。将玻璃杯放入含去离子水的密闭容器中,调节环境温度为30℃。每隔一个小时测量一次玻璃杯的重量,直至玻璃杯的重量没有显著变化时,停止测量。膜的水蒸气透过性通过一下公式进行计算:Dry CaCl 2 was placed in a glass with a diameter of 40 mm and a depth of 25 mm, and the glass was sealed with a membrane. Place the glass in an airtight container containing deionized water and adjust the ambient temperature to 30°C. Measure the weight of the glass every hour until the weight of the glass does not change significantly, stop measuring. The water vapor permeability of the membrane is calculated by the following formula:
WVP(g m-1s-1Pa-1)=wlA-1t-1(P2–P1)-1,WVP(gm -1 s -1 Pa -1 )=wlA -1 t -1 (P 2 -P 1 ) -1 ,
w代表玻璃杯增长的重量(g),l是膜的厚度(m),A是膜封口的面积(m2),t是玻璃杯重量变化的时间(s),P2-P1是膜两侧的蒸气压差(4244.9Pa at 30℃)。测试结构如表1所示。w represents the weight of the glass growing (g), l is the thickness of the film (m), A is the area of the film seal (m 2 ), t is the time for the weight of the glass to change (s), P 2 -P 1 is the film Vapor pressure difference on both sides (4244.9Pa at 30°C). The test structure is shown in Table 1.
四、纳米明胶膜光阻隔性的测试4. Test of light barrier properties of nano-gelatin film
用分光光度计对膜的光阻隔性进行测量,可见光的方位在200nm到800nm之间。测试结构如表2所示。The light-blocking properties of the films were measured with a spectrophotometer, with an azimuth of visible light between 200 nm and 800 nm. The test structure is shown in Table 2.
五、DPPH自由基清除能力5. DPPH free radical scavenging ability
用无水乙醇配置0.1mmol/l的DPPH溶液,避光保存。将2ml测试样品溶液及2mlDPPH溶液加入到同一试管中,摇匀,室温下暗处静置30min后测定其吸光度A1,同时测定2mlDPPH溶液与2ml溶剂混合后的吸光度A0,DPPH的计算公式为:Prepare a 0.1 mmol/l DPPH solution with absolute ethanol and store in the dark. Add 2ml of the test sample solution and 2ml of DPPH solution into the same test tube, shake well, and stand in the dark for 30min at room temperature to measure the absorbance A 1 , and simultaneously measure the absorbance A 0 of 2ml of DPPH solution mixed with 2ml of solvent. The calculation formula of DPPH is: :
A0为未加样品时的DPPH在520nm处的吸光度,A1为样品与DPPH试剂在520nm处的吸光度。测试结果如图1所示。A 0 is the absorbance of DPPH at 520 nm when no sample is added, and A 1 is the absorbance of the sample and DPPH reagent at 520 nm. The test results are shown in Figure 1.
表1复合明胶膜膜厚、拉伸强度、断裂伸长率、水蒸气透过性数据Table 1 Data of film thickness, tensile strength, elongation at break and water vapor permeability of composite gelatin films
表2复合明胶膜光阻隔性数据Table 2 Light barrier data of composite gelatin film
以上对本发明的实施例进行了详细说明,但所述内容仅为本发明的较佳实施例,并不用以限制本发明。凡在本发明的申请范围内所做的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。The embodiments of the present invention have been described in detail above, but the above contents are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the scope of the application of the present invention shall be included within the protection scope of the present invention.
Claims (9)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010204190.4A CN111286056B (en) | 2020-03-21 | 2020-03-21 | Preparation method of nano antioxidant film |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010204190.4A CN111286056B (en) | 2020-03-21 | 2020-03-21 | Preparation method of nano antioxidant film |
Publications (2)
Publication Number | Publication Date |
---|---|
CN111286056A CN111286056A (en) | 2020-06-16 |
CN111286056B true CN111286056B (en) | 2022-09-27 |
Family
ID=71025893
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010204190.4A Active CN111286056B (en) | 2020-03-21 | 2020-03-21 | Preparation method of nano antioxidant film |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111286056B (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112623447B (en) * | 2020-12-14 | 2022-09-23 | 宁波市农业科学研究院 | Clean vegetable fresh-keeping package and using method thereof |
CN116535867A (en) * | 2023-04-26 | 2023-08-04 | 上海应用技术大学 | Antibacterial and oil-resistant degradable aromatic packaging material, method and application |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104194354A (en) * | 2014-09-05 | 2014-12-10 | 山东省海洋生物研究院 | Edible biological preservative film and preparation method thereof |
CN104231291A (en) * | 2014-09-05 | 2014-12-24 | 安徽科技学院 | Preparation method of freshness-retaining packaging film with antibacterial and antioxidant function |
CN107383895A (en) * | 2017-07-24 | 2017-11-24 | 青岛金典生化器材有限公司 | A kind of oxidation resistant collagen film and preparation method thereof |
CN108727836A (en) * | 2018-06-11 | 2018-11-02 | 海南大学 | A kind of preparation method with the edible biogelatin film for being sustained EGCG performances |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109021587B (en) * | 2018-06-07 | 2020-12-04 | 宁夏金博乐食品科技有限公司 | Edible gelatin-based film and method of making same |
-
2020
- 2020-03-21 CN CN202010204190.4A patent/CN111286056B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104194354A (en) * | 2014-09-05 | 2014-12-10 | 山东省海洋生物研究院 | Edible biological preservative film and preparation method thereof |
CN104231291A (en) * | 2014-09-05 | 2014-12-24 | 安徽科技学院 | Preparation method of freshness-retaining packaging film with antibacterial and antioxidant function |
CN107383895A (en) * | 2017-07-24 | 2017-11-24 | 青岛金典生化器材有限公司 | A kind of oxidation resistant collagen film and preparation method thereof |
CN108727836A (en) * | 2018-06-11 | 2018-11-02 | 海南大学 | A kind of preparation method with the edible biogelatin film for being sustained EGCG performances |
Non-Patent Citations (1)
Title |
---|
"Effect of ultrasound treatment on the properties of nano-emulsion films obtained from hazelnut meal protein and clove essential oil";Osman Gul et al.;《Ultrasonics - Sonochemistry》;20171012;全文 * |
Also Published As
Publication number | Publication date |
---|---|
CN111286056A (en) | 2020-06-16 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Ahammed et al. | Effect of transglutaminase crosslinking on solubility property and mechanical strength of gelatin-zein composite films | |
Zhou et al. | pH-responsive double-layer indicator films based on konjac glucomannan/camellia oil and carrageenan/anthocyanin/curcumin for monitoring meat freshness | |
Mohajer et al. | Physico-chemical and microstructural properties of fish gelatin/agar bio-based blend films | |
Hu et al. | Effects of ultrasound pretreatment on functional property, antioxidant activity, and digestibility of soy protein isolate nanofibrils | |
CN111286056B (en) | Preparation method of nano antioxidant film | |
CN104987516B (en) | A kind of nano-cellulose strengthens the preparation method of tara gum substrate pH intelligent response film | |
CN104211975B (en) | Preparation method of water-blocking oxygen-blocking edible film | |
CN108586828A (en) | A kind of edible compound fresh-keeping film and its preparation method and application | |
CN104210162B (en) | The preparation method of the hydrophobic edible film of a kind of height | |
Wang et al. | Waxy maize starch nanoparticles incorporated tea polyphenols to stabilize Pickering emulsion and inhibit oil oxidation | |
CN103113628B (en) | Edible composite film and preparation method thereof | |
CN107254182A (en) | Edible film is into film liquid and preparation method thereof and edible film and preparation method thereof | |
Napso et al. | Cellulose gel dispersion: From pure hydrogel suspensions to encapsulated oil-in-water emulsions | |
CN105440701B (en) | A kind of preparation method of edibility albumen nanometer film | |
CN106036368A (en) | Preparation process capable of increasing encapsulation rate of essential oil microcapsules | |
Wang et al. | Fabrication and characterization of fish gelatin/soluble soybean polysaccharide edible blend films through complex coacervation | |
Li et al. | A versatile bilayer smart packaging based on konjac glucomannan/alginate for maintaining and monitoring seafood freshness | |
CN111423604B (en) | A kind of preparation method of ultrasonically modified composite gelatin film | |
CN105995948B (en) | A kind of agar compound colloid with high low-temperature soluble gel strength and preparation method thereof | |
CN104448368B (en) | A kind of preparation method of soybean protein isolate/PLA composite package film | |
Chen et al. | Complex bio‐nanoparticles assembled by a pH‐driven method: environmental stress stability and oil–water interfacial behavior | |
CN106519708A (en) | Preparation method of gelatin film containing methylcellulose and glycerin | |
CN115678070A (en) | Preparation and application of AgNPs composite film | |
CN115449131A (en) | Octenyl succinic acid cassava starch ester/chitosan/nano ZnO modified film and preparation method and application thereof | |
CN115449114A (en) | Preparation method and application of high-barrier double-effect active packaging film with internal and external linkage |
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 |