[go: up one dir, main page]

CN103910911B - A kind of preparation method of the long acting antibiotic edible film having slow releasing function - Google Patents

A kind of preparation method of the long acting antibiotic edible film having slow releasing function Download PDF

Info

Publication number
CN103910911B
CN103910911B CN201410119943.6A CN201410119943A CN103910911B CN 103910911 B CN103910911 B CN 103910911B CN 201410119943 A CN201410119943 A CN 201410119943A CN 103910911 B CN103910911 B CN 103910911B
Authority
CN
China
Prior art keywords
essential oil
cyclodextrin
film
long
edible film
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.)
Expired - Fee Related
Application number
CN201410119943.6A
Other languages
Chinese (zh)
Other versions
CN103910911A (en
Inventor
陈国�
刘斌
陈宏文
林毅
张光亚
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Huaqiao University
Original Assignee
Huaqiao University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Huaqiao University filed Critical Huaqiao University
Priority to CN201410119943.6A priority Critical patent/CN103910911B/en
Publication of CN103910911A publication Critical patent/CN103910911A/en
Application granted granted Critical
Publication of CN103910911B publication Critical patent/CN103910911B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Medicinal Preparation (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

本发明公开了一种具缓释作用的长效抗菌可食膜的制备方法。该方法采用纤维素硫酸钠作为基材,天然精油作为抗菌剂,环糊精作为缓释剂和除味剂,经过溶解、均质、脱气、制膜、干燥等步骤,最后制备成一种具缓释精油特性的长效抗菌可食性包装膜。本发明方法可以提高精油的利用率、延长精油的释放时间,制得的可食膜具有良好的机械性能、阻隔性能和长效的抗菌性能,能满足饼干、蛋糕、水果等其它食品包装的要求。The invention discloses a preparation method of a long-acting antibacterial edible film with slow release effect. The method uses cellulose sodium sulfate as the substrate, natural essential oil as the antibacterial agent, and cyclodextrin as the slow-release agent and deodorant. Long-lasting antibacterial edible packaging film with slow-release properties of essential oils. The method of the invention can improve the utilization rate of the essential oil and prolong the release time of the essential oil, and the prepared edible film has good mechanical properties, barrier properties and long-term antibacterial properties, and can meet the packaging requirements of biscuits, cakes, fruits and other foods .

Description

一种具缓释作用的长效抗菌可食膜的制备方法A kind of preparation method of long-acting antibacterial edible film with slow-release effect

技术领域technical field

本发明涉及食品加工领域,更具体的说,是涉及一种可食膜的制备方法。The invention relates to the field of food processing, and more specifically, relates to a preparation method of an edible film.

背景技术Background technique

随着食品自身的安全问题及其包装带来的环境问题日益受到人们的广泛关注,可食膜以其安全、易降解、无环境污染,且可作为营养强化剂、抗菌剂载体等优点,成为食品包装领域研究的热点。可食膜是一种以天然可食性物质(如蛋白质、多糖、脂类等)为原料,以包装或涂布等形式覆盖于食品表面,控制水、氧气及各种溶质的渗透,起保护作用的薄层。可食性膜本身营养较丰富,易滋生微生物,会造成保存过程中产品的机械性能、阻隔性能等质量下降。因此强化可食膜的抗菌功能,可以防止食品及膜本身受到微生物的污染,从而延长食品的货架期。可食性抗菌膜是一种在可食性膜中添加抗菌剂,达到抗菌、保鲜作用的功能性薄膜。With the safety of food itself and the environmental problems brought about by its packaging, people are paying more and more attention to it. Edible film has become a Research hotspots in the field of food packaging. Edible film is a kind of natural edible substance (such as protein, polysaccharide, lipid, etc.) TLC. The edible film itself is rich in nutrients and is easy to breed microorganisms, which will cause a decline in the mechanical properties and barrier properties of the product during storage. Therefore, strengthening the antibacterial function of the edible film can prevent the food and the film itself from being contaminated by microorganisms, thereby prolonging the shelf life of the food. Edible antibacterial film is a functional film that adds antibacterial agents to the edible film to achieve antibacterial and fresh-keeping effects.

添加到可食性膜中的抗菌剂主要包括无机抗菌剂、合成抗菌剂和天然抗菌剂。天然抗菌剂因其特有的安全性优势,更易为消费者所接受。精油作为一种常用的天然抗菌剂之一,因具有良好的抗氧化性和抗菌性能,受到食品生产者和消费者们的共同欢迎。目前含精油类抗菌可食膜的制备方法主要是直接混匀法,这种方法在膜干燥的过程中及膜后期保藏当中,因为精油的易挥发性,会导致精油的大量损失,造成精油的利用率极低,且不能长效抗菌,限制了该类膜的应用。因此,开发一种精油利用率高且能长效抗菌的可食膜的制备方法是十分必要的。Antibacterial agents added to edible films mainly include inorganic antibacterial agents, synthetic antibacterial agents, and natural antibacterial agents. Natural antibacterial agents are more acceptable to consumers because of their unique safety advantages. As one of the commonly used natural antibacterial agents, essential oil is welcomed by food producers and consumers because of its good antioxidant and antibacterial properties. At present, the preparation method of antibacterial edible films containing essential oils is mainly the direct mixing method. This method will cause a large loss of essential oils due to the volatility of the essential oils during the drying process of the films and the later preservation of the films, resulting in the loss of essential oils. The utilization rate is extremely low, and it cannot be antibacterial for a long time, which limits the application of this type of film. Therefore, it is very necessary to develop a method for preparing an edible film with high utilization rate of essential oil and long-acting antibacterial properties.

发明内容Contents of the invention

本发明的目的是为了克服现有精油类抗菌可食膜中精油大量损失的技术问题,提供一种具缓释作用的长效抗菌可食膜的制备方法,可替代或部分替代塑料包装膜,应用于食品包装领域。The purpose of the present invention is to provide a kind of preparation method of the long-acting antibacterial edible film with slow-release effect in order to overcome the technical problem of a large amount of loss of essential oil in the existing essential oil antibacterial edible film, which can replace or partially replace plastic packaging film, Used in the field of food packaging.

一种具缓释作用的长效抗菌可食膜的制备方法,包括如下步骤:A preparation method of a long-acting antibacterial edible film with sustained release, comprising the steps of:

(1)将环糊精加入蒸馏水中,制得环糊精水溶液;(1) Add cyclodextrin to distilled water to obtain cyclodextrin aqueous solution;

(2)在环糊精水溶液中添加精油-乙醇混合液,室温搅拌2-6h,制得环糊精-精油包合物悬浊液;(2) Add the essential oil-ethanol mixture to the cyclodextrin aqueous solution, and stir at room temperature for 2-6 hours to prepare the cyclodextrin-essential oil inclusion compound suspension;

(3)在步骤(2)制得的悬浊液中加入稳定剂,室温搅拌5-30min,制得稳定的环糊精-精油包合物乳浊液;(3) Add a stabilizer to the suspension prepared in step (2), and stir at room temperature for 5-30 minutes to obtain a stable cyclodextrin-essential oil inclusion compound emulsion;

此稳定的环糊精-精油包合物乳浊液中,精油的重量比为0.02-1.2%,环糊精的重量比为0.2-0.8%,乙醇的重量比为0.02-1.2%,稳定剂的重量比为0.02-0.24%;In this stable cyclodextrin-essential oil clathrate emulsion, the weight ratio of essential oil is 0.02-1.2%, the weight ratio of cyclodextrin is 0.2-0.8%, the weight ratio of ethanol is 0.02-1.2%, and the stabilizer The weight ratio is 0.02-0.24%;

(4)在步骤(3)制得的乳浊液中加入纤维素硫酸钠粉末和增塑剂,室温搅拌2-4h,然后真空脱气,制得纤维素硫酸钠-环糊精-精油成膜液;(4) Add cellulose sodium sulfate powder and plasticizer to the emulsion prepared in step (3), stir at room temperature for 2-4 hours, and then vacuum degassing to obtain cellulose sodium sulfate-cyclodextrin-essential oil composition Membrane fluid;

此纤维素硫酸钠-环糊精-精油成膜液中,纤维素硫酸钠粉末的重量比为1-2%,增塑剂的重量比0.15-0.30%;In the cellulose sodium sulfate-cyclodextrin-essential oil film-forming liquid, the weight ratio of the cellulose sodium sulfate powder is 1-2%, and the weight ratio of the plasticizer is 0.15-0.30%;

(5)用步骤(4)制得的成膜液制膜,成型后在25~45℃干燥24-48h,即得到含精油的缓释长效抗菌可食膜。(5) The film-forming solution prepared in step (4) is used to form a film, and after forming, it is dried at 25-45°C for 24-48 hours to obtain a slow-release long-acting antibacterial edible film containing essential oil.

所述的环糊精采用α-环糊精、β-环糊精、γ-环糊精中的一种或多种的组合。Said cyclodextrin adopts one or more combinations of α-cyclodextrin, β-cyclodextrin and γ-cyclodextrin.

所述的天然精油采用芥末精油、牛至精油、肉桂精油、丁香精油、大蒜精油、百里香精油、柠檬香茅精油、佛手柑精油、柠檬精油、茶树精油、迷迭香精油、薄荷精油、洋甘菊精油、酸橙精油、香茅精油、胡荽精油、龙蒿精油、蔷薇精油中的一种或多种的组合。Described natural essential oil adopts mustard essential oil, oregano essential oil, cinnamon essential oil, clove essential oil, garlic essential oil, thyme essential oil, lemongrass essential oil, bergamot essential oil, lemon essential oil, tea tree essential oil, rosemary essential oil, peppermint essential oil, chamomile essential oil , lime essential oil, citronella essential oil, coriander essential oil, tarragon essential oil, rose essential oil in one or more combination.

所述的稳定剂采用吐温-80、吐温-20中的一种或两种的组合。The stabilizer adopts one or a combination of Tween-80 and Tween-20.

所述的纤维素硫酸钠-环糊精-精油成膜液中,所使用的纤维素硫酸钠其重量百分比为2%的水溶液的运动粘度为300-1200mPa·S-1In the cellulose sodium sulfate-cyclodextrin-essential oil film-forming liquid, the kinematic viscosity of the 2% by weight aqueous solution of the cellulose sodium sulfate used is 300-1200mPa·S -1 .

所述增塑剂采用水、甘油、丙二醇、山梨醇、木糖醇、甘露醇、乙二醇、葡萄糖、果糖、蔗糖、柠檬酸中的一种或两种的组合。The plasticizer adopts one or a combination of water, glycerin, propylene glycol, sorbitol, xylitol, mannitol, ethylene glycol, glucose, fructose, sucrose, and citric acid.

采用上述方案后,本发明一种具缓释作用的长效抗菌可食膜的制备方法中,纤维素硫酸钠是纤维素的一种磺化衍生物,具有优良的成膜性能。然而普通的纤维素硫酸钠基可食膜由于其营养较丰富,易滋生微生物,会造成保存过程中产品的机械性能、阻隔性能等质量下降。为了弥补这个缺陷,本发明采用添加天然精油的方式,制备出可以抗微生物的纤维素硫酸钠-精油抗菌复合膜。After adopting the above-mentioned scheme, in the preparation method of a long-acting antibacterial edible film with slow-release effect of the present invention, cellulose sodium sulfate is a sulfonated derivative of cellulose, which has excellent film-forming properties. However, the ordinary cellulose sodium sulfate-based edible film is rich in nutrients and easy to breed microorganisms, which will cause the deterioration of the mechanical properties and barrier properties of the product during storage. In order to make up for this defect, the present invention adopts the mode of adding natural essential oil to prepare antimicrobial cellulose sodium sulfate-essential oil antibacterial composite film.

目前国内外制备含精油的抗菌可食膜方法主要是直接混匀法。直接混匀法具有精油利用率低,且不能长效抗菌等缺点。本发明在制备中添加环糊精,对精油进行包合,然后再与膜基质进行混匀,可以提高精油的利用率,且能够达到缓释长效抗菌的效果。At present, the method of preparing antibacterial edible films containing essential oils at home and abroad is mainly the direct mixing method. The direct mixing method has the disadvantages of low utilization rate of essential oil and incapable of long-acting antibacterial. In the present invention, cyclodextrin is added during the preparation to clathrate the essential oil, and then mix it with the membrane matrix, so that the utilization rate of the essential oil can be improved, and the slow-release and long-acting antibacterial effect can be achieved.

本发明具有如下优点:The present invention has the following advantages:

1、本发明制备的纤维素硫酸钠-环糊精-精油抗菌复合膜具有良好的机械强度、透明度、阻油性、柔韧性和抗老化性能,具有可食性、全降解性和抗菌性能,可避免非降解食品包装对环境的污染和微生物对膜及食品的污染。1. The cellulose sodium sulfate-cyclodextrin-essential oil antibacterial composite film prepared by the present invention has good mechanical strength, transparency, oil resistance, flexibility and anti-aging performance, has edibility, full degradability and antibacterial performance, and can avoid The pollution of non-degradable food packaging to the environment and the pollution of microbes to film and food.

2、本发明在膜的制备过程当中添加缓释剂环糊精,提高了精油的利用率,且能够达到缓释长效抗菌的效果。2. The present invention adds a slow-release agent cyclodextrin in the preparation process of the film, which improves the utilization rate of essential oils and can achieve slow-release and long-acting antibacterial effects.

具体实施方式detailed description

本发明一种具缓释作用的长效抗菌可食膜的制备方法中,环糊精采用α-环糊精、β-环糊精、γ-环糊精中的一种或多种的组合。天然精油采用芥末精油、牛至精油、肉桂精油、丁香精油、大蒜精油、百里香精油、柠檬香茅精油、佛手柑精油、柠檬精油、茶树精油、迷迭香精油、薄荷精油、洋甘菊精油、酸橙精油、香茅精油、胡荽精油、龙蒿精油、蔷薇精油中的一种或多种的组合。稳定剂采用吐温-80、吐温-20中的一种或两种的组合。纤维素硫酸钠-环糊精-精油成膜液中,所使用的纤维素硫酸钠其水溶液(2%w/w)的运动粘度为300-1200mPa·S-1。增塑剂采用水、甘油、丙二醇、山梨醇、木糖醇、甘露醇、乙二醇、葡萄糖、果糖、蔗糖、柠檬酸中的一种或两种的组合。In the preparation method of a long-acting antibacterial edible film with slow-release effect of the present invention, the cyclodextrin is a combination of one or more of α-cyclodextrin, β-cyclodextrin, and γ-cyclodextrin . Natural essential oils are mustard essential oil, oregano essential oil, cinnamon essential oil, clove essential oil, garlic essential oil, thyme essential oil, lemongrass essential oil, bergamot essential oil, lemon essential oil, tea tree essential oil, rosemary essential oil, peppermint essential oil, chamomile essential oil, lime One or a combination of essential oils, citronella essential oils, coriander essential oils, tarragon essential oils, and rose essential oils. The stabilizer adopts one or a combination of Tween-80 and Tween-20. In the cellulose sodium sulfate-cyclodextrin-essential oil film-forming liquid, the kinematic viscosity of the aqueous solution (2% w/w) of the cellulose sodium sulfate used is 300-1200mPa·S -1 . The plasticizer adopts one or a combination of water, glycerin, propylene glycol, sorbitol, xylitol, mannitol, ethylene glycol, glucose, fructose, sucrose, and citric acid.

实施例1:Example 1:

(1)将0.2gβ-环糊精加入100ml蒸馏水中,制得β-环糊精水溶液;(1) Add 0.2g of β-cyclodextrin to 100ml of distilled water to prepare an aqueous solution of β-cyclodextrin;

(2)在步骤(1)制得的β-环糊精水溶液中添加0.04ml芥茉精油与乙醇的混合液,其中芥茉精油与乙醇的体积比为1:1,25℃电磁搅拌2h,制得β-环糊精-芥茉精油包合物悬浊液;(2) Add 0.04ml of a mixture of mustard essential oil and ethanol to the β-cyclodextrin aqueous solution prepared in step (1), wherein the volume ratio of mustard essential oil to ethanol is 1:1, and stir electromagnetically at 25°C for 2 hours. Prepare β-cyclodextrin-mustard essential oil clathrate suspension;

(3)在步骤(2)制得的悬浊液中加入0.02ml的吐温-80,搅拌5min,制得稳定的β-环糊精-芥茉精油包合物乳浊液;(3) Add 0.02ml of Tween-80 to the suspension prepared in step (2), and stir for 5 minutes to obtain a stable β-cyclodextrin-mustard essential oil inclusion compound emulsion;

(4)在步骤(3)制得的乳浊液中加入2g纤维素硫酸钠粉末和0.3g甘油,搅拌2h,然后真空脱气,制得纤维素硫酸钠-β-环糊精-芥茉精油成膜液;(4) Add 2g of cellulose sodium sulfate powder and 0.3g of glycerin to the emulsion prepared in step (3), stir for 2 hours, and then vacuum degassing to obtain sodium cellulose sulfate-β-cyclodextrin-mustard Essential oil film-forming liquid;

(5)将步骤(4)制得的成膜液倾倒在光滑的聚丙烯塑料板上制膜,成型后在30℃干燥48h,可制得厚度为30μm、抗大肠杆菌的具缓释作用的长效抗菌可食膜。(5) Pour the film-forming solution prepared in step (4) onto a smooth polypropylene plastic plate to form a film, and dry it at 30°C for 48 hours after molding to obtain a slow-release film with a thickness of 30 μm and anti-Escherichia coli Long-lasting antibacterial edible film.

将制得的可食膜与表面涂有大肠杆菌的琼脂培养基平板,共同置于密闭容器中,60天无大肠杆菌菌落生成。The prepared edible film and the agar medium plate coated with Escherichia coli on the surface were placed in a closed container together, and no Escherichia coli colony was formed in 60 days.

实施例2:Example 2:

本实施例与实施例1的区别仅在于:γ-环糊精的用量为0.6g,芥茉精油-乙醇混合液的用量为0.36ml,吐温-80的用量为0.04ml。其余条件同实施例1。可制得厚度为35μm、抗大肠杆菌和金黄色葡萄球菌的具缓释作用的长效抗菌可食膜。The difference between this example and Example 1 is that the dosage of γ-cyclodextrin is 0.6g, the dosage of mustard essential oil-ethanol mixture is 0.36ml, and the dosage of Tween-80 is 0.04ml. All the other conditions are with embodiment 1. A long-acting antibacterial edible film with a thickness of 35 μm, anti-Escherichia coli and Staphylococcus aureus with slow release effect can be prepared.

将制得的可食膜、表面涂有大肠杆菌的琼脂培养基平板和金黄色葡萄球菌的琼脂培养基平板,共同置于密闭容器中,60天未观察到金黄色葡萄球菌菌落和大肠杆菌菌落。The prepared edible film, the agar medium plate coated with Escherichia coli and the agar medium plate of Staphylococcus aureus were placed together in an airtight container, and Staphylococcus aureus colonies and Escherichia coli colonies were not observed in 60 days .

实施例3:Example 3:

(1)将0.6gβ-环糊精加入100ml蒸馏水中,制得β-环糊精水溶液;(1) Add 0.6g of β-cyclodextrin to 100ml of distilled water to prepare an aqueous solution of β-cyclodextrin;

(2)在步骤(1)制得的β-环糊精水溶液中添加0.8ml牛至精油与乙醇的混合液,其中牛至精油与乙醇的体积比为1:1比,25℃电磁搅拌4h,制得β-环糊精-牛至精油包合物悬浊液;(2) Add 0.8ml of a mixture of oregano essential oil and ethanol to the β-cyclodextrin aqueous solution prepared in step (1), wherein the volume ratio of oregano essential oil and ethanol is 1:1, and stir electromagnetically at 25°C for 4 hours , making β-cyclodextrin-oregano essential oil clathrate suspension;

(3)在步骤(2)制得的悬浊液中加入0.08ml的吐温-80,搅拌10min,制得稳定的β-环糊精-牛至精油包合物乳浊液;(3) Add 0.08ml of Tween-80 to the suspension prepared in step (2), and stir for 10 minutes to prepare a stable β-cyclodextrin-oregano essential oil inclusion compound emulsion;

(4)在步骤(3)制得的乳浊液中加入1g纤维素硫酸钠粉末和0.15g甘油,搅拌2h,然后真空脱气,制得纤维素硫酸钠-β-环糊精-牛至精油成膜液;(4) Add 1g of cellulose sodium sulfate powder and 0.15g of glycerin to the emulsion prepared in step (3), stir for 2 hours, and then vacuum degassing to prepare sodium cellulose sulfate-β-cyclodextrin-oregano Essential oil film-forming liquid;

(5)将步骤(4)制得的成膜液倾倒在光滑的聚丙烯塑料板上制膜,成型后在25℃干燥48h,可制得厚度为40μm、抗大肠杆菌和金黄色葡萄球菌的具缓释作用的长效抗菌可食膜。(5) Pour the film-forming solution prepared in step (4) onto a smooth polypropylene plastic plate to form a film, and dry it at 25°C for 48 hours after molding to obtain a film with a thickness of 40 μm and resistance to Escherichia coli and Staphylococcus aureus. Long-acting antibacterial edible film with sustained release.

将制得的可食膜、表面涂有大肠杆菌的琼脂培养基平板和金黄色葡萄球菌的琼脂培养基平板,共同置于密闭容器中,60天未观察到金黄色葡萄球菌菌落和大肠杆菌菌落。The prepared edible film, the agar medium plate coated with Escherichia coli and the agar medium plate of Staphylococcus aureus were placed together in an airtight container, and Staphylococcus aureus colonies and Escherichia coli colonies were not observed in 60 days .

实施例4:Example 4:

(1)将0.6gβ-环糊精加入100ml蒸馏水中,制得β-环糊精水溶液;(1) Add 0.6g of β-cyclodextrin to 100ml of distilled water to prepare an aqueous solution of β-cyclodextrin;

(2)在步骤(1)制得的环糊精水溶液中添加1.2ml丁香精油与乙醇的混合液,其中丁香精油与乙醇的体积比为1:1,25℃电磁搅拌6h,制得β-环糊精-丁香精油包合物悬浊液;(2) Add 1.2ml of a mixture of clove essential oil and ethanol to the cyclodextrin aqueous solution prepared in step (1), wherein the volume ratio of clove essential oil to ethanol is 1:1, and stir electromagnetically at 25°C for 6 hours to obtain β- Cyclodextrin-clove essential oil clathrate suspension;

(3)在步骤(2)制得的悬浊液中加入0.12ml的吐温-20,搅拌10min,制得稳定的β-环糊精-丁香精油包合物乳浊液;(3) Add 0.12ml of Tween-20 to the suspension prepared in step (2), and stir for 10 minutes to obtain a stable β-cyclodextrin-clove essential oil inclusion compound emulsion;

(4)在步骤(3)制得的乳浊液中加入2g纤维素硫酸钠粉末和0.3g甘油,搅拌2h,然后真空脱气,制得纤维素硫酸钠-β-环糊精-丁香精油成膜液;(4) Add 2g of sodium cellulose sulfate powder and 0.3g of glycerin to the emulsion prepared in step (3), stir for 2 hours, and then vacuum degassing to obtain sodium cellulose sulfate-β-cyclodextrin-clove essential oil Film-forming liquid;

(5)将步骤(4)制得的成膜液倾倒在光滑的聚丙烯塑料板上制膜,成型后在30℃干燥40h,可制得厚度为44μm、抗大肠杆菌和金黄色葡萄球菌的具缓释作用的长效抗菌可食膜。(5) Pour the film-forming solution prepared in step (4) onto a smooth polypropylene plastic plate to form a film, and dry it at 30°C for 40 hours after molding to obtain a film with a thickness of 44 μm and resistance to Escherichia coli and Staphylococcus aureus. Long-acting antibacterial edible film with sustained release.

将制得的可食膜、表面涂有大肠杆菌的琼脂培养基平板和金黄色葡萄球菌的琼脂培养基平板,共同置于密闭容器中,60天未观察到金黄色葡萄球菌菌落和大肠杆菌菌落。The prepared edible film, the agar medium plate coated with Escherichia coli and the agar medium plate of Staphylococcus aureus were placed together in an airtight container, and Staphylococcus aureus colonies and Escherichia coli colonies were not observed in 60 days .

实施例5:Example 5:

(1)将0.6gα-环糊精加入100ml蒸馏水中,制得α-环糊精水溶液;(1) Add 0.6g of α-cyclodextrin to 100ml of distilled water to prepare an aqueous solution of α-cyclodextrin;

(2)在步骤(1)制得的β-环糊精水溶液中添加0.8ml牛至精油与乙醇的混合液,其中牛至精油与乙醇的体积比为1:1比,25℃电磁搅拌4h,制得β-环糊精-牛至精油包合物悬浊液;(2) Add 0.8ml of a mixture of oregano essential oil and ethanol to the β-cyclodextrin aqueous solution prepared in step (1), wherein the volume ratio of oregano essential oil and ethanol is 1:1, and stir electromagnetically at 25°C for 4 hours , making β-cyclodextrin-oregano essential oil clathrate suspension;

(3)在步骤(2)制得的悬浊液中加入0.08ml的吐温-80,搅拌10min,制得稳定的β-环糊精-牛至精油包合物乳浊液;(3) Add 0.08ml of Tween-80 to the suspension prepared in step (2), and stir for 10 minutes to prepare a stable β-cyclodextrin-oregano essential oil inclusion compound emulsion;

(4)在步骤(3)制得的乳浊液中加入2g纤维素硫酸钠粉末和0.2g甘油,搅拌2h,然后真空脱气,制得纤维素硫酸钠-α-环糊精-牛至精油成膜液;(4) Add 2g of cellulose sodium sulfate powder and 0.2g of glycerin to the emulsion prepared in step (3), stir for 2 hours, and then vacuum degassing to obtain cellulose sulfate sodium-α-cyclodextrin-oregano Essential oil film-forming liquid;

(5)将步骤(4)制得的成膜液倾倒在光滑的聚丙烯塑料板上制膜,成型后在35℃干燥24h,可制得厚度为40μm、抗大肠杆菌和金黄色葡萄球菌的具缓释作用的长效抗菌可食膜。(5) Pour the film-forming solution prepared in step (4) onto a smooth polypropylene plastic plate to form a film, and dry it at 35°C for 24 hours after molding to obtain a film with a thickness of 40 μm and resistance to Escherichia coli and Staphylococcus aureus. Long-acting antibacterial edible film with sustained release.

将制得的可食膜、表面涂有大肠杆菌的琼脂培养基平板和金黄色葡萄球菌的琼脂培养基平板,共同置于密闭容器中,60天未观察到金黄色葡萄球菌菌落和大肠杆菌菌落。The prepared edible film, the agar medium plate coated with Escherichia coli and the agar medium plate of Staphylococcus aureus were placed together in an airtight container, and Staphylococcus aureus colonies and Escherichia coli colonies were not observed in 60 days .

Claims (6)

1.一种具缓释作用的长效抗菌可食膜的制备方法,其特征在于:包括如下步骤:1. a kind of preparation method of the long-acting antibacterial edible film of tool slow release, it is characterized in that: comprise the steps: (1)将环糊精加入蒸馏水中,制得环糊精水溶液;(1) Add cyclodextrin to distilled water to obtain cyclodextrin aqueous solution; (2)在环糊精水溶液中添加精油-乙醇混合液,室温搅拌2-6h,制得环糊精-精油包合物悬浊液;(2) Add the essential oil-ethanol mixture to the cyclodextrin aqueous solution, and stir at room temperature for 2-6 hours to prepare the cyclodextrin-essential oil inclusion compound suspension; (3)在步骤(2)制得的悬浊液中加入稳定剂,室温搅拌5-30min,制得稳定的环糊精-精油包合物乳浊液;(3) Add a stabilizer to the suspension prepared in step (2), and stir at room temperature for 5-30 minutes to obtain a stable cyclodextrin-essential oil inclusion compound emulsion; 此稳定的环糊精-精油包合物乳浊液中,精油的重量比为0.02-1.2%,环糊精的重量比为0.2-0.8%,乙醇的重量比为0.02-1.2%,稳定剂的重量比为0.02-0.24%;In this stable cyclodextrin-essential oil clathrate emulsion, the weight ratio of essential oil is 0.02-1.2%, the weight ratio of cyclodextrin is 0.2-0.8%, the weight ratio of ethanol is 0.02-1.2%, and the stabilizer The weight ratio is 0.02-0.24%; (4)在步骤(3)制得的乳浊液中加入纤维素硫酸钠粉末和增塑剂,室温搅拌2-4h,然后真空脱气,制得纤维素硫酸钠-环糊精-精油成膜液;(4) Add cellulose sodium sulfate powder and plasticizer to the emulsion prepared in step (3), stir at room temperature for 2-4 hours, and then vacuum degassing to obtain cellulose sodium sulfate-cyclodextrin-essential oil composition Membrane fluid; 此纤维素硫酸钠-环糊精-精油成膜液中,纤维素硫酸钠粉末的重量比为1-2%,增塑剂的重量比0.15-0.30%;In the cellulose sodium sulfate-cyclodextrin-essential oil film-forming liquid, the weight ratio of the cellulose sodium sulfate powder is 1-2%, and the weight ratio of the plasticizer is 0.15-0.30%; (5)用步骤(4)制得的成膜液制膜,成型后在25~45℃干燥24-48h,即得到具缓释作用的长效抗菌可食膜。(5) Use the film-forming solution prepared in step (4) to form a film, and dry it at 25-45°C for 24-48 hours after forming to obtain a long-acting antibacterial edible film with slow-release effect. 2.根据权利要求1所述的一种具缓释作用的长效抗菌可食膜的制备方法,其特征在于:所述的环糊精采用α-环糊精、β-环糊精、γ-环糊精中的一种或多种的组合。2. The preparation method of a long-acting antibacterial edible film with slow-release effect according to claim 1, characterized in that: the cyclodextrin adopts α-cyclodextrin, β-cyclodextrin, γ-cyclodextrin - one or more combinations of cyclodextrins. 3.根据权利要求1所述的一种具缓释作用的长效抗菌可食膜的制备方法,其特征在于:所述的天然精油采用芥末精油、牛至精油、肉桂精油、丁香精油、大蒜精油、百里香精油、柠檬香茅精油、佛手柑精油、柠檬精油、茶树精油、迷迭香精油、薄荷精油、洋甘菊精油、酸橙精油、香茅精油、胡荽精油、龙蒿精油、蔷薇精油中的一种或多种的组合。3. the preparation method of a kind of long-acting antibacterial edible film of tool sustained release according to claim 1, is characterized in that: described natural essential oil adopts mustard essential oil, oregano essential oil, cinnamon essential oil, clove essential oil, garlic Essential oils, thyme essential oil, lemongrass essential oil, bergamot essential oil, lemon essential oil, tea tree essential oil, rosemary essential oil, peppermint essential oil, chamomile essential oil, lime essential oil, citronella essential oil, coriander essential oil, tarragon essential oil, rose essential oil one or a combination of more. 4.根据权利要求1所述的一种具缓释作用的长效抗菌可食膜的制备方法,其特征在于:所述的稳定剂采用吐温-80、吐温-20中的一种或两种的组合。4. The preparation method of a long-acting antibacterial edible film with slow-release effect according to claim 1, characterized in that: the stabilizing agent adopts one of Tween-80, Tween-20 or A combination of the two. 5.根据权利要求1所述的一种具缓释作用的长效抗菌可食膜的制备方法,其特征在于:所述的纤维素硫酸钠-环糊精-精油成膜液中,所使用的纤维素硫酸钠其重量百分比为2%的水溶液的运动粘度为300-1200mPa·S-15. The preparation method of a long-acting antibacterial edible film with sustained release according to claim 1, characterized in that: in the described sodium cellulose sulfate-cyclodextrin-essential oil film-forming liquid, the used The kinematic viscosity of 2% aqueous solution of sodium cellulose sulfate by weight is 300-1200mPa·S -1 . 6.根据权利要求1所述的一种具缓释作用的长效抗菌可食膜的制备方法,其特征在于:所述增塑剂采用水、甘油、丙二醇、山梨醇、木糖醇、甘露醇、乙二醇、葡萄糖、果糖、蔗糖、柠檬酸中的一种或两种的组合。6. the preparation method of a kind of long-acting antibacterial edible film of tool slow-release according to claim 1, is characterized in that: described plasticizer adopts water, glycerin, propylene glycol, sorbitol, xylitol, sweet dew Alcohol, ethylene glycol, glucose, fructose, sucrose, citric acid or a combination of two.
CN201410119943.6A 2014-03-27 2014-03-27 A kind of preparation method of the long acting antibiotic edible film having slow releasing function Expired - Fee Related CN103910911B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410119943.6A CN103910911B (en) 2014-03-27 2014-03-27 A kind of preparation method of the long acting antibiotic edible film having slow releasing function

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410119943.6A CN103910911B (en) 2014-03-27 2014-03-27 A kind of preparation method of the long acting antibiotic edible film having slow releasing function

Publications (2)

Publication Number Publication Date
CN103910911A CN103910911A (en) 2014-07-09
CN103910911B true CN103910911B (en) 2016-10-05

Family

ID=51036949

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410119943.6A Expired - Fee Related CN103910911B (en) 2014-03-27 2014-03-27 A kind of preparation method of the long acting antibiotic edible film having slow releasing function

Country Status (1)

Country Link
CN (1) CN103910911B (en)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104441899B (en) * 2014-12-03 2016-08-17 华侨大学 Meet water sensitivity, the preparation method of high-efficiency antimicrobial laminated film
CN104910502B (en) * 2015-06-03 2017-10-27 上海海洋大学 Slow release food fresh keeping film and preparation method thereof
CN105111511B (en) * 2015-07-31 2017-12-19 河南科技大学 A kind of compound edible film of antimicrobial nano and preparation method thereof
CL2015003698A1 (en) * 2015-12-22 2016-06-17 Univ Santiago Chile Degradable film for packaging of fruits and vegetables comprising a polymer matrix based on polyolefin, which incorporates an antimicrobial active agent (biocide or fungicide) of essential oil or said essential oil, and also incorporates degrading agents, and microencapsulation process of said Active antimicrobial essential oil agent, and film preparation method.
CN106857713A (en) * 2017-02-23 2017-06-20 东莞市隆威实业有限公司 A kind of essential oil composition of antibacterial and mouldproof and the packing film using its preparation
CN106929940A (en) * 2017-03-24 2017-07-07 李军 The spinning fabric and its preparation technology of a kind of delicate fragrance antibacterial
CN107198769A (en) * 2017-05-04 2017-09-26 艾伯尔生物科技(重庆)有限公司 Oral disinfecting spray and preparation method thereof
CN107372778A (en) * 2017-08-14 2017-11-24 内蒙古农业大学 A kind of antibacterial pad fresh-keeping for cold fresh meat and preparation method thereof
CN107691636A (en) * 2017-09-22 2018-02-16 中国热带农业科学院海口实验站 A kind of fruit antistaling agent and preparation method thereof and preservation method
CN108384064B (en) * 2018-02-05 2020-11-03 广西大学 A kind of bagasse-based nano antibacterial fresh-keeping film and preparation method thereof
CN111019173B (en) * 2019-12-31 2021-05-04 江南大学 A kind of preparation method of degradable polylactic acid-glycolic acid composite material
CN113082119A (en) * 2021-04-24 2021-07-09 孙乐河 Antibacterial agent for resisting escherichia coli and preparation method thereof

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101501052A (en) * 2006-06-13 2009-08-05 嘉吉公司 Large-particle cyclodextrin inclusion complexes and methods of preparing same
CN102585412A (en) * 2011-01-14 2012-07-18 邓靖 Active packaging film based on essential oil/beta-cyclodextrin inclusion compound and preparation method for active packaging film
CN102703221A (en) * 2012-05-29 2012-10-03 商洛学院 Preparation method of rose essence beta-cyclodextrin polymer microsphere inclusion compound
CN102794139A (en) * 2012-08-28 2012-11-28 河南省科学院化学研究所有限公司 Controlled-release osmanthus essential oil molecule microcapsule inclusion compound and preparation method thereof
CN102847102A (en) * 2012-08-16 2013-01-02 重庆灵方生物科技有限公司 Preparation method of zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate and preparation method of zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate injection
CN102925290A (en) * 2012-11-21 2013-02-13 广东省微生物研究所 Litsea cubeba essential oil inclusion compound and preparation method thereof
CN103170286A (en) * 2013-01-30 2013-06-26 天津商业大学 Method for preparing melissa officinalis L. essential oil and beta-cyclodextrin molecule microcapsule
CN103263651A (en) * 2013-05-25 2013-08-28 江苏丰园生物技术有限公司 Fresh ginger essential oil and mixed cyclodextrin inclusion compound and preparation method thereof
CN103271991A (en) * 2013-05-25 2013-09-04 江苏丰园生物技术有限公司 Peppermint essential oil and mixed cyclodextrin inclusion compound and preparation method thereof
CN103283828A (en) * 2013-06-24 2013-09-11 湖南工业大学 Preparation method for essential oil/beta-cyclodextrin inclusion based antibacterial fruit wax
CN103360499A (en) * 2012-04-11 2013-10-23 厦门大学 Simple synthesis process of cellulose sulfate

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101501052A (en) * 2006-06-13 2009-08-05 嘉吉公司 Large-particle cyclodextrin inclusion complexes and methods of preparing same
CN102585412A (en) * 2011-01-14 2012-07-18 邓靖 Active packaging film based on essential oil/beta-cyclodextrin inclusion compound and preparation method for active packaging film
CN103360499A (en) * 2012-04-11 2013-10-23 厦门大学 Simple synthesis process of cellulose sulfate
CN102703221A (en) * 2012-05-29 2012-10-03 商洛学院 Preparation method of rose essence beta-cyclodextrin polymer microsphere inclusion compound
CN102847102A (en) * 2012-08-16 2013-01-02 重庆灵方生物科技有限公司 Preparation method of zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate and preparation method of zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate injection
CN102794139A (en) * 2012-08-28 2012-11-28 河南省科学院化学研究所有限公司 Controlled-release osmanthus essential oil molecule microcapsule inclusion compound and preparation method thereof
CN102925290A (en) * 2012-11-21 2013-02-13 广东省微生物研究所 Litsea cubeba essential oil inclusion compound and preparation method thereof
CN103170286A (en) * 2013-01-30 2013-06-26 天津商业大学 Method for preparing melissa officinalis L. essential oil and beta-cyclodextrin molecule microcapsule
CN103263651A (en) * 2013-05-25 2013-08-28 江苏丰园生物技术有限公司 Fresh ginger essential oil and mixed cyclodextrin inclusion compound and preparation method thereof
CN103271991A (en) * 2013-05-25 2013-09-04 江苏丰园生物技术有限公司 Peppermint essential oil and mixed cyclodextrin inclusion compound and preparation method thereof
CN103283828A (en) * 2013-06-24 2013-09-11 湖南工业大学 Preparation method for essential oil/beta-cyclodextrin inclusion based antibacterial fruit wax

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
壳聚糖/纤维素硫酸钠复合膜性能的研究;朱丽英等;《食品与生物技术学报》;20121231;第31卷(第2期);全文 *
层层自组装纤维素硫酸钠-壳聚糖复合膜;谢瑜亮;《化工学报》;20081130;第59卷(第11期);全文 *

Also Published As

Publication number Publication date
CN103910911A (en) 2014-07-09

Similar Documents

Publication Publication Date Title
CN103910911B (en) A kind of preparation method of the long acting antibiotic edible film having slow releasing function
Figueroa-Lopez et al. Development of electrospun active films of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) by the incorporation of cyclodextrin inclusion complexes containing oregano essential oil
Qu et al. A review on the preparation and characterization of chitosan-clay nanocomposite films and coatings for food packaging applications
CN107840981A (en) A kind of sodium alginate chitosan bilayer edible film, its preparation method and its application
CN102786702B (en) Preparation method of controlled release antibacterial film
CN104558663B (en) A kind of film and preparation method thereof with excellent antibacterial and degradability
CN109233161A (en) A method of it adding garlic oil-beta cyclodextrin clathrate-caryophyllus oil and prepares antibacterial food fresh-keeping film
Kumar et al. Halloysite nanotube as a functional material for active food packaging application: a review
CN104479155A (en) Preparation method of chitosan/titanium dioxide sol antibacterialpackaging film
CN110591314A (en) A kind of preparation method of controlled-release antibacterial active polylactic acid packaging film
CN104098793B (en) A kind of cm-chitosan natural complex fresh-keeping film and preparation method thereof
CN109566954A (en) A kind of liposome/chitosan anti-bacteria, anti-oxidant coating liquid and preparation method and application embedding laurin oil and nano silver
CN105968511A (en) Sustained-release antioxidant food packaging film and method for preparing same
Fernandes Nassar et al. Soy protein isolate nanocomposite film enriched with eugenol, an antimicrobial agent: Interactions and properties
CN108752610A (en) A kind of edibility antibacterial film and preparation method thereof of sustained release essential oil
CN102604343A (en) Food antimicrobial packaging material with slow release performance and preparation method of food antimicrobial packaging material
CN106867038A (en) A kind of anti-bacterial packaging film and preparation method thereof
CN114411331A (en) Nanometer film added with oregano essential oil cyclodextrin inclusion compound and preparation method and application thereof
JP4683925B2 (en) Humidity-dependent antibacterial powder composition, method for producing the same, humidity-dependent antibacterial food preservation article, and food preservation method
CN103254471B (en) A kind of edibility film using chitosan-sodium tripolyphosphate nanoparticle as matrix and preparation method thereof
Salar Behrestaghi et al. Physical, mechanical, and antimicrobial properties of carboxymethyl cellulose edible films activated with artemisia sieberi essential oil
CN109021262A (en) A kind of immobilized pickering emulsion bacteriostatic film and its preparation method and application
CN115353655B (en) Preparation method and application of edible antibacterial film composite material
CN103172892A (en) Preparation method for biomass antibacterial plastic products
Chen et al. Progress in release‐activated food packaging films

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20161005

Termination date: 20200327

CF01 Termination of patent right due to non-payment of annual fee