CN109566954B - 一种包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液及制备方法与应用 - Google Patents
一种包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液及制备方法与应用 Download PDFInfo
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Abstract
本发明公开一种包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液的制备方法与应用。本发明采用木质素为还原剂制备木质素包覆的纳米银抗菌剂,并以天然磷脂或合成磷脂、胆固醇为脂质双分子层基质,油溶性月桂精油为抗氧化增强剂,与木质素包覆的纳米银抗菌剂复合,制备得到包埋月桂精油和纳米银的多功能脂质体;然后该多功能脂质体与壳聚糖溶液混合,制备得到所述涂膜液。本发明的包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液应用于食品包装时,作为抗氧化作用的月桂精油具有良好的持久抗氧化作用;木质素包覆的纳米银具有良好的抗菌作用,且纳米银为缓慢释放,大大降低了其在食品应用中的毒性,减少了对人体造成的潜在危害。
Description
技术领域
本发明涉及食品包装材料领域,特别涉及包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液及其制备方法与在食品包装的应用。
背景技术
随着人们生活水平的不断提高,鲜切或生鲜食品发展迅速。传统的食品包装功能性单一,不能满足现代食品贮藏保鲜的需求。因此,需要开发出一种新型的多功能的(抗菌、抗氧化)食品保鲜材料,以防止食品氧化或受微生物侵入而引起的衰败、腐烂,从而延长食品的新鲜度及贮藏期。月桂精油来源于月桂树,是一种具有强抗氧化作用的活性物质,其主要成分为松萜或蒎烯、月桂烯、柠檬油精、芳樟醇、蒿脑、丁子香酚和胡椒酚等。月桂精油作为天然抗氧化剂被广泛应用于化妆品、食品添加剂、药物等领域,但其在使用过程中易受外界因素的影响,如易挥发、对光热敏感等,这限制了其进一步的广泛应用,故寻找一种良好的载体来包埋精油,避免其受外界干扰,更甚可达到缓慢释放的效果,具有重要的意义。
银纳米颗粒是一种强的抗菌剂、不产生耐药性。但近年来有研究发现银纳米颗粒具有潜在累积毒性,会对人身体造成潜在的伤害。当银纳米颗粒作为抗菌剂添加到包装材料中时,游离的银纳米颗粒会对人体造成累积损伤。因此,寻找一种载体来包埋银纳米颗粒,防止其大量泄漏、溢出是很有必要的。
脂质体是一种人工膜,可将药物包埋于类脂质双分子层内而形成的微囊包结构,其膜壁主要由磷脂和胆固醇构成。脂质体微囊包结构中含有亲疏水部分,可将亲水性物质包埋于内部亲水层,而疏水性物质被包封于双分子层间。
壳聚糖是一种具有良好成膜性、无毒、可生物降解的天然多糖,在食品活性包装材料领域具有广泛应用。但壳聚糖本身抗菌活性低,且功能单一。
发明内容
本发明的目的在于针对现有技术的不足,提供了一种食品包装用涂膜液,具体为有抗菌和抗氧化活性的、包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液。
本发明的目的还在于提供一种包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液的制备方法。该制备方法采用天然磷脂或合成磷脂、胆固醇为脂质双分子层基质,油溶性月桂精油为抗氧化增强剂,与木质素包覆的纳米银抗菌剂复合,制备得到包埋月桂精油和纳米银的多功能脂质体;然后该多功能脂质体与壳聚糖溶液混合,制备得到包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液。
本发明的目的还在于所述的一种包埋月桂精油和纳米银的脂质体/壳聚糖涂膜液可应用于食品包装。
本发明的目的通过如下技术方案实现。
一种包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液的制备方法,采用木质素还原银氨溶液,制备亲水性木质素纳米银复合抗菌剂;再与磷脂、胆固醇以及月桂精油混合,获得复合脂质体;而后与壳聚糖溶液混合,制备抗菌、抗氧化活性的壳聚糖基涂膜液,具体包括如下步骤:
(1)按照专利ZL201410034717.8公开的方法,搅拌条件下,将银氨溶液加入木质素溶液中混合均匀,辅以微波加热进行反应,将得到的木质素包覆的纳米银复合物用超纯水透析至检测不出银离子,得到木质素包覆的纳米银复合抗菌剂;
(2)在搅拌条件下,向无水乙醇中加入磷脂和胆固醇,使其充分溶解,再加入月桂精油抗氧化剂,混合均匀,除去溶剂得到复合膜;
(3)将所得复合薄膜置于含步骤(1)所述的纳米银抗菌剂的超纯水或磷酸盐缓冲溶液中震荡水化,再经一定温度下水合,而后以超声细胞破碎仪超声,得到多功能脂质体;
(4)向醋酸溶液中加入壳聚糖,然后与所述多功能脂质体复合,得到所述包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液。
进一步地,步骤(2)中,所述磷脂为天然磷脂(大豆卵磷脂、蛋黄磷脂)或合成磷脂(二棕榈酰磷脂酰胆碱、二棕榈酰磷脂酰乙醇胺、二硬脂酰磷脂酰胆碱)中的一种或两种以上组成的混合物。
进一步地,步骤(2)中,所述磷脂溶液的浓度为1-10 g/L。
进一步地,步骤(2)中,所述胆固醇与磷脂的质量比为1:2-1:8。
进一步地,步骤(2)中,所述月桂精油的添加量占混合溶液总体积的0.1%-2%。
进一步地,步骤(3)中,所述纳米银抗菌剂质量浓度为0.001%-5%。
进一步地,步骤(3)中,所述添加超纯水或磷酸盐缓冲溶液的体积与磷脂的质量比为1000:1-100:1。
进一步地,步骤(3)中,所述水合温度为40-60℃。
进一步地,步骤(3)中,所述水合时间为30 min-2 h。
进一步地,步骤(3)中,所述超声破碎仪超声功率为200-400 W。
进一步地,步骤(3)中,所述超声时间为1 min-60 min。
进一步地,步骤(4)中,所述壳聚糖醋酸溶液中,醋酸相对于壳聚糖溶液的体积分数为0.1-1%。
进一步地,步骤(4)中,壳聚糖的质量分数为0. 1-1%。
进一步地,步骤(4)中,所述复合涂膜液中多功能脂质体溶液与壳聚糖溶液的体积比1:1-1:10。
本发明得到的涂膜液,月桂精油、纳米银均为缓慢释放,且存放168小时后,月桂精油的累积释放率为30-40 wt%、纳米银的累积释放率为8-12 wt%。
由上述任一项所述的制备方法制得的包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液,同时具有良好的抗菌、抗氧化活性。
本发明利用木质素与银纳米颗粒的表面效应,以及木质素亲水特性,解决银纳米颗粒疏水性的问题,而且可作为纳米银合成过程中的绿色还原剂;利用月桂精油作为抗氧化剂,抗氧化活性强,解决壳聚糖活性包装无抗氧化的问题;利用脂质体将具有抗菌作用的水溶性木质素纳米银包埋于内水相,抗氧化作用的疏水性精油包封于双分子层间,形成一种具有抗菌、抗氧化活性的复合脂质体结构,从而解决月桂精油易挥发、热敏性等问题,提高其稳定性,促进抗氧化活性的持久性;且固定银纳米颗粒,减缓其释放,在保证具有良好抗菌活性的同时降低纳米银对人体产生的累积毒性作用。使脂质体/壳聚糖复合涂膜液具有优良的抗菌、抗氧化活性,拓展壳聚糖在食品保鲜领域的应用。
所述的包埋月桂精油和纳米银的脂质体/壳聚糖涂膜液应用于食品包装中。
本发明得到的涂膜液中,月桂精油、纳米银为缓慢释放,且存放168小时后,月桂精油的累积释放率为30-40 wt%、纳米银的累积释放率为8-12 wt%。本发明的包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液应用于食品包装时,作为抗氧化作用的月桂精油具有良好的持久抗氧化作用;木质素包覆的纳米银具有良好的抗菌作用,且纳米银为缓慢释放,大大降低了其在食品应用中的毒性,减少了对人体造成的潜在危害。
与现有技术相比,本发明具有如下优点和有益效果:
(1)本发明采用的脂质体作为月桂精油、木质素纳米银的理想包封囊包,可提高精油的热稳定性,减缓其挥发;可减缓或降低银纳米颗粒的释放,大大降低了其在食品应用中的毒性,减少了对人体造成潜在的危害,拓展了银纳米颗粒作为抗菌剂在食品保鲜中的应用;
(2)本发明利用木质素亲水性,包覆银纳米颗粒,提高其亲水性,有利于脂质体对银纳米颗粒的包封;
(3)本发明制备方法工艺简单,原料来源广,能耗低,有利于大规模工业化生产;
(4)本发明的包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液,具有良好的抗菌、抗氧化效果,且活性持久,有利于应用于食品包装中。
附图说明
图1是实施例2得到的脂质体中月桂精油和银纳米颗粒的累积释放结果图;
图2是实施例2得到的脂质体/壳聚糖基涂膜液对金黄色葡萄球菌和大肠杆菌抗菌的实验抑菌圈的直径数据图。
具体实施方式
以下结合具体实施例及附图对本发明技术方案作进一步详细说明,但本发明实施例及保护范围不限于此。
实施例1
包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液的制备,具体步骤如下:
(1)在搅拌条件下,向无水乙醇中加入磷脂和胆固醇,使其充分溶解,磷脂浓度为1g/L,胆固醇与磷脂比为1:8,随后添加占总体积0.1%的月桂精油抗氧化剂,混合均匀,除去溶剂成复合膜;
(2)将所得复合膜置于含质量浓度0.001%木质素包覆纳米银复合抗菌剂的超纯水或磷酸盐缓冲溶液中震荡水化(水化溶液的体积与磷脂质量比为100:1),再经40 ℃下水合30 min,而后用功率为200 W超声细胞破碎仪超声1 min,得到所述多功能脂质体;
(3)配置0.1%的壳聚糖醋酸稀溶液(醋酸浓度相对于壳聚糖溶液的体积分数为0.1%),与该多功能脂质体复合,体积比为10:1,得到所述包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液。
实施例2
包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液的制备,具体步骤如下:
(1)在搅拌条件下,向无水乙醇中加入磷脂和胆固醇,使其充分溶解,磷脂浓度为2.5 g/L,胆固醇与磷脂比为1:5,随后添加占总体积0.25%的月桂精油抗氧化剂,混合均匀,除去溶剂成复合膜;
(2)将所得复合膜置于含0.05%木质素包覆纳米银复合抗菌剂的超纯水或磷酸盐缓冲溶液中震荡水化(水化溶液的体积与磷脂质量比为400:1),再经50 ℃下水合1 h,而后用功率为300 W超声细胞破碎仪超声5 min,得到所述多功能脂质体;
(3)配置0.5%的壳聚糖醋酸稀溶液(醋酸浓度相对于壳聚糖质量分数为0.2%),与该多功能脂质体复合,体积比为5:1,得到所述包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液。
制备的多功能脂质体中月桂精油和纳米银的累积释放率结果图如图1所示,由图1可知,脂质体中月桂精油和纳米银的释放较缓慢,释放168 h后,复合脂质体中月桂精油和纳米银的释放率较低,分别仅为39.62%、11.79%,说明脂质体对疏水性月桂精油和亲水性纳米银均具有很好的包覆效率,从而达到缓慢释放。
制备的壳聚糖/复合脂质体抗菌涂膜液对金黄色葡萄球菌和大肠杆菌抗菌的实验抑菌圈的直径数据图如图2所示,由图2可知,将涂膜液涂抹在聚乙烯醇膜上,得到聚乙烯醇/壳聚糖/复合脂质体抗菌复合膜,而后将其用于抗菌实验中。所制备的聚乙烯醇/壳聚糖/复合脂质体抗菌复合膜对金黄色葡萄球菌和大肠杆菌均有较好的抗菌效果,说明脂质体包覆纳米银并没有降低其抗菌效果;而没有包覆纳米银的脂质体复合膜没有抗菌活性。
制备的复合脂质体的抗氧化实验数据如表1所示,由表1可知,以三种方法对复合脂质体的抗氧化性能进行了考察,结果表明所制备的复合脂质体具有良好的持久性抗氧化效果,说明脂质体包埋月桂精油降低了其释放率,提高了精油的稳定性,使其用于食品保鲜中时可达到持久抗氧化效果。
表1复合脂质体的抗氧化性能:分别以维生素C、硫酸亚铁和水溶性维生素E为当量
DPPH (μg Vc/0.1 mL) | FRAP (μg FeSO<sub>4</sub>/0.1 mL) | ABTS (μg Trolox/0.1 mL) | |
月桂精油脂质体 | 7.68±0.28 | 32.95±0.28 | 165.32±1.63 |
月桂精油/纳米银脂质体 | 6.98±0.35 | 30.31±0.56 | 155.56±5.51 |
实施例3
包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液的制备,具体步骤如下:
(1)在搅拌条件下,向无水乙醇中加入磷脂和胆固醇,使其充分溶解,磷脂浓度为5g/L,胆固醇与磷脂比为1:3,随后添加占总体积1%的月桂精油抗氧化剂,混合均匀,除去溶剂成复合膜;
(2)将所得复合膜置于含1%木质素包覆纳米银复合抗菌剂的超纯水或磷酸盐缓冲溶液中震荡水化(水化溶液的体积与磷脂质量比为600:1),再经55 ℃下水合1.5小时,而后用功率为400 W超声细胞破碎仪超声30 min,得到所述多功能脂质体;
(3)配置0.8%的壳聚糖醋酸稀溶液(醋酸浓度相对于壳聚糖溶液的体积分数为0.5%),与该多功能脂质体复合,体积比为3:1,得到所述包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液。
实施例4
包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液的制备,具体步骤如下:
(1)在搅拌条件下,向无水乙醇中加入磷脂和胆固醇,使其充分溶解,磷脂浓度为10 g/L,胆固醇与磷脂比为1:2,随后添加占总体积2%的月桂精油抗氧化剂,混合均匀,除去溶剂成复合膜;
(2)将所得复合膜置于含5%木质素包覆纳米银复合抗菌剂的超纯水或磷酸盐缓冲溶液中震荡水化(水化溶液的体积与磷脂质量比为1000:1),再经60 ℃下水合2 h,而后用功率为400 W超声细胞破碎仪超声1 min,得到所述多功能脂质体;
(3)配置1%的壳聚糖醋酸稀溶液(醋酸浓度相对于壳聚糖溶液的体积分数为1%),与该多功能脂质体复合,体积比为1:1,得到所述包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液。
以上实施例仅为本发明较优的实施方式,仅用于解释本发明,而非限制本发明,本领域技术人员在未脱离本发明精神实质下所作的改变、替换、修饰等均应属于本发明的保护范围。
Claims (9)
1.一种包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液的制备方法,其特征在于,包括如下步骤:
(1)搅拌条件下,将银氨溶液加入木质素溶液中混合均匀,辅以微波加热进行反应,将得到的木质素包覆的纳米银复合物用超纯水透析至检测不出银离子,得到木质素包覆的纳米银抗菌剂;
(2)在搅拌条件下,向无水乙醇中加入磷脂和胆固醇,使其充分溶解,再加入月桂精油,混合均匀,除去溶剂成复合膜;
(3)将所得复合膜置于含步骤(1)中所述木质素包覆的纳米银抗菌剂的超纯水或磷酸盐缓冲溶液中震荡水化,再经水合,而后以超声细胞破碎仪超声,得到多功能脂质体;
(4)向醋酸溶液中加入壳聚糖并充分溶解,然后与所述多功能脂质体复合,得到所述包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液。
2.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,所述磷脂为天然磷脂或合成磷脂中的一种或两种以上组成的混合物。
3.根据权利要求2所述的制备方法,其特征在于,天然磷脂为大豆卵磷脂或蛋黄磷脂,合成磷脂为二棕榈酰磷脂酰胆碱、二棕榈酰磷脂酰乙醇胺或二硬脂酰磷脂酰胆碱。
4.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,所述磷脂溶液的浓度为1-10 g/L;所述胆固醇与磷脂的质量比为1:2-1:8;所述月桂精油的添加量占混合溶液总体积的0.1%-2%。
5.根据权利要求1所述的制备方法,其特征在于,步骤(3)中,所述木质素包覆的纳米银抗菌剂质量浓度为0.001%-5%;所述超纯水或磷酸盐缓冲溶液的体积与磷脂的质量比为1000:1-100:1;所述水合的温度为40-60 ℃;所述水合时间为30 min-2 h;所述超声破碎仪超声的功率为200-400 W;所述超声的时间为1min-60 min。
6.根据权利要求1所述的制备方法,其特征在于,步骤(4)中,所述壳聚糖醋酸溶液中,醋酸相对于壳聚糖溶液的体积分数为0.1-1%;壳聚糖的质量分数为0. 1-1%。
7.根据权利要求1所述的制备方法,其特征在于,步骤(4)中,所述涂膜液中多功能脂质体溶液与壳聚糖溶液的体积比1:1-1:10。
8.由权利要求1-7任一项所述的制备方法制得的包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液,其特征在于,存放168 h后,月桂精油的累积释放率为30-40 wt%、纳米银的累积释放率为8-12 wt%。
9.权利要求8所述的一种包埋月桂精油和纳米银的脂质体/壳聚糖抗菌、抗氧化涂膜液应用于食品包装材料中。
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