葛根淀粉基可食性包装膜物化与抗菌性能的研究
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摘要
可食性包装膜能够减少食品的水分散失和营养成分消耗，防止微生物污染，有效延长食品的贮藏保鲜和销售期限，提高其商品价值与市场竞争力，已受到全世界的关注。在众多成膜基材中，淀粉产量丰富、廉价易得、处理简单、易生物降解且具有良好的阻气性能，是最具应用前景的原材料之一。
葛根作为一种天然药物和保健食品，在我国储量丰富、分布广泛。目前葛根主要被用于提取药用成分，而其中含量丰富的淀粉却随废渣排出，未被有效利用，这既污染环境又浪费资源。若将废弃的淀粉充分回收并加以利用，将会获得更大的综合价值。因此，本论文以葛根淀粉为基材，制备了系列可食性包装膜并研究了相关物化特性，以期拓展葛根淀粉的应用，促进葛根产业的健康发展。
研究内容及方法分以下四部分：
一、考察制膜工艺（糊化温度80°C–100°C、糊化时间5min–60min、淀粉糊浓度1%–6%）对葛根淀粉可食性包装膜机械性能、透湿能力的影响；分析甘油含量（0%–40%）和环境相对湿度（50%、75%、100%）变化对葛根淀粉膜的综合影响，指标包括红外光谱、X–射线衍射图谱、热重差热分析、等温吸湿曲线等。结果发现：①本实验在糊化温度100°C、糊化时间15min、淀粉糊液浓度3%、甘油添加量30%的条件下得到了综合性能最优的葛根淀粉膜。②红外光谱表明淀粉C–O–C基团中C–O键对应峰的偏移受甘油含量及相对湿度变化的双重影响。③甘油能够促进葛根淀粉B型结晶的发展且能够与葛根淀粉形成V型结晶；相对湿度升高使得塑化葛根淀粉膜V型结晶峰强度减弱。④葛根淀粉膜的热重曲线可分为水分蒸发、甘油富集相分解和淀粉分解三个阶段，且淀粉分解阶段的活化能随甘油含量的增加而降低。
二、研究非离子表面活性剂（吐温20、司盘80）对葛根淀粉/抗坏血酸膜液表面张力及润湿性能、抗坏血酸自膜中释放能力、膜结晶情况、表面及内部形貌、机械性能、阻水能力及水溶性等的影响。结果表明：①吐温20及司盘80均可显著降低葛根淀粉/抗坏血酸膜液的表面张力（P<0.05）。②单独加入吐温20可增强膜液在玻璃及石蜡基材上的润湿性，使膜变得更加平整，增大膜的水溶性；单独加入司盘80降低了膜液在石蜡基材上的接触角大小，增强了膜表面的粗糙度；混合表面活性剂增大了葛根淀粉膜的水蒸气透过率。③抗坏血酸从葛根淀粉膜向水中的扩散系数约为2.22×10~(–11)m~2s~(–1)，表面活性剂的加入减缓了抗坏血酸的释放速率。④吐温20及司盘80均能有效抑制葛根淀粉B型结晶的发展，吐温20亦与葛根淀粉络合形成V型结晶。
三、探讨壳聚糖酸溶剂（1%的乙酸、乳酸、苹果酸）对葛根淀粉/壳聚糖复合膜性能的影响及不同储藏环境（25°C常温储藏、–20°C冷冻储藏）下膜性能的变化；考察膜液流动性能、复合膜抗菌效果、分子间作用力、结晶情况、吸湿能力、机械性能、阻水能力、水溶性、颜色等指标。发现：①葛根淀粉/壳聚糖复合膜液是剪切变稀的假塑性流体；以乙酸、乳酸、苹果酸配制的膜液按此顺序表现出假塑性变小、牛顿性增大、稠度降低的规律。②复合膜对大肠杆菌的抑制效果优于对金黄色葡萄球菌的作用。③红外光谱、X–射线衍射分析表明，各成膜组分间具有良好的相容性。④乙酸葛根淀粉/壳聚糖膜的机械强度最大、水溶性最小、颜色最浅；乳酸葛根淀粉/壳聚糖膜的延展性最优；苹果酸葛根淀粉/壳聚糖膜的抗菌性最佳、吸水性最小、阻水性最强。⑤储藏时间显著影响复合膜水分含量、机械性能、阻水能力、颜色及水溶性（P<0.05）；冷冻储藏能够延缓复合膜颜色变化，但对复合膜结晶性能、水分含量及水溶性的影响与常温储藏无显著性差异（P>0.05）。
四、评价加入0.1%吐温20的葛根淀粉/壳聚糖/抗坏血酸复合膜的综合性能，指标包括膜液表面张力、接触角及流动性能、复合膜抗菌效果、抗坏血酸释放性能、机械性能、阻水能力、水溶性及颜色等。①膜液表面张力显著低于同等条件下葛根淀粉/抗坏血酸膜液的表面张力（P<0.05）；膜液在玻璃基板上的接触角小于30°，在石蜡基板上的接触角小于90°；壳聚糖酸溶剂未对膜液表面张力及润湿性产生显著影响（P>0.05）。②乙酸葛根淀粉/壳聚糖膜中抗坏血酸释放主要受膜溶胀过程控制，乳酸、苹果酸葛根淀粉/壳聚糖膜中的释放还同时受膜溶蚀过程的影响。③和葛根淀粉/壳聚糖膜相比较，葛根淀粉/壳聚糖/抗坏血酸膜对大肠杆菌及金黄色葡萄球菌的抑制效果更为明显、膜亮度更低、颜色更深。
研究结果表明，葛根淀粉能够与多种添加剂有效复配，制备性能较为理想的可食性复合包装膜，为拓展葛根淀粉的应用领域提供一定理论支持。
Edible films can reduce moisture loss and nutrient consumption, preventmicrobial contamination, and prolong the shelf life of food products. Edible filmsprovide bright application prospects in improving the market competitiveness of foodproducts and have attracted broad attentions nowadays. Among many naturalbiopolymers for forming edible films, starch is one of the most promising rawmaterials due to its abundance, low cost, simple treatment, biodegradability and goodvapor barrier ability.
Kudzu as a natural medicine and healthy food is widely distributed in China.Kudzu is mainly used to extract medicinal ingredients now, whereas a great amount ofstarch rich in its root is just discharged, which not only spoils the environment butalso wastes resources. If the starch can be recovered and effectively utilized, it willget more comprehensive values. Therefore, in order to expaned the application filedsof kudzu starch and promote the healthy development of kudzu industry, thephysiochemical properties of kudzu starch based edible films were studied in thispaper. The main research methods and contents are as follows:
(1) The influences of film–forming processes (pasting temperature from80°Cto100°C, gelatinization time from5min to60min, starch concentration from1%to6%) on mechanical property and water vapor permeability of kudzu starch edible filmwere studied; The effects of glycerol content (from0%to40%) and relative humidity(50%,75%, and100%) on the comprehensive properties (including FT–IR, XRD,TG–DTA, water sorption isotherms and so on) of the films were also evaluated. Theresults showed that:①The film showed the best performance when we chose thepasting temperature of100°C, gelatinization time of15min, starch concentration of3%, and glycerol content of30%.②FT–IR displayed that the shift of peakcorresponding to C–O in C–O–C group was affected by dual factors of glycerol content and relative humidity.③The intensity of B–type crystal diffraction enhancedgradually as glycerol content increased, and glycerol could form V–type crystal withkudzu starch; the intensity of diffraction peak relating to V–type crystal weakenedwith the increase of relative humidity.④TG curve of kudzu starch film presented3degradation steps representing water evaporation, degradation of the glycerol–richphase, and starch degradation, respectively. The activation energy value relating to themain starch degradation step was found to be negative linear with glycerol content.
(2) The effects of surfactant (tween20and span80) on the surface tension andwettability of kudzu starch/ascorbic acid film–forming solution, the release behaviorof ascorbic acid from film to water, as well as the crystal structure, microstructure,mechanical property, water vapor permeability and solubility of the film wereevaluated. It was found that:①Each surfactant effectively decreased the surfacetension of the film–forming solution (P<0.05).②Only adding tween20improved thewettability of film–forming solution on both glass and paraffin wax substrates,smoothened the film’s surface, and enhanced the film’s solubility; Adding span80alone reduced the contact angle of film–forming solution on paraffin wax substratebut enhanced the surface roughness of the film; the use of blended–surfactantincreased the film’s water vapor permeability;③The diffusion coefficient ofwater–soluble ascorbic acid from kudzu starch/ascorbic acid film to water was about2.22×10~(–11)m~2s~(–1), and each surfactant could delay the release of ascorbic acid.④The addition of surfactant decreased the B–type crystal structure of the film, andadding tween20promoted the formation of V–type crystal.
(3) Effects of acid types (acetic acid, lactic acid and malic acid at concentrationof1%) and storage conditions (25°C and–20°C, respectively) on the properties ofkudzu starch/chitosan composite film were investigated, including the fluidity offilm–forming solution, antibacterial activity, functional group interaction, crystalstructure, water sorption ability, mechanical property, water vapor barrier ability,solubility and color index of the resulting film. The data displayed that:①Thefilm–forming solution belonged to shear–thinning fluid. When chose acetic acid,lactic acid, and malic acid as solvent, the pseudoplasticity of film–forming solutiondeclined, newtonianism increased, and consistency decreased following the aboveorder.②The antibacterial effect of the composite film was stronger against E. colithan against S. aureus.③The film–forming component was compatible with eachother as evidenced by FT–IR and XRD spectra.④The composite film choosing acetic acid as solvent presented the strongest mechanical property, the smallestsolubility, and the lightest yellowness. The film mading from lactic acid solutiondisplayed the greatest flexible property. The film using malic acid as solvent showedthe best antibacterial activity and water barrier property, and the lowest water sorptionability.⑤Storage time significantly affected film’s water content, mechanicalproperty, water barrier ability, color and solubility (P <0.05); subzero temperaturedelayed the color changes of the film during storage. However, storage temperaturedid not influence the crystallization, water content, mechanical property and solubilityof the film (P>0.05).
(4) The overall performance of kudzu starch/chitosan/ascorbic acid compositefilm with addition of0.1%tween20was evaluated, including surface tension, contactangle and fluidity of the film–forming solution, the antibacterial activity, releasebehavior of ascorbic acid, mechanical propertiy, water vapor permeability, solubility,and color index of the film.①Surface tension of kudzu starch/chitosan/ascorbic acidfilm–forming solution was significantly lower than the value of kudzu starch/ascorbicacid film–forming solution under the same experiment condition (P<0.05); the contactangle of the film–forming solution on the glass substrate was less than30°, and thecontact angle was less than90°on solid paraffin substrate; acid solvent type did notsignificantly affect the surface tension and wettability of film–forming solution(P>0.05).②The release of ascorbic acid from film choosing acetic acid as solventwas mainly controlled by film swelling process, and the release behavior of ascorbicacid from film made from lactic acid or malic acid was affected by thefilm–dissolution as well.③As compared with kudzu starch/chitosan composite film,the antibacterial ability was better, and the color was darker of kudzu starch/chitosan/ascorbic acid film.
The results showed that kuzu starch can form relatively desired compositepackaging film by effectively blending with a variety of additives, and this manuscriptprovided some theoretical supports for expanding the application area of kuzu starch.
葛根作为一种天然药物和保健食品，在我国储量丰富、分布广泛。目前葛根主要被用于提取药用成分，而其中含量丰富的淀粉却随废渣排出，未被有效利用，这既污染环境又浪费资源。若将废弃的淀粉充分回收并加以利用，将会获得更大的综合价值。因此，本论文以葛根淀粉为基材，制备了系列可食性包装膜并研究了相关物化特性，以期拓展葛根淀粉的应用，促进葛根产业的健康发展。
研究内容及方法分以下四部分：
一、考察制膜工艺（糊化温度80°C–100°C、糊化时间5min–60min、淀粉糊浓度1%–6%）对葛根淀粉可食性包装膜机械性能、透湿能力的影响；分析甘油含量（0%–40%）和环境相对湿度（50%、75%、100%）变化对葛根淀粉膜的综合影响，指标包括红外光谱、X–射线衍射图谱、热重差热分析、等温吸湿曲线等。结果发现：①本实验在糊化温度100°C、糊化时间15min、淀粉糊液浓度3%、甘油添加量30%的条件下得到了综合性能最优的葛根淀粉膜。②红外光谱表明淀粉C–O–C基团中C–O键对应峰的偏移受甘油含量及相对湿度变化的双重影响。③甘油能够促进葛根淀粉B型结晶的发展且能够与葛根淀粉形成V型结晶；相对湿度升高使得塑化葛根淀粉膜V型结晶峰强度减弱。④葛根淀粉膜的热重曲线可分为水分蒸发、甘油富集相分解和淀粉分解三个阶段，且淀粉分解阶段的活化能随甘油含量的增加而降低。
二、研究非离子表面活性剂（吐温20、司盘80）对葛根淀粉/抗坏血酸膜液表面张力及润湿性能、抗坏血酸自膜中释放能力、膜结晶情况、表面及内部形貌、机械性能、阻水能力及水溶性等的影响。结果表明：①吐温20及司盘80均可显著降低葛根淀粉/抗坏血酸膜液的表面张力（P<0.05）。②单独加入吐温20可增强膜液在玻璃及石蜡基材上的润湿性，使膜变得更加平整，增大膜的水溶性；单独加入司盘80降低了膜液在石蜡基材上的接触角大小，增强了膜表面的粗糙度；混合表面活性剂增大了葛根淀粉膜的水蒸气透过率。③抗坏血酸从葛根淀粉膜向水中的扩散系数约为2.22×10~(–11)m~2s~(–1)，表面活性剂的加入减缓了抗坏血酸的释放速率。④吐温20及司盘80均能有效抑制葛根淀粉B型结晶的发展，吐温20亦与葛根淀粉络合形成V型结晶。
三、探讨壳聚糖酸溶剂（1%的乙酸、乳酸、苹果酸）对葛根淀粉/壳聚糖复合膜性能的影响及不同储藏环境（25°C常温储藏、–20°C冷冻储藏）下膜性能的变化；考察膜液流动性能、复合膜抗菌效果、分子间作用力、结晶情况、吸湿能力、机械性能、阻水能力、水溶性、颜色等指标。发现：①葛根淀粉/壳聚糖复合膜液是剪切变稀的假塑性流体；以乙酸、乳酸、苹果酸配制的膜液按此顺序表现出假塑性变小、牛顿性增大、稠度降低的规律。②复合膜对大肠杆菌的抑制效果优于对金黄色葡萄球菌的作用。③红外光谱、X–射线衍射分析表明，各成膜组分间具有良好的相容性。④乙酸葛根淀粉/壳聚糖膜的机械强度最大、水溶性最小、颜色最浅；乳酸葛根淀粉/壳聚糖膜的延展性最优；苹果酸葛根淀粉/壳聚糖膜的抗菌性最佳、吸水性最小、阻水性最强。⑤储藏时间显著影响复合膜水分含量、机械性能、阻水能力、颜色及水溶性（P<0.05）；冷冻储藏能够延缓复合膜颜色变化，但对复合膜结晶性能、水分含量及水溶性的影响与常温储藏无显著性差异（P>0.05）。
四、评价加入0.1%吐温20的葛根淀粉/壳聚糖/抗坏血酸复合膜的综合性能，指标包括膜液表面张力、接触角及流动性能、复合膜抗菌效果、抗坏血酸释放性能、机械性能、阻水能力、水溶性及颜色等。①膜液表面张力显著低于同等条件下葛根淀粉/抗坏血酸膜液的表面张力（P<0.05）；膜液在玻璃基板上的接触角小于30°，在石蜡基板上的接触角小于90°；壳聚糖酸溶剂未对膜液表面张力及润湿性产生显著影响（P>0.05）。②乙酸葛根淀粉/壳聚糖膜中抗坏血酸释放主要受膜溶胀过程控制，乳酸、苹果酸葛根淀粉/壳聚糖膜中的释放还同时受膜溶蚀过程的影响。③和葛根淀粉/壳聚糖膜相比较，葛根淀粉/壳聚糖/抗坏血酸膜对大肠杆菌及金黄色葡萄球菌的抑制效果更为明显、膜亮度更低、颜色更深。
研究结果表明，葛根淀粉能够与多种添加剂有效复配，制备性能较为理想的可食性复合包装膜，为拓展葛根淀粉的应用领域提供一定理论支持。
Edible films can reduce moisture loss and nutrient consumption, preventmicrobial contamination, and prolong the shelf life of food products. Edible filmsprovide bright application prospects in improving the market competitiveness of foodproducts and have attracted broad attentions nowadays. Among many naturalbiopolymers for forming edible films, starch is one of the most promising rawmaterials due to its abundance, low cost, simple treatment, biodegradability and goodvapor barrier ability.
Kudzu as a natural medicine and healthy food is widely distributed in China.Kudzu is mainly used to extract medicinal ingredients now, whereas a great amount ofstarch rich in its root is just discharged, which not only spoils the environment butalso wastes resources. If the starch can be recovered and effectively utilized, it willget more comprehensive values. Therefore, in order to expaned the application filedsof kudzu starch and promote the healthy development of kudzu industry, thephysiochemical properties of kudzu starch based edible films were studied in thispaper. The main research methods and contents are as follows:
(1) The influences of film–forming processes (pasting temperature from80°Cto100°C, gelatinization time from5min to60min, starch concentration from1%to6%) on mechanical property and water vapor permeability of kudzu starch edible filmwere studied; The effects of glycerol content (from0%to40%) and relative humidity(50%,75%, and100%) on the comprehensive properties (including FT–IR, XRD,TG–DTA, water sorption isotherms and so on) of the films were also evaluated. Theresults showed that:①The film showed the best performance when we chose thepasting temperature of100°C, gelatinization time of15min, starch concentration of3%, and glycerol content of30%.②FT–IR displayed that the shift of peakcorresponding to C–O in C–O–C group was affected by dual factors of glycerol content and relative humidity.③The intensity of B–type crystal diffraction enhancedgradually as glycerol content increased, and glycerol could form V–type crystal withkudzu starch; the intensity of diffraction peak relating to V–type crystal weakenedwith the increase of relative humidity.④TG curve of kudzu starch film presented3degradation steps representing water evaporation, degradation of the glycerol–richphase, and starch degradation, respectively. The activation energy value relating to themain starch degradation step was found to be negative linear with glycerol content.
(2) The effects of surfactant (tween20and span80) on the surface tension andwettability of kudzu starch/ascorbic acid film–forming solution, the release behaviorof ascorbic acid from film to water, as well as the crystal structure, microstructure,mechanical property, water vapor permeability and solubility of the film wereevaluated. It was found that:①Each surfactant effectively decreased the surfacetension of the film–forming solution (P<0.05).②Only adding tween20improved thewettability of film–forming solution on both glass and paraffin wax substrates,smoothened the film’s surface, and enhanced the film’s solubility; Adding span80alone reduced the contact angle of film–forming solution on paraffin wax substratebut enhanced the surface roughness of the film; the use of blended–surfactantincreased the film’s water vapor permeability;③The diffusion coefficient ofwater–soluble ascorbic acid from kudzu starch/ascorbic acid film to water was about2.22×10~(–11)m~2s~(–1), and each surfactant could delay the release of ascorbic acid.④The addition of surfactant decreased the B–type crystal structure of the film, andadding tween20promoted the formation of V–type crystal.
(3) Effects of acid types (acetic acid, lactic acid and malic acid at concentrationof1%) and storage conditions (25°C and–20°C, respectively) on the properties ofkudzu starch/chitosan composite film were investigated, including the fluidity offilm–forming solution, antibacterial activity, functional group interaction, crystalstructure, water sorption ability, mechanical property, water vapor barrier ability,solubility and color index of the resulting film. The data displayed that:①Thefilm–forming solution belonged to shear–thinning fluid. When chose acetic acid,lactic acid, and malic acid as solvent, the pseudoplasticity of film–forming solutiondeclined, newtonianism increased, and consistency decreased following the aboveorder.②The antibacterial effect of the composite film was stronger against E. colithan against S. aureus.③The film–forming component was compatible with eachother as evidenced by FT–IR and XRD spectra.④The composite film choosing acetic acid as solvent presented the strongest mechanical property, the smallestsolubility, and the lightest yellowness. The film mading from lactic acid solutiondisplayed the greatest flexible property. The film using malic acid as solvent showedthe best antibacterial activity and water barrier property, and the lowest water sorptionability.⑤Storage time significantly affected film’s water content, mechanicalproperty, water barrier ability, color and solubility (P <0.05); subzero temperaturedelayed the color changes of the film during storage. However, storage temperaturedid not influence the crystallization, water content, mechanical property and solubilityof the film (P>0.05).
(4) The overall performance of kudzu starch/chitosan/ascorbic acid compositefilm with addition of0.1%tween20was evaluated, including surface tension, contactangle and fluidity of the film–forming solution, the antibacterial activity, releasebehavior of ascorbic acid, mechanical propertiy, water vapor permeability, solubility,and color index of the film.①Surface tension of kudzu starch/chitosan/ascorbic acidfilm–forming solution was significantly lower than the value of kudzu starch/ascorbicacid film–forming solution under the same experiment condition (P<0.05); the contactangle of the film–forming solution on the glass substrate was less than30°, and thecontact angle was less than90°on solid paraffin substrate; acid solvent type did notsignificantly affect the surface tension and wettability of film–forming solution(P>0.05).②The release of ascorbic acid from film choosing acetic acid as solventwas mainly controlled by film swelling process, and the release behavior of ascorbicacid from film made from lactic acid or malic acid was affected by thefilm–dissolution as well.③As compared with kudzu starch/chitosan composite film,the antibacterial ability was better, and the color was darker of kudzu starch/chitosan/ascorbic acid film.
The results showed that kuzu starch can form relatively desired compositepackaging film by effectively blending with a variety of additives, and this manuscriptprovided some theoretical supports for expanding the application area of kuzu starch.
引文
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