CN114411331A - 一种添加牛至精油环糊精包合物的纳米膜及其制备方法和应用 - Google Patents
一种添加牛至精油环糊精包合物的纳米膜及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种添加牛至精油环糊精包合物的纳米膜及其制备方法和应用，涉及纳米膜技术领域，所述纳米膜为将牛至精油包覆至β‑环糊精后获得包合物再将所述包合物加入到聚乳酸和聚己内酯混合的纺丝溶液中采用静电纺丝方法获得。本发明适用于对果蔬贮藏期间的包装，对黑莓的试验显示，该保鲜膜具有较好的减少腐败变质、保色、延缓营养品质损失的作用。
Description
技术领域
本发明涉及纳米膜技术领域，具体涉及一种添加牛至精油环糊精包合物的纳米膜及其制备方法和应用。
背景技术
精油是一种广泛存在于天然植物的化合物，常被提取并用于活性食品包装中，以防止食品酸败、增强抗菌性能。源自牛至(Origanum vulgare)的牛至精油含有大量香芹酚和百里酚，具有出色的抗细菌真菌特性。近年来，在活性食品包装中加入牛至精油作为天然抗菌剂备受关注。一些研究表明，添加牛至精油的包装材料，通过抑制了大肠杆菌、单核细胞增生李斯特菌等，但同时，牛至精油主要由挥发性化合物组成，这种性质影响活性食品包装的稳定性，限制其应用。
β-环糊精是一种由淀粉酶促降解环状寡糖生物分子，该化合物无毒、可食用、生物相容性良好且能够生物降解。β-环糊精由7个吡喃葡萄糖环通过α-1，4糖苷键连接形成截锥型甜甜圈结构，这种分子环结构使得精油、多酚、维生素等小分子化合物可以被包裹到β-环糊精中，形成非共价的主客体包合物。通过缓释作用，可以一定程度上克服牛至精油易挥发的缺点，从而提高生物利用度，扩大应用范围。
黑莓果实柔软多汁，易受机械损伤和病原菌感染，在采后贮藏过程中极易腐败变质。提供一种具有抑菌性的包装材料才是市场所需，提出一种添加牛至精油环糊精包合物的纳米膜及其制备方法和应用。
发明内容
本发明的目的在于克服现有技术的不足，提供了一种添加牛至精油环糊精包合物的纳米膜及其制备方法和应用。
本发明通过以下技术方案来实现上述目的：
本发明提供了一种添加牛至精油环糊精包合物的纳米膜，所述纳米膜为将牛至精油包覆至β-环糊精后获得包合物再将所述包合物加入到聚乳酸和聚己内酯混合的纺丝溶液中采用静电纺丝方法获得。
本发明还提供了上述添加牛至精油环糊精包合物的纳米膜在抗菌材料中的应用。
进一步改进在于，所述纳米膜的抗菌种类包括大肠杆菌(Escherichia coli)、金黄色葡萄球菌(Staphylococcus aureus)、匍枝根霉(Rhizopus stolonifer)、灰葡萄孢菌(Botrytis cinerea)。
本发明还提供了上述添加牛至精油环糊精包合物的纳米膜在果蔬贮藏保鲜膜中的应用。
进一步改进在于，所述果蔬具体为黑莓。
本发明还提供了一种桑树添加牛至精油环糊精包合物的纳米膜的制备方法，包括以下步骤：
(1)将β-环糊精加入蒸馏水，加热搅拌使β-环糊精完全溶解，将牛至精油溶于无水乙醇，缓慢滴加到β-环糊精溶液中，加热并搅拌，低温冷却过夜后离心分离并用无水乙醇溶液洗涤3次沉淀，冷冻干燥后，获得包合物干粉；
(2)将聚乳酸PLA和聚己内酯PCL溶解在六氟异丙醇中搅拌过夜，获得PLA/PCL混合溶液，然后分别加入所述包合物干粉，搅拌使包埋物分散均匀，获得纺丝溶液；
(3)将所述纺丝溶液装入注射器中，推进泵的进料速率设置为1.5mL/h，针头和飞轮收集器(300r/min)之间的距离为15cm，使用高压电源施加20kV的电压，进行电纺丝，获得纳米膜。
进一步改进在于，所述步骤(1)中，牛至精油和β-环糊精的质量比为1:5。
进一步改进在于，所述步骤(2)中，PLA/PCL混合溶液中聚乳酸PLA和聚己内酯PCL的体积分数均为12％。
进一步改进在于，所述步骤(2)中，纺丝溶液中包合物干粉的质量分数2-6wt％。
本发明提具有如下有益效果：
(1)本发明的保鲜复合抑菌包装膜采用静电纺丝方法进行制备，由透射电镜观察发现，牛至精油包合物被包裹在纳米纤维中，由此可以实现精油的包埋，延缓释放。
(2)纳米膜表现出良好的热稳定性，在350-400℃时才发生分解；拉伸强度1.5Mpa，机械性能良好；水接触角大于90°，疏水性强；水蒸气透过率0.85g mm/m2 h kPa，对水蒸气阻隔性能良好。
(3)抗菌实验表明，纳米膜对于大肠杆菌(Escherichia coli)、金黄色葡萄球菌(Staphylococcus aureus)、匍枝根霉(Rhizopus stolonifer)、灰葡萄孢菌(Botrytiscinerea)具有良好持久的抗菌能力。
(4)纳米膜与斑马鱼共培养15天，斑马鱼存活率100％，证明其具有生物安全性。
(5)纳米膜延缓了黑莓采后腐烂、变质、软化等品质劣变，作为活性食品包装具有巨大潜力。
附图说明
图1为本发明纳米膜的生产工作原理图；
图2为本发明纳米膜微观结构(A：实施例3扫描电镜图，B：实施例3透射电镜图)；
图3为本发明纳米膜的热力性能(A)、机械性能(B)；
图4为本发明纳米膜对于大肠杆菌(A)、金黄色葡萄球菌(B)、匍枝根霉(C)、灰葡萄孢菌(D)的抗菌能力；
图5为本发明纳米膜共培养15天斑马鱼生长状态(A)、共培养15天斑马鱼存活率(B)；
图6为不同处理情况下黑莓在25℃，55％相对湿度贮藏四天的外观形态。
具体实施方式
下面结合附图对本申请作进一步详细描述，有必要在此指出的是，以下具体实施方式只用于对本申请进行进一步的说明，不能理解为对本申请保护范围的限制，该领域的技术人员可以根据上述申请内容对本申请作出一些非本质的改进和调整。
本发明一种桑树添加牛至精油环糊精包合物的纳米膜，制备方法包括以下步骤：
(1)将β-环糊精加入蒸馏水，加热搅拌使β-环糊精完全溶解，将牛至精油溶于无水乙醇，牛至精油和β-环糊精的质量比为1:5)，缓慢滴加到β-环糊精溶液中，加热并搅拌，低温冷却过夜后离心分离并用无水乙醇溶液洗涤3次沉淀，冷冻干燥后，获得包合物干粉；
(2)将聚乳酸PLA和聚己内酯PCL溶解在六氟异丙醇中搅拌过夜，聚乳酸PLA和聚己内酯PCL的体积分数均为12％，获得PLA/PCL混合溶液，然后分别加入所述包合物干粉，搅拌使包埋物分散均匀，获得纺丝溶液，纺丝溶液中包合物干粉的质量分数2-6wt％；
(3)将所述纺丝溶液装入注射器中，推进泵的进料速率设置为1.5mL/h，针头和飞轮收集器(300r/min)之间的距离为15cm，使用高压电源施加20kV的电压，进行电纺丝，获得纳米膜。
为了证明本发明制备的纳米膜的效果，提供以下具体实施方式。
牛至精油环糊精包合物制备
将5g的β-环糊精加入100mL蒸馏水中，将混合物加热至50℃并以500r/min搅拌使β-环糊精完全溶解，将1g牛至精油溶于无水乙醇，缓慢滴加到β-环糊精溶液中，将溶液在50℃下加热并搅拌3小时，然后在4℃下冷却过夜，通过离心(8000×g，15分钟)分离并用无水乙醇溶液洗涤3次沉淀，以去除未包埋的牛至精油，将牛至精油环糊精包合物冷冻干燥12小时后，获得包合物干粉。
实施例1
将1.2gPLA和1.2gPCL溶解在10mL六氟异丙醇中搅拌过夜，获得PLA(12％v/v)和PCL(12％v/v)混合溶液，然后分别加入0.076g(2wt％)的包合物干粉，然后将混合物搅拌4小时使包埋物分散均匀，随后将纺丝溶液装入5mL注射器中，推进泵的进料速率设置为1.5mLh-1，针头和飞轮收集器(300r/min)之间的距离为15cm，使用高压电源施加20kV的电压。
实施例2
将1.2gPLA和1.2gPCL溶解在10mL六氟异丙醇中搅拌过夜，获得PLA(12％v/v)和PCL(12％v/v)混合溶液，然后分别加入0.1g(4wt％)的包合物干粉，然后将混合物搅拌4小时使包埋物分散均匀，随后将纺丝溶液装入5mL注射器中，推进泵的进料速率设置为1.5mLh-1，针头和飞轮收集器(300r/min)之间的距离为15cm，使用高压电源施加20kV的电压。
实施例3
将1.2gPLA和1.2gPCL溶解在10mL六氟异丙醇中搅拌过夜，获得PLA(12％v/v)和PCL(12％v/v)混合溶液，然后分别加入0.154g(6wt％)的包合物干粉，然后将混合物搅拌4小时使包埋物分散均匀，随后将纺丝溶液装入5mL注射器中，推进泵的进料速率设置为1.5mLh-1，针头和飞轮收集器(300r/min)之间的距离为15cm，使用高压电源施加20kV的电压。
实施例3制备的静电纺丝纳米膜微观结构如图2所示。
对比例1
将1.2gPLA和1.2gPCL溶解在10mL六氟异丙醇中搅拌过夜，获得PLA(12％v/v)和PCL(12％v/v)混合溶液，随后将纺丝溶液装入5mL注射器中，推进泵的进料速率设置为1.5mLh-1，针头和飞轮收集器(300r/min)之间的距离为15cm，使用高压电源施加20kV的电压。
1、物理化学性能
从图3中可看出，A：实施例1-3所制备而成的纳米膜表现出良好的热稳定性，在350-400℃时才发生分解；B：实施例1-3所制备而成的纳米膜拉伸强度达到1.5Mpa，机械性能良好，拉伸率达到120％-140％；
2、抗菌性能
从图4中可看出，实施例1-3所制备而成的纳米膜对于大肠杆菌(Escherichiacoli)、金黄色葡萄球菌(Staphylococcus aureus)、匍枝根霉(Rhizopus stolonifer)、灰葡萄孢菌(Botrytis cinerea)具有良好持久的抗菌能力，尤其实施例3抑菌效果优异。
3、生物安全性分析
使用实验斑马鱼(Daniorerio)进行生物安全性分析，所有斑马鱼均健康无病，平均体长为1.9±0.2cm。驯化用水预曝气12h，保证氧气充足，温度23±1℃，pH值7.0-7.7，硬度245mg/L，溶解氧5.3-6.5mg/L。将斑马鱼分别置于空白和含有15mg的添加实施例3的培养基中培养15天。不同处理设置三个重复，每个重复包含十条斑马鱼。斑马鱼以16：8小时的昼夜循环进行培养，在培养期间不进食，第15天对斑马鱼拍照并计算存活率。
生物安全性分析结果如图5所示，纳米膜与斑马鱼共培养15天，斑马鱼存活率100％，证明其具有生物安全性。
4、保鲜性能应用
黑莓“赫尔”在中国南京溧水江苏省植物研究所的试验田中种植，通过人工采收九成熟果实，2小时内运至实验室。选择大小、颜色和成熟度均一的黑莓果实。在4±1℃和90％相对湿度环境中预冷12小时后，将125±5g的果实随机分装在PET容器(17.5cm×13.5cm×5.5cm)中。四种处理包括无处理的水果(对照)、用对比例1和实施例3覆盖的水果(17.5cm×13.5cm)，以及用9.15mg/L牛至精油熏蒸。样品在25℃、55％RH中贮藏4天，每个处理3个重复。
贮藏4天黑莓外观如图6所示，纳米膜延缓了黑莓采后腐烂、变质、软化等品质劣变。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。
Claims (9)
1.一种添加牛至精油环糊精包合物的纳米膜，其特征在于，所述纳米膜为将牛至精油包覆至β-环糊精后获得包合物再将所述包合物加入到聚乳酸和聚己内酯混合的纺丝溶液中采用静电纺丝方法获得。
2.一种如权利要求1所述的添加牛至精油环糊精包合物的纳米膜在抗菌材料中的应用。
3.根据权利要求2所述的应用，其特征在于，所述纳米膜的抗菌种类包括大肠杆菌(Escherichia coli)、金黄色葡萄球菌(Staphylococcus aureus)、匍枝根霉(Rhizopusstolonifer)、灰葡萄孢菌(Botrytis cinerea)。
4.一种如权利要求1所述的添加牛至精油环糊精包合物的纳米膜在果蔬贮藏保鲜膜中的应用。
5.根据权利要求4所述的应用，其特征在于，所述果蔬具体为黑莓。
6.一种如权利要求1所述的添加牛至精油环糊精包合物的纳米膜的制备方法，其特征在于，包括以下步骤：
(1)将β-环糊精加入蒸馏水，加热搅拌使β-环糊精完全溶解，将牛至精油溶于无水乙醇，缓慢滴加到β-环糊精溶液中，加热并搅拌，低温冷却过夜后离心分离并用无水乙醇溶液洗涤3次沉淀，冷冻干燥后，获得包合物干粉；
(2)将聚乳酸PLA和聚己内酯PCL溶解在六氟异丙醇中搅拌过夜，获得PLA/PCL混合溶液，然后分别加入所述包合物干粉，搅拌使包埋物分散均匀，获得纺丝溶液；
(3)将所述纺丝溶液装入注射器中，推进泵的进料速率设置为1.5mL/h，针头和飞轮收集器(300r/min)之间的距离为15cm，使用高压电源施加20kV的电压，进行电纺丝，获得纳米膜。
7.根据权利要求6所述的一种添加牛至精油环糊精包合物的纳米膜的制备方法，其特征在于，所述步骤(1)中，牛至精油和β-环糊精的质量比为1:5。
8.根据权利要求6所述的一种添加牛至精油环糊精包合物的纳米膜的制备方法，其特征在于，所述步骤(2)中，PLA/PCL混合溶液中聚乳酸PLA和聚己内酯PCL的体积分数均为12％。
9.根据权利要求6所述的一种添加牛至精油环糊精包合物的纳米膜的制备方法，其特征在于，所述步骤(2)中，纺丝溶液中包合物干粉的质量分数2-6wt％。
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