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CN104893007A - Starch-based film with antibacterial microcapsules and method for manufacturing starch-based film - Google Patents

Starch-based film with antibacterial microcapsules and method for manufacturing starch-based film Download PDF

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CN104893007A
CN104893007A CN201510368922.2A CN201510368922A CN104893007A CN 104893007 A CN104893007 A CN 104893007A CN 201510368922 A CN201510368922 A CN 201510368922A CN 104893007 A CN104893007 A CN 104893007A
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starch
microcapsules
antibacterial
film
cyclodextrin
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钱怡
闫丹丹
张新昌
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Jiangnan University
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Abstract

本发明公开了一种含抗菌微胶囊的淀粉基薄膜(见附图)及其制备方法。该材料以淀粉作为成膜基材,加入具有抗菌性的微胶囊,以及明胶、甘油、CaCl2等助剂,在模具中采用流延法制成。首先将丁香精油和β-环糊精通过分子包埋法制成微胶囊备用;第二将淀粉在一定温度下搅拌糊化,将一定量的明胶加热溶解,称取一定量的甘油,CaCl2备用;第三将明胶、微胶囊、甘油、CaCl2等按比例加入糊化后的淀粉溶液中搅拌20min;第四将混合溶液冷却至室温后,倒入自制模具中流延,并放入干燥箱干燥至恒重;第五揭膜并测试性能。本发明制得的含抗菌微胶囊的淀粉基薄膜,具有原料来源广泛,安全卫生,绿色可降解等优点,且对食品中的微生物具有良好的抑制性。可用于生鲜食品的抗菌包装,具有广阔的发展前景。

The invention discloses a starch-based film containing antibacterial microcapsules (see the accompanying drawings) and a preparation method thereof. The material uses starch as the film-forming substrate, adds microcapsules with antibacterial properties, and additives such as gelatin, glycerin, and CaCl 2 , and is made by casting in a mold. Firstly, clove essential oil and β-cyclodextrin are made into microcapsules by molecular embedding method; secondly, the starch is stirred and gelatinized at a certain temperature, a certain amount of gelatin is heated and dissolved, and a certain amount of glycerin is weighed, and CaCl 2 is set aside ; thirdly, add gelatin, microcapsules, glycerin, CaCl2 , etc. into the gelatinized starch solution in proportion and stir for 20 minutes; fourthly, after cooling the mixed solution to room temperature, pour it into a self-made mold for casting, and put it in a drying oven to dry To constant weight; the fifth film and test performance. The starch-based film containing antibacterial microcapsules prepared by the invention has the advantages of wide source of raw materials, safety and sanitation, green and degradable, etc., and has good inhibitory effect on microorganisms in food. It can be used for antibacterial packaging of fresh food and has broad development prospects.

Description

一种含抗菌微胶囊的淀粉基薄膜及其制备方法A kind of starch-based film containing antibacterial microcapsules and preparation method thereof

技术领域 technical field

本发明涉及一种含微胶囊的淀粉基抗菌薄膜及其制备方法。 The invention relates to a starch-based antibacterial film containing microcapsules and a preparation method thereof.

背景技术 Background technique

淀粉被认为是最具发展前景的生物降解包装材料之一。淀粉经糊化、凝沉、干燥后制成的淀粉膜具有拉伸性能好、透明度高等优点,但用于包装时仍存在抗菌性不好的缺点。多项研究表明可以通过复合的方式,对淀粉薄膜的抗菌性能进行改善。丁香精油具有较强的抑菌效果,但难溶于水,稳定性较差,易氧化、挥发,一定程度上限制了其抗菌效果。微胶囊技术是一种用成膜材料把固体或液体包覆使之形成微小粒子的技术。通过微胶囊技术可以将丁香精油包裹在壁材中,既能保持丁香精油的抗菌性,又能延长其有效期。 Starch is considered to be one of the most promising biodegradable packaging materials. The starch film made of starch after gelatinization, retrogradation and drying has the advantages of good tensile properties and high transparency, but it still has the disadvantage of poor antibacterial properties when used for packaging. A number of studies have shown that the antibacterial properties of starch films can be improved by compounding. Clove essential oil has a strong antibacterial effect, but it is difficult to dissolve in water, has poor stability, and is easy to oxidize and volatilize, which limits its antibacterial effect to a certain extent. Microcapsule technology is a technology that uses film-forming materials to coat solids or liquids to form tiny particles. The clove essential oil can be wrapped in the wall material through the microcapsule technology, which can not only maintain the antibacterial property of the clove essential oil, but also prolong its validity period.

关于抗菌淀粉基薄膜的制备方法有这样一些文献报道: There are some bibliographical reports about the preparation method of antibacterial starch-based film:

Kuorwel等对涂有芳樟醇、香芹酚或百里香酚的淀粉基薄膜对体外或接种在切达干酪表面的金黄色葡萄球菌的抗菌活性(AM)进行了研究。研究表明:在一定浓度范围内,金黄色葡萄球菌对抗菌剂的敏感性顺序是:百里香酚>香芹酚>芳樟醇。 studied the antimicrobial activity (AM) of starch-based films coated with linalool, carvacrol, or thymol against Staphylococcus aureus in vitro or inoculated on the surface of cheddar cheese. Studies have shown that within a certain concentration range, the order of sensitivity of Staphylococcus aureus to antibacterial agents is: thymol>carvacrol>linalool.

赵国华等大蒜精油添加到木薯淀粉中制成了抗菌淀粉可食膜,结果表明添加大蒜精油为木薯淀粉质量的1.5%时,抗菌淀粉可食膜对大肠杆菌和金黄色葡萄球菌具有最好的抗菌效果。 Zhao Guohua et al. added garlic essential oil to tapioca starch to make an edible film of antibacterial starch. The results showed that when garlic essential oil was added to 1.5% of the mass of cassava starch, the edible film of antibacterial starch had the best antibacterial effect on Escherichia coli and Staphylococcus aureus. Effect.

赵丹将肉桂精油、壳聚糖和溶菌酶添加到玉米淀粉膜中,制成了抗菌淀粉膜,并研究了其对大肠杆菌和金黄色葡萄球菌抑制效果。结果表明,添加壳聚糖的玉米淀粉膜对大肠杆菌具有最好的抑制效果,添加肉桂精油的玉米淀粉膜对金黄色葡萄球菌具有最好的抑制效果。 Zhao Dan added cinnamon essential oil, chitosan and lysozyme to corn starch film to make antibacterial starch film, and studied its inhibitory effect on Escherichia coli and Staphylococcus aureus. The results showed that the corn starch film added with chitosan had the best inhibitory effect on Escherichia coli, and the corn starch film added with cinnamon essential oil had the best inhibitory effect on Staphylococcus aureus.

综上所述,目前国内外学者对抗菌淀粉基薄膜制备的研究主要集中在向淀粉膜中添加天然或人工抗菌剂。植物精油是一种性能良好的天然抗菌剂,但其主要的复合方法是添加到成膜基材中,或者涂布在薄膜的表面。由于精油具有挥发性,这在一定程度上限制了其抗菌效果。将丁香精油包裹在壁材中,制成具有抗菌性的微胶囊,并将抗菌微胶囊添加到淀粉膜液中,可以使淀粉基薄膜获得良好的抗 菌性,同时延长其抗菌有效期,是抗菌淀粉基薄膜制备的一个重要发展方向。 To sum up, the current domestic and foreign scholars' research on the preparation of antibacterial starch-based films mainly focuses on adding natural or artificial antibacterial agents to starch films. Plant essential oil is a natural antibacterial agent with good performance, but its main compounding method is to add it to the film-forming substrate or coat it on the surface of the film. Due to the volatility of essential oils, this limits their antibacterial effect to some extent. The clove essential oil is wrapped in the wall material to make antibacterial microcapsules, and the antibacterial microcapsules are added to the starch film liquid, which can make the starch-based film obtain good antibacterial properties and prolong its antibacterial validity period. An important development direction of starch-based film preparation.

发明内容 Contents of the invention

本发明专利主要针对的是现有国内外抗菌淀粉基薄膜制备中存在的问题,提供一种抗菌效果好,有效期长的含抗菌微胶囊的淀粉基薄膜及其制备方法。 The patent of the present invention mainly aims at the problems existing in the preparation of the existing domestic and foreign antibacterial starch-based films, and provides a starch-based film containing antibacterial microcapsules with good antibacterial effect and long validity period and a preparation method thereof.

本发明为实现上述目的,是通过下面的技术方案来实现的。 In order to achieve the above object, the present invention is achieved through the following technical solutions.

本发明的含抗菌微胶囊的淀粉基薄膜制备的质量百分比: The mass percent prepared by the starch-based film containing antibacterial microcapsules of the present invention:

按照技术方案提供的百分比,本发明含抗菌微胶囊的淀粉基薄膜制备方法如下: According to the percentage provided by the technical scheme, the preparation method of the starch-based film containing antibacterial microcapsules of the present invention is as follows:

1)将6gβ-环糊精用36ml蒸馏水溶解,备用。 1) Dissolve 6g of β-cyclodextrin in 36ml of distilled water and set aside.

2)将1g丁香精油溶于20ml体积分数为60%的乙醇,并逐滴加入β-环糊精的水溶液中。 2) Dissolve 1 g of clove essential oil in 20 ml of ethanol with a volume fraction of 60%, and add dropwise to the aqueous solution of β-cyclodextrin.

3)在60℃温度下搅拌2.5小时后取出,待溶液冷至室温后放在4℃的冰箱静置24小时。 3) Take it out after stirring at 60°C for 2.5 hours, and put the solution in a refrigerator at 4°C for 24 hours after cooling to room temperature.

4)将静置后的溶液抽滤,滤渣用无水乙醇和蒸馏水分别洗涤。 4) Suction filter the solution after standing, and wash the filter residue with absolute ethanol and distilled water respectively.

5)在50℃温度下干燥,制成丁香精油/β-环糊精抗菌微胶囊,备用。 5) Dried at a temperature of 50° C. to make clove essential oil/β-cyclodextrin antibacterial microcapsules for future use.

6)称取薄膜总重44-50%的淀粉配成溶液,在80℃下糊化20min。 6) Weigh 44-50% of the total weight of the film to make a starch solution, and gelatinize at 80° C. for 20 minutes.

7)称取薄膜总重9-17%的明胶,在60摄氏度下继续搅拌20min。 7) Weigh 9-17% gelatin of the total weight of the film, and continue to stir at 60 degrees Celsius for 20 minutes.

8)再加入26%的甘油,9-17%抗菌微胶囊以及4-8%CaCl2搅拌反应20min制成成膜液。  8) Add 26% glycerin, 9-17% antibacterial microcapsules and 4-8% CaCl 2 and stir for 20 minutes to make a film-forming solution.

9)将成膜液进行消泡,冷却。然后倒入自制模具中,放入50℃恒温干燥箱,干燥至恒重后揭膜。 9) Defoaming the film-forming solution and cooling. Then pour it into a self-made mold, put it in a 50°C constant temperature drying oven, and dry it to a constant weight before peeling off the film.

本发明关于含抗菌微胶囊的淀粉基薄膜的制备方法,该制备方法利用微胶囊技术将丁香精油包裹在β-环糊精中,并添加到淀粉基液里,通过溶液流延法在自制模具中流延后,恒温干燥一定时间后揭模即可制成含抗菌微胶囊的淀粉基薄 膜。本发明的特点: The present invention relates to a preparation method of a starch-based film containing antibacterial microcapsules. The preparation method uses microcapsule technology to wrap clove essential oil in β-cyclodextrin, and adds it to the starch-based liquid, and casts it on a self-made mold by solution casting After being cast in medium, dry at constant temperature for a certain period of time and then remove the mold to make a starch-based film containing antibacterial microcapsules. Features of the present invention:

1)本发明技术以淀粉等作为成膜基材,具有来源广泛,成本低廉,绿色可降解等优点; 1) The technology of the present invention uses starch and the like as the film-forming substrate, which has the advantages of wide sources, low cost, green and degradable;

2)本发明技术采用的丁香精油是一种抗菌效果优良的天然抗菌剂,且对人体无毒无害,安全卫生; 2) the clove essential oil that the technology of the present invention adopts is a kind of natural antibacterial agent with excellent antibacterial effect, and is nontoxic and harmless to human body, safe and hygienic;

3)运用微胶囊技术将丁香精油包裹在β-环糊精中,克服精油易挥发的缺点,延长抗菌的时效性; 3) Use microcapsule technology to wrap clove essential oil in β-cyclodextrin, overcome the shortcoming of essential oil being volatile, and prolong the timeliness of antibacterial;

4)本发明工艺制备的含抗菌微胶囊的淀粉基薄膜具有良好的抗菌性能和卫生性能,可用于生鲜食品的包装,具有广阔的发展前景。 4) The starch-based film containing antibacterial microcapsules prepared by the process of the present invention has good antibacterial performance and hygienic performance, can be used for the packaging of fresh food, and has broad development prospects.

附图说明 Description of drawings

图1为本发明的含抗菌微胶囊的淀粉基薄膜的外观图。 Fig. 1 is the exterior view of the starch-based film containing antibacterial microcapsules of the present invention.

实施例: Example:

1)将6gβ-环糊精用36ml蒸馏水在45℃下不断搅拌溶解。将1g丁香精油溶于20ml体积分数为60%的乙醇,并逐滴加入β-环糊精的水溶液中。保持60℃恒温搅拌2.5h后,待溶液冷至室温后将其放在4℃冰箱中静置24h。将静置后的溶液抽滤,滤渣用无水乙醇和蒸馏水分别洗涤。在50℃温度下干燥,制成丁香精油/β-环糊精抗菌微胶囊,备用。 1) Dissolve 6g of β-cyclodextrin in 36ml of distilled water with constant stirring at 45°C. Dissolve 1 g of clove essential oil in 20 ml of ethanol with a volume fraction of 60%, and add dropwise to the aqueous solution of β-cyclodextrin. After stirring at a constant temperature of 60°C for 2.5h, the solution was cooled to room temperature and placed in a refrigerator at 4°C for 24h. The solution after standing was filtered with suction, and the filter residue was washed with absolute ethanol and distilled water respectively. Dry at a temperature of 50°C to prepare clove essential oil/β-cyclodextrin antibacterial microcapsules for future use.

2)称取2.5g淀粉,100ml蒸馏水配成溶液,在80℃下糊化20min。再称取1g明胶加入糊化后的淀粉溶液中,在60℃下继续搅拌20min。 2) Weigh 2.5g of starch and 100ml of distilled water to make a solution, and gelatinize at 80°C for 20min. Then weigh 1 g of gelatin and add it to the starch solution after gelatinization, and continue stirring at 60° C. for 20 min.

3)再将1.5g甘油,0.5g抗菌微胶囊以及0.2gCaCl2加入到膜液中,搅拌20min制成成膜液。 3) Add 1.5g of glycerin, 0.5g of antibacterial microcapsules and 0.2g of CaCl 2 into the film solution, and stir for 20 minutes to make a film-forming solution.

4)将成膜液进行消泡,冷却至50摄氏度左右。然后倒入200mm*250mm的自制有机玻璃模具中,放入50℃恒温干燥箱,干燥至恒重后揭膜。 4) Defoaming the film-forming solution and cooling to about 50 degrees Celsius. Then pour it into a 200mm*250mm self-made plexiglass mold, put it in a 50°C constant temperature drying oven, dry it to a constant weight, and then peel off the film.

Claims (4)

1.一种含抗菌微胶囊的淀粉基薄膜制备方法。1. A method for preparing a starch-based film containing antibacterial microcapsules. 2.权利要求1所述的原料质量百分比为:2. the raw material mass percent described in claim 1 is: 所述抗菌微胶囊为自制,其中芯材丁香精油质量为1g,壁材β-环糊精质量为6g,制备方法为分子包埋法。The antibacterial microcapsules are self-made, wherein the quality of clove essential oil as a core material is 1 g, and the mass of β-cyclodextrin as a wall material is 6 g, and the preparation method is a molecular embedding method. 3.权利要求1所述其特征为流延法成膜,干燥后揭膜,干燥温度为50℃。3. The feature of claim 1 is that the film is formed by casting method, and the film is peeled off after drying, and the drying temperature is 50°C. 权利要求1所述的含抗菌微胶囊的淀粉基薄膜制备方法,其特征在于:将6gβ-环糊精用蒸馏水溶解搅拌形成β-环糊精的饱和溶液,随后将1g丁香精油溶于乙醇并逐滴加入β-环糊精的水溶液中,60℃温度下搅拌2.5小时后取出,待溶液冷至室温后放在4℃的冰箱静置24小时,抽滤,滤渣用无水乙醇和蒸馏水分别洗涤,在50℃温度下干燥,制成丁香精油/β-环糊精抗菌微胶囊备用。然后称取薄膜总重44-50%的淀粉配成溶液,在80℃下糊化20min,加入9-17%的明胶,在60摄氏度下继续搅拌20min,再加入26%的甘油,9-17%抗菌微胶囊以及4-8%CaCl2搅拌反应20min制成膜液,将混合膜液进行消泡,冷却,然后倒入自制模具中,放入50℃恒温干燥箱,干燥至恒重后揭膜。The method for preparing a starch-based film containing antibacterial microcapsules according to claim 1, characterized in that: 6g beta-cyclodextrin is dissolved and stirred in distilled water to form a saturated solution of beta-cyclodextrin, then 1g clove essential oil is dissolved in ethanol and Add dropwise to the aqueous solution of β-cyclodextrin, stir at 60°C for 2.5 hours, take it out, wait for the solution to cool to room temperature, put it in a refrigerator at 4°C for 24 hours, filter it with suction, and use absolute ethanol and distilled water to separate the filter residue Wash and dry at a temperature of 50°C to prepare clove essential oil/β-cyclodextrin antibacterial microcapsules for future use. Then weigh 44-50% of the total weight of the film to make a starch solution, gelatinize at 80°C for 20 minutes, add 9-17% gelatin, continue stirring at 60°C for 20 minutes, then add 26% glycerin, 9-17 % antibacterial microcapsules and 4-8% CaCl 2 were stirred and reacted for 20 minutes to form a film liquid, the mixed film liquid was defoamed, cooled, then poured into a self-made mold, placed in a 50°C constant temperature drying oven, dried to a constant weight, and then exposed membrane. 4.权利要求1所述其成型在自制的专用有机玻璃模具中进行。4. Its molding described in claim 1 is carried out in self-made special organic glass mould.
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CN106905564A (en) * 2017-01-18 2017-06-30 华南理工大学 A kind of feature edible film and preparation method thereof
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CN107280142A (en) * 2017-05-31 2017-10-24 苏州峰佳医疗科技有限公司 Foot orthopedic insoles and preparation method thereof
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CN110055820B (en) * 2019-03-06 2022-02-11 浙江工业大学 A kind of preparation method of functional fresh-keeping paper base material with compound strengthening and slow release
CN110055820A (en) * 2019-03-06 2019-07-26 浙江工业大学 A kind of preparation method of the compound fresh-keeping paper base material of functionality for reinforcing sustained release
CN110078958A (en) * 2019-04-28 2019-08-02 齐鲁工业大学 A kind of preparation method and application of bacteriostatic activity food package film
CN111607018A (en) * 2020-06-05 2020-09-01 江南大学 A kind of preparation method of thymol-embedded intelligent antibacterial fresh-keeping film
CN112553786A (en) * 2020-11-30 2021-03-26 四川农业大学 Antibacterial composite fiber membrane and preparation method and application thereof
CN113334661A (en) * 2021-06-09 2021-09-03 蚌埠学院 Extraction element is used in peppermint essential oil curtain coating film forming
CN114249926A (en) * 2021-12-20 2022-03-29 多麦(福建)食品有限公司 A kind of edible film and preparation method thereof
CN114736436A (en) * 2022-05-09 2022-07-12 吉林大学 Preparation method of antioxidant cyperus esculentus starch composite edible film
CN114711366A (en) * 2022-05-12 2022-07-08 贵州南山婆食品加工有限公司 Plant and physical preservation combined multi-stage preservation method and application
CN114773664A (en) * 2022-05-26 2022-07-22 刘磊 Production method of starch modified plastic film
CN119709317A (en) * 2024-11-27 2025-03-28 中国科学院西双版纳热带植物园 Cinnamomum tenuifolium leaf essential oil and application thereof in preparation of Cinnamomum tenuifolium leaf essential oil preservative film

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