醋酸酯淀粉抗菌薄膜的制备及其性质研究
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摘要
抗菌活性包装材料是近二十年发展起来的一种新型活性包装材料。将能抑制或杀灭微生物的抗菌剂加入到环境友好型基材中,制备抗菌活性包装材料应用于食品包装,可抑制食品中微生物的滋生,防止环境微生物对食品的干扰,提高食品的安全性并延长货架期,是一种具有发展潜力的活性包装材料。
本论文在淀粉分子中引入疏水性乙酰基团,改性后得到醋酸酯淀粉,制备疏水性的淀粉薄膜;考察不同抗菌剂的抗菌活性,筛选出活性高的抗菌剂,加入到醋酸酯淀粉薄膜中,制备出淀粉抗菌薄膜材料;通过分析抗菌剂从薄膜中的溶出规律及抗菌材料的抗菌活性,得出了基材对抗菌剂溶出的影响规律,为淀粉基抗菌材料的应用和发展提供理论基础;此外还考察了抗菌材料的热性能和力学性能,为淀粉基抗菌薄膜实际应用于肉肠包装提供了理论依据。
由于天然淀粉分子中含有大量亲水性羟基,使淀粉材料的防水性和耐湿性不能满足包装应用要求。本论文采用化学改性法在淀粉分子中引入了疏水性乙酰基团,合成了几种不同取代度的醋酸酯淀粉。接触角测试结果显示高取代度的醋酸酯淀粉的疏水性很强,取代度为2.9的醋酸酯淀粉的接触角为82.54°,但仍显微弱的吸湿性,为醋酸酯淀粉调控抗菌薄膜中抗菌剂的溶出提供了依据。XRD结果表明酯化后的淀粉结晶结构转变为V型,说明淀粉分子间的氢键被削弱,有序化结晶结构被破坏,趋于无序化。热性能及力学性能分析表明醋酸酯化淀粉具有较好的成膜性及可塑性。
论文筛选出了三种强抗菌能力及耐热性的抗菌剂,分别为水不溶性壳聚糖A、水溶性壳聚糖C及壳寡糖E,且热处理对它们的抗菌活性影响不大。将筛选出的这三种抗菌剂分别添加到取代度为2.5的改性淀粉中,制备出几种醋酸酯淀粉抗菌薄膜,并对比它们的溶出及抗菌能力。30℃、30rpm下加速溶出144h结果显示,不溶性壳聚糖A膜基本不溶出,可溶性壳聚糖C膜及壳寡糖E膜溶出性较好,均在24h时溶出率近40%,之后缓慢溶出,144h时C膜及E膜的溶出率分别为45%及60%。三种膜的抗菌性能与之相吻合,A膜抗菌能力很差,基本上没有抗菌效果,C膜及E膜较显著,尤其E膜。说明醋酸酯淀粉抗菌膜中抗菌剂的溶出能力与抗菌能力相对应。膜中的抗菌剂越易迁移溶出,膜的抗菌能力越强。薄膜材料越亲水,薄膜中抗菌剂越易迁移溶出。然而,抗菌剂过快溶出,则维持不了薄膜材料的长效抗菌性,因此,控缓释溶出速率是决定抗菌薄膜材料抗菌时效性及长效性的关键。
采用DMA、拉伸测试仪分析了影响醋酸酯淀粉抗菌薄膜热性能及力学性能的主要因素。结果显示增塑剂添加量对薄膜的玻璃化转变温度Tg影响很大,增塑剂添加量越高,Tg越低,40%添加量时,Tg接近室温。力学性能结果表明壳聚糖抗菌剂可提高淀粉基薄膜材料的力学性能。
综上所述,本论文采用乙酰化反应塑化淀粉分子,制备了不同取代度及亲疏水性能的醋酸酯淀粉,并筛选出了对大肠杆菌及金黄色葡萄球菌抗菌率均在90%以上的几种抗菌剂,采用流涎法制备了高抗菌活性的醋酸酯淀粉抗菌薄膜。考察了影响薄膜中抗菌剂溶出及抗菌能力的主要因素。通过调节薄膜的厚度、增塑剂用量、改性淀粉取代度等,得到了模拟肉肠环境下强防腐抗菌能力的抗菌活性包装薄膜材料,为控缓释性抗菌活性材料应用于食品领域提供了工艺条件及理论依据。
Packing material of antimicrobial activity is a new pattern activity material which is developing in recent twenty years. If the packing material of antimicrobiol activity which is made by base material of environmental friendly with antibacterialagent is used in Food Packing, it would substitute some use of preservatives in food. Because the packing material of antimicrobiol activity is could not only avoid microbe disturbing food, but also improve the safety of food and prolong its shelf life. So it has been considered as a development potential activity packing material. As people’s life become better and better, the quantity demand of delicious sausages become more and more. While the sterilizing effection is not very satisfied and the additive of preservatives for sausages are always get out of line. Both of the problems are the hot spots recently and should be solved as soon as possible.
In the thesis, firstly prepared the starch acetate by modifing starch with hydrophobicity acetyls. Secondly, according to characters of sausages as Water activity, pH value, and so on, built the imitating medium model of suasage. Thirdly, screened out antibacterialagents with strong ability of antibiotic. Then maked out antibiosis material of starch acetate for sausage packaging. As analyzing dissolving out rule for antibacterialagents coming out from film, and the relation with film’s antibiosis capacity, conclude that the base material could control and slow release of antibacterialagent coming out from film. What’s more, the aspects of thermal behavior, crystallize character, and other aspects have been researched in system, which provide theory basis for starch base film applied to sausage packaging.
As natural starch molecules own lots of hydrophily hydroxies, so that the waterproofness and moisture-proof of starch material cann’t satisfy application requirements for sausage packaging. What’s else, natural starch’s melting temperature nears to its decomposition temperature, so it also doesn't have plasticity. In the thesis, the natural starch molecules have been modified by lipophilicity acetyl groups, and composed several acetate starches with different degrees. Results of Contact Angle Test show that hydrophobicity of starch acetate with high degree is strong. When the degree of starch acetate reaches to 2.9, the largest contact angle of it would be 82.54. While the material also apparents weak hygroscopic. Which could provide judging for dissolving out rule of antibacterialagents from antibiosis film by regulating and controlling. XRD result manifests that natural starch’s crystal structure has been changed to V. So hydrogen bonds of starch molecules have been weakened, and the structure’s ordering tends to disorder. Thermal and mechanical properties analysis show that starch acetate is good at becoming film and plasticity.
In the research, three antimicrobials including non water-soluble chitosan A, water-soluble chitosan C, and oligochitosan E have been selected out, which not only are good at antibacterial activity and thermostability, but also their antibacterial activity doesn’t effect greatly by high degree of temperature. All of them have been mixed to modified starch with degree of 2.5, and maked antimicrobial film of acetate starch out. After that, compared their dissolving out regularity to their antibacterial ability. The conclusion of accelerate dissolution test by temperature of 30℃and rate of 30rpm showed that non water-soluble chitosan A basically couldn’t dissolve out. While water-soluble chitosan C and oligochitosan E could dissolve out better. Both of them could dissolve out from base material nearly 40% in 24 hours, and then dissolve out slowly that dissolving rate respectively are 45% and 60% for film C and E in 144 hours. The three kinds of film’s antimicrobial ability agree with their dissolving regularity. Film A is bad at antimicrobial effection, while film C and E are good at it, especially film E. So acetate starch antimicrobial film’s dissolving energy is corresponding to its antimicrobial ability. If antimicrobialagents came out easier from film, the film’s antimicrobial energy would be stronger. If the film was more hydrophily, the film’s antimicrobialagents would dissolve out easier. But if the rate of antimicrobialagents dissolved out was too fast, the film wouldn’t maintain its long-term antibacterial properties. So the rate of control and release dissolving is the key for deciding antibacterial film material’s antibacterial timeliness and long-lasting.
DMA and Instron Tensile Tester were used to analysis the influence factors of acetate starch antimicrobial film’s thermal and mechanical properties. The results show that plasticizers’quantity influence glass transition temperature Tg of film greatly. The more quantity of plasticizers, the lower of film’s Tg. When the quantity reaches to 40%, Tg nears to room temperature. Mechanical property result showes that chitosan could increase mechanical properties of starch film.
From the above, the thesis modifies natural starch with acetyl and makes out acetate starch with different degree and characters of hydrophibic and hydrophobic. Then screening out several antimicrobialagents which could reach antibacterial rates of Escherichia coli and Staphylococcus aureus above 90%. Using the method of Tape Casting maked out the high antibacterial activity film of acetate starch. The mainly factors which could effect antibacterialagents' dissolution and antibiosis energy have been investigated. Via accommodating film’s thickness, quantity of plasticizers, degree of modified starch, and other conditions, could gain antibacterial activity packaging film which own strong antibacterial activity at the condition of imitating sausage environment. So that could provide the conditions of processing technology and theoretical basis for antimicrobial activity material of control and release character which would apply in the food field.
本论文在淀粉分子中引入疏水性乙酰基团,改性后得到醋酸酯淀粉,制备疏水性的淀粉薄膜;考察不同抗菌剂的抗菌活性,筛选出活性高的抗菌剂,加入到醋酸酯淀粉薄膜中,制备出淀粉抗菌薄膜材料;通过分析抗菌剂从薄膜中的溶出规律及抗菌材料的抗菌活性,得出了基材对抗菌剂溶出的影响规律,为淀粉基抗菌材料的应用和发展提供理论基础;此外还考察了抗菌材料的热性能和力学性能,为淀粉基抗菌薄膜实际应用于肉肠包装提供了理论依据。
由于天然淀粉分子中含有大量亲水性羟基,使淀粉材料的防水性和耐湿性不能满足包装应用要求。本论文采用化学改性法在淀粉分子中引入了疏水性乙酰基团,合成了几种不同取代度的醋酸酯淀粉。接触角测试结果显示高取代度的醋酸酯淀粉的疏水性很强,取代度为2.9的醋酸酯淀粉的接触角为82.54°,但仍显微弱的吸湿性,为醋酸酯淀粉调控抗菌薄膜中抗菌剂的溶出提供了依据。XRD结果表明酯化后的淀粉结晶结构转变为V型,说明淀粉分子间的氢键被削弱,有序化结晶结构被破坏,趋于无序化。热性能及力学性能分析表明醋酸酯化淀粉具有较好的成膜性及可塑性。
论文筛选出了三种强抗菌能力及耐热性的抗菌剂,分别为水不溶性壳聚糖A、水溶性壳聚糖C及壳寡糖E,且热处理对它们的抗菌活性影响不大。将筛选出的这三种抗菌剂分别添加到取代度为2.5的改性淀粉中,制备出几种醋酸酯淀粉抗菌薄膜,并对比它们的溶出及抗菌能力。30℃、30rpm下加速溶出144h结果显示,不溶性壳聚糖A膜基本不溶出,可溶性壳聚糖C膜及壳寡糖E膜溶出性较好,均在24h时溶出率近40%,之后缓慢溶出,144h时C膜及E膜的溶出率分别为45%及60%。三种膜的抗菌性能与之相吻合,A膜抗菌能力很差,基本上没有抗菌效果,C膜及E膜较显著,尤其E膜。说明醋酸酯淀粉抗菌膜中抗菌剂的溶出能力与抗菌能力相对应。膜中的抗菌剂越易迁移溶出,膜的抗菌能力越强。薄膜材料越亲水,薄膜中抗菌剂越易迁移溶出。然而,抗菌剂过快溶出,则维持不了薄膜材料的长效抗菌性,因此,控缓释溶出速率是决定抗菌薄膜材料抗菌时效性及长效性的关键。
采用DMA、拉伸测试仪分析了影响醋酸酯淀粉抗菌薄膜热性能及力学性能的主要因素。结果显示增塑剂添加量对薄膜的玻璃化转变温度Tg影响很大,增塑剂添加量越高,Tg越低,40%添加量时,Tg接近室温。力学性能结果表明壳聚糖抗菌剂可提高淀粉基薄膜材料的力学性能。
综上所述,本论文采用乙酰化反应塑化淀粉分子,制备了不同取代度及亲疏水性能的醋酸酯淀粉,并筛选出了对大肠杆菌及金黄色葡萄球菌抗菌率均在90%以上的几种抗菌剂,采用流涎法制备了高抗菌活性的醋酸酯淀粉抗菌薄膜。考察了影响薄膜中抗菌剂溶出及抗菌能力的主要因素。通过调节薄膜的厚度、增塑剂用量、改性淀粉取代度等,得到了模拟肉肠环境下强防腐抗菌能力的抗菌活性包装薄膜材料,为控缓释性抗菌活性材料应用于食品领域提供了工艺条件及理论依据。
Packing material of antimicrobial activity is a new pattern activity material which is developing in recent twenty years. If the packing material of antimicrobiol activity which is made by base material of environmental friendly with antibacterialagent is used in Food Packing, it would substitute some use of preservatives in food. Because the packing material of antimicrobiol activity is could not only avoid microbe disturbing food, but also improve the safety of food and prolong its shelf life. So it has been considered as a development potential activity packing material. As people’s life become better and better, the quantity demand of delicious sausages become more and more. While the sterilizing effection is not very satisfied and the additive of preservatives for sausages are always get out of line. Both of the problems are the hot spots recently and should be solved as soon as possible.
In the thesis, firstly prepared the starch acetate by modifing starch with hydrophobicity acetyls. Secondly, according to characters of sausages as Water activity, pH value, and so on, built the imitating medium model of suasage. Thirdly, screened out antibacterialagents with strong ability of antibiotic. Then maked out antibiosis material of starch acetate for sausage packaging. As analyzing dissolving out rule for antibacterialagents coming out from film, and the relation with film’s antibiosis capacity, conclude that the base material could control and slow release of antibacterialagent coming out from film. What’s more, the aspects of thermal behavior, crystallize character, and other aspects have been researched in system, which provide theory basis for starch base film applied to sausage packaging.
As natural starch molecules own lots of hydrophily hydroxies, so that the waterproofness and moisture-proof of starch material cann’t satisfy application requirements for sausage packaging. What’s else, natural starch’s melting temperature nears to its decomposition temperature, so it also doesn't have plasticity. In the thesis, the natural starch molecules have been modified by lipophilicity acetyl groups, and composed several acetate starches with different degrees. Results of Contact Angle Test show that hydrophobicity of starch acetate with high degree is strong. When the degree of starch acetate reaches to 2.9, the largest contact angle of it would be 82.54. While the material also apparents weak hygroscopic. Which could provide judging for dissolving out rule of antibacterialagents from antibiosis film by regulating and controlling. XRD result manifests that natural starch’s crystal structure has been changed to V. So hydrogen bonds of starch molecules have been weakened, and the structure’s ordering tends to disorder. Thermal and mechanical properties analysis show that starch acetate is good at becoming film and plasticity.
In the research, three antimicrobials including non water-soluble chitosan A, water-soluble chitosan C, and oligochitosan E have been selected out, which not only are good at antibacterial activity and thermostability, but also their antibacterial activity doesn’t effect greatly by high degree of temperature. All of them have been mixed to modified starch with degree of 2.5, and maked antimicrobial film of acetate starch out. After that, compared their dissolving out regularity to their antibacterial ability. The conclusion of accelerate dissolution test by temperature of 30℃and rate of 30rpm showed that non water-soluble chitosan A basically couldn’t dissolve out. While water-soluble chitosan C and oligochitosan E could dissolve out better. Both of them could dissolve out from base material nearly 40% in 24 hours, and then dissolve out slowly that dissolving rate respectively are 45% and 60% for film C and E in 144 hours. The three kinds of film’s antimicrobial ability agree with their dissolving regularity. Film A is bad at antimicrobial effection, while film C and E are good at it, especially film E. So acetate starch antimicrobial film’s dissolving energy is corresponding to its antimicrobial ability. If antimicrobialagents came out easier from film, the film’s antimicrobial energy would be stronger. If the film was more hydrophily, the film’s antimicrobialagents would dissolve out easier. But if the rate of antimicrobialagents dissolved out was too fast, the film wouldn’t maintain its long-term antibacterial properties. So the rate of control and release dissolving is the key for deciding antibacterial film material’s antibacterial timeliness and long-lasting.
DMA and Instron Tensile Tester were used to analysis the influence factors of acetate starch antimicrobial film’s thermal and mechanical properties. The results show that plasticizers’quantity influence glass transition temperature Tg of film greatly. The more quantity of plasticizers, the lower of film’s Tg. When the quantity reaches to 40%, Tg nears to room temperature. Mechanical property result showes that chitosan could increase mechanical properties of starch film.
From the above, the thesis modifies natural starch with acetyl and makes out acetate starch with different degree and characters of hydrophibic and hydrophobic. Then screening out several antimicrobialagents which could reach antibacterial rates of Escherichia coli and Staphylococcus aureus above 90%. Using the method of Tape Casting maked out the high antibacterial activity film of acetate starch. The mainly factors which could effect antibacterialagents' dissolution and antibiosis energy have been investigated. Via accommodating film’s thickness, quantity of plasticizers, degree of modified starch, and other conditions, could gain antibacterial activity packaging film which own strong antibacterial activity at the condition of imitating sausage environment. So that could provide the conditions of processing technology and theoretical basis for antimicrobial activity material of control and release character which would apply in the food field.
引文
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