CN110859184B - 一种纳米抗菌葡糖基复合粒子及其加工方法与应用 - Google Patents

一种纳米抗菌葡糖基复合粒子及其加工方法与应用 Download PDF

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CN110859184B
CN110859184B CN201911134115.9A CN201911134115A CN110859184B CN 110859184 B CN110859184 B CN 110859184B CN 201911134115 A CN201911134115 A CN 201911134115A CN 110859184 B CN110859184 B CN 110859184B
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缪铭
刘瑶
支朝晖
张涛
金征宇
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Jiangnan University
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Abstract

本发明公开了一种纳米抗菌葡糖基复合粒子及其加工方法与应用，属于现代食品加工技术领域。本发明以天然葡糖基纳米颗粒为原料，利用颗粒表面定位改性与物理场电荷转移技术来制备纳米抗菌复合粒子。所得纳米抗菌葡糖基复合粒子的粒径50～1000nm，表面zeta电位0～‑10mV，广谱抑菌率>98％；能够有效延长食品的货架期，防止产品腐败变质；可用于食品、纺织、日化、医药等诸多领域等领域，应用前景非常广阔。

Description

一种纳米抗菌葡糖基复合粒子及其加工方法与应用
技术领域
本发明涉及一种纳米抗菌葡糖基复合粒子及其加工方法与应用，属于现代食品加工技术领域。
背景技术
纳米技术是上世纪80年代末期崛起并正在迅猛发展的新型前沿高技术，涉及现代物理学、化学、生物学、医学、材料科学、信息科学、能源科学和先进制造科学，是一门高度交叉学科。纳米技术是研究在纳米尺度(通常指1～100nm)下材料的性质和应用。利用纳米技术可以使人类认识与改造物质世界的手段和能力延伸到原子和分子。在纳米尺度下，物质具有量子尺寸效应、表面效应和宏观量子隧道效应等特点，展现出与宏观尺度下物质的物理、化学、光学、力学、生物学等不同或宏观不具备的特性。目前，纳米科技已经对世界产生了深远影响，其应用领域已慢慢渗入到食品、农业、医药等传统产业中，欧美发达国家已投入大量的人力物力进行纳米尺度系列产品的研究与开发，如活性因子纳米载体、食品抗菌包装、纳米封装化学投入品、纳米乳液、纳米传感器等。
近年来，由于抗生素的滥用导致了全球范围内不断的出现多药耐药菌株，新型高效抗菌剂的研究越来越受到重视，其中金属及金属氧化物的纳米粒子具备高效抗菌活性，如Ag、TiO2、ZnO、Fe3O4等，他们破坏细菌细胞壁或细胞膜、阻断跨膜的电子转移、抑制酶活性和DNA合成等。但是，这些纳米抗菌粒子存在安全性、成本高、药效不佳等问题，如纳米Ag和纳米TiO2都具有一定程度的毒性，可能会对人体健康和环境产生负面影响，而对天然可降解生物大分子物质制备抗菌纳米粒子的研究报道较少，至今未见纳米抗菌葡糖基复合粒子相关报道。基于上述原因，为了拓宽天然纳米材料的应用领域并提升附加值，开发一种纳米抗菌葡糖基复合粒子加工方法与应用是有迫切需求的。
发明内容
为了解决上述问题，本发明提供了一种纳米抗菌葡糖基复合粒子，本发明纳米抗菌葡糖基复合粒子具有优异的抗菌性能，可以作为基体材料用于食品、纺织、日化、医药等领域。该方法具有工艺简单、过程可控、绿色环保等特点。
本发明的第一个目的是提供一种纳米抗菌葡糖基复合粒子的加工方法，所述方法包括如下步骤：
(1)将天然葡糖基纳米颗粒分散在水中，添加50～200U/g天然葡糖基纳米颗粒的微生物GH13家族糖苷水解酶进行催化反应；
(2)反应完全后，加入有机酸酐酯化剂、醚化试剂，调节pH至7～13，微波环境下进行反应；
(3)反应完全后，加入相对天然葡糖基纳米颗粒0.01-1％质量百分比的防腐剂，超声环境下进行反应，然后取沉淀、干燥。
在本发明实施方式中，天然葡糖基纳米颗粒来源于植物、动物或微生物，其中植物和动物源采用生长期谷物籽粒、藻类和动物某些组织提取获得，微生生物源经过活化培养、发酵获得菌体提取获得。所得产物分子量106～108g/mol，分散分子密度1000～2000g/(mol·nm3)。
在本发明实施方式中，步骤(1)中的天然葡糖基纳米颗粒在水中的质量浓度为10～40％。
在本发明实施方式中，步骤(1)中的反应是在温度30～70℃、pH值3.5～7.0下恒温催化0.5～12h。
在本发明实施方式中，微生物GH13家族糖苷水解酶包括麦芽糖苷酶、淀粉葡糖苷酶、淀粉水解酶等一种或多种。
在本发明实施方式中，有机酸酐酯化剂包括丁二酸酐、顺丁烯二酸酐、乙酸酐、硬脂酸酐、柠檬酸酐等一种或多种，醚化试剂包括环氧氯丙烷、环氧乙烯、甲基氯、乙基氯、二甲基硫酸等一种或多种。
在本发明实施方式中，步骤(2)中的有机酸酐酯化剂的添加量为相对天然葡糖基纳米颗粒质量的0.5％～3％。
在本发明实施方式中，步骤(2)中的醚化试剂的添加量为相对天然葡糖基纳米颗粒质量的1％～10％。
在本发明实施方式中，所述步骤(2)中微波的功率为400～1000W。所述步骤(2)中的反应是在30～50℃条件下反应1～10h。
在本发明实施方式中，防腐剂包括乳酸链球菌素、溶菌酶、甲壳素、ε-聚赖氨酸、纳他霉素、百里酚、丁香酚、Gemini季铵盐等一种或多种。
在本发明实施方式中，步骤(3)中超声的频率20～100kHz。步骤(3)中的反应是在20～50℃条件下反应0.1～5h，实现电荷转移。
本发明的第二个目的是利用上述方法制备得到一种纳米抗菌葡糖基复合粒子。
本发明的第三个目的是将上述的纳米抗菌葡糖基复合粒子应用于食品活性包装、化妆品、纺织品、水凝胶、胶黏剂等方面。
本发明具有以下优点：
1.本发明原料来源广，包括谷物、藻类、动物或微生物，不受产地和季节的限制。
2.以天然葡糖基纳米粒子为原料，利用颗粒表面定位改性与物理场电荷转移技术来制备纳米抗菌复合粒子，应用于抗菌膜及其他表面接触类包装能够有效延长食品的货架期，防止产品腐败变质；
3.该纳米抗菌葡糖基复合粒子的粒径50～1000nm，表面zeta电位0～-10mV，广谱抑菌率>98％；可用于食品、纺织、日化、医药等诸多领域等领域，如食品活性包装、化妆品、纺织品、水凝胶、胶黏剂等方面具有应用前景。
附图说明
图1为实施例1所得纳米抗菌葡糖基复合粒子的电镜照片(bar 100nm)。
具体实施方式
广谱抑菌率测定方法：
大肠杆菌(E.coli)、金黄色葡萄球菌(S.aureus)、鼠伤寒沙门氏菌(S.typhimurium)、单核细胞增生李斯特菌(L.monocytogenes)等食源性腐败菌种于营养琼脂培养基上划线，37℃培养12h后，挑取单菌落，再于营养肉汤培养基中37℃培养12h，平板计数，并吸取一定量的菌液于100mL营养肉汤培养基中(最终为107CFU/mL)，再适量放入纳米抗菌葡糖基复合粒子，于恒温培养箱中37℃培养，分别在0h、4h、6h、8h、10h、12h和24h测定试样的OD600值，并对培养12h的样品进行平板计数，以测定其抑菌率大小，每组样品三次平行，计算公式如下：
抑菌率(％)＝(空白样品回收菌数-样品回收菌数)/空白样品回收菌数×100％。
表面zeta电位测定方法：
将待测纳米抗菌葡糖基复合粒子配制成0.1％(w/v)的溶液，25℃下用马尔文NanoZS测定仪进行表面zeta电位测定。
天然葡糖基纳米颗粒来源：可利用现有技术手段从生长期谷物籽粒、藻类和动物某些组织提取获得，或者微生物经过活化培养、发酵获得菌体提取获得。具体可参考文献制得：Structure and digestibility of endosperm water-soluble a-glucans fromdifferent sugary maize mutants，Food Chemistry 143(2014)156–162。
实施例1
称取来源于牡蛎的葡糖基纳米颗粒【2.3×107g/mol，分散分子密度1230g/(mol·nm3】配成质量百分比浓度40％的均一水溶液，添加200U/g底物的微生物GH13家族淀粉葡糖苷酶，调节反应体系参数：温度50℃、pH值7.0，恒温催化0.5h；加入底物质量百分比0.5％丁二酸酐、3％环氧乙烯，调节反应体系pH 12，同时结合微波辅助加工技术，调节微波功率800W，50℃条件下反应6h；加入底物质量百分比0.01％甲壳素，利用物理场电荷转移技术，控制超声频率100kHz，20℃条件下反应0.5h，然后沉淀、干燥处理即得到目标产物。
所得目标产物的平均粒径110nm，表面zeta电位-5.2mV，广谱抑菌率98.7％。
实施例2
称取来源于稻米的葡糖基纳米颗粒【7.3×106g/mol，分散分子密度1510(mol·nm3)】配成质量百分比浓度10％的均一水溶液，添加50U/g底物的微生物GH13家族麦芽糖苷酶，调节反应体系参数：温度30℃、pH值6.0，恒温催化8h；加入底物质量百分比3％乙酸酐、1％环氧乙烯，调节反应体系pH 10，同时结合微波辅助加工技术，调节微波功率400W，30℃条件下反应10h；加入底物质量百分比0.5％乳酸链球菌素，利用物理场电荷转移技术，控制超声频率50kHz，50℃条件下反应2h，然后沉淀、干燥处理即得到目标产物。
所得目标产物的平均粒径170nm，表面zeta电位-7.5mV，广谱抑菌率99.4％。
实施例3
称取来源于马克斯克鲁维酵母的葡糖基纳米颗粒【1.8×106g/mol，分散分子密度1080g/(mol·nm3)】配成质量百分比浓度20％的均一水溶液，添加100U/g底物的微生物GH13家族麦芽糖苷酶，调节反应体系参数：温度60℃、pH值5.0，恒温催化2h；加入底物质量百分比1％顺丁烯二酸酐、5％乙基氯，调节反应体系pH 8，同时结合微波辅助加工技术，调节微波功率500W，35℃条件下反应3h；加入底物质量百分比1％溶菌酶，利用物理场电荷转移技术，控制超声频率80kHz，30℃条件下反应1h，然后沉淀、干燥处理即得到目标产物。
所得目标产物的平均粒径290nm，表面zeta电位-1.2mV，广谱抑菌率99.3％。
实施例4优化酶的用量
参考实施例1，将微生物GH13家族糖苷水解酶的用量分别替换为30U/g、300U/g，其他条件不变，分别制得相应的复合粒子。测定复合粒子的性能，结构见表1。
表1不同酶用量制得的复合粒子的性能结果
酶用量(U/g) 表面zeta电位(mV) 抑菌率(％)
30 -11.2 75.2
300 -10.5 80.2
结果发现，酶用量过低或酶用量过高，得到复合粒子的表面电荷均小于-10mV，抑菌率也均低于90％。
对比例1
称取来源于牡蛎的葡糖基纳米颗粒【2.3×107g/mol，分散分子密度1230g/(mol·nm3)】配成质量百分比浓度40％的均一水溶液，添加200U/g底物的微生物GH13家族淀粉葡糖苷酶，调节反应体系参数：温度50℃、pH值7.0，恒温催化0.5h；加入底物质量百分比0.5％丁二酸酐、3％环氧乙烯，调节反应体系pH 12，同时结合微波辅助加工技术，调节微波功率800W，50℃条件下反应6h；然后沉淀、干燥处理即得到目标产物。
所得目标产物的表面zeta电位-32.5mV，广谱抑菌率0％。可见，单纯的纳米葡糖基粒子的抗菌活性为0。此外，单纯利用等量的甲壳素进行抗菌实验，发现广谱抑菌率为89.4％。
对比例2
称取来源于牡蛎的葡糖基纳米颗粒【2.3×107g/mol，分散分子密度1230g/(mol·nm3】配成质量百分比浓度40％的均一水溶液，添加200U/g底物的微生物GH13家族淀粉葡糖苷酶，调节反应体系参数：温度50℃、pH值7.0，恒温催化0.5h；加入底物质量百分比0.5％丁二酸酐、3％环氧乙烯，调节反应体系pH 12，同时结合微波辅助加工技术，调节微波功率800W，50℃条件下反应6h；加入底物质量百分比0.01％甲壳素，省略超声电荷转移过程，在20℃条件下直接搅拌反应0.5h，然后沉淀、干燥处理即得到目标产物。
所得目标产物的平均粒径625nm，表面zeta电位-9.2mV，广谱抑菌率91.7％。

Claims (9)

1.一种纳米抗菌葡糖基复合粒子的加工方法，其特征在于，所述方法包括如下步骤：
（1）将天然葡糖基纳米颗粒分散在水中，添加50~200 U/g天然葡糖基纳米颗粒的微生物GH13家族糖苷水解酶进行催化反应；
（2）反应完全后，加入有机酸酐酯化剂、醚化试剂，调节pH至7 ~ 13，微波环境下进行反应；
（3）反应完全后，加入相对天然葡糖基纳米颗粒0.01-1%质量百分比的防腐剂，超声环境下进行反应，然后沉淀、干燥；
防腐剂包括乳酸链球菌素、溶菌酶、甲壳素中的一种或多种。
2.根据权利要求1所述的方法，其特征在于，所述天然葡糖基纳米颗粒的分子量为106 g/mol ~108 g/mol，分散分子密度（1000~2000 ）g·mol-1·nm-3。
3.根据权利要求1所述的方法，其特征在于，步骤（1）中的天然葡糖基纳米颗粒在水中的质量浓度为10~40%。
4.根据权利要求1所述的方法，其特征在于，步骤（1）中的反应是在温度30~70℃、pH值3.5~7.0下恒温催化0.5~12 h。
5.根据权利要求1所述的方法，其特征在于，步骤（2）中的有机酸酐酯化剂的添加量为相对天然葡糖基纳米颗粒质量的0.5%~3 %。
6.根据权利要求1所述的方法，其特征在于，步骤（2）中的醚化试剂的添加量为相对天然葡糖基纳米颗粒质量的1%~10 %。
7.根据权利要求1所述的方法，其特征在于，步骤（3）中超声的频率20~100 kHz， 步骤（3）中的反应是在20~50℃条件下反应0.1~5 h，实现电荷转移。
8.权利要求1-7任一所述的方法制得的纳米抗菌葡糖基复合粒子。
9.权利要求8所述的纳米抗菌葡糖基复合粒子在食品活性包装、化妆品、纺织品、水凝胶、胶黏剂方面的应用。
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