CN113321852A - Lae和植物精油复合抗菌剂及可降解包装薄膜制备方法 - Google Patents

Lae和植物精油复合抗菌剂及可降解包装薄膜制备方法 Download PDF

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CN113321852A
CN113321852A CN202110658528.8A CN202110658528A CN113321852A CN 113321852 A CN113321852 A CN 113321852A CN 202110658528 A CN202110658528 A CN 202110658528A CN 113321852 A CN113321852 A CN 113321852A
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lae
antibacterial agent
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汤晓智
徐瑶瑶
高成成
孟令晗
侯克洪
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Tianjin Suxing Material Technology Co ltd
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Abstract

本发明提出的是一种LAE和植物精油复合抗菌剂及可降解抗菌包装薄膜的制备方法,利用LAE和羟丙基‑β‑环糊精协同乳化作用,以及利用羟丙基‑β‑环糊精的空腔结构包埋LAE和植物精油制备复合抗菌剂,并通过挤压热加工使复合抗菌剂与热加工温度较低的可降解材料混合完成可降解抗菌包装薄膜。本发明利用表面活性剂LAE和羟丙基‑β‑环糊精协同乳化,增强包埋乳化的效果,利用空腔结构对LAE和植物精油的保护提高复合抗菌剂的热稳定性,与热加工温度低的可降解材料复合进一步提高利用度和抗菌效果,降低其与食品中其他物质的相互作用,具有协同抗菌作用,可以降低每种抗菌剂的添加量,提高使用安全性和抗菌保鲜能力。

Description

LAE和植物精油复合抗菌剂及可降解包装薄膜制备方法
技术领域
本发明涉及的是抗菌材料的制备方法,特别是一种Nα-月桂酰-L-精氨酸乙酯盐酸盐和植物精油复合抗菌可降解抗菌包装薄膜及其制备方法,属于食品保鲜技术领域。
背景技术
植物精油是由植物产生的具有芳香气味的代谢产物,不溶于水,易溶于乙醇等有机溶剂。作为一种天然提取物,植物精油具有广谱抗菌性,但在使用过程中存在易挥发、易氧化、气味强、使用量大等缺点。Nα-月桂酰-L-精氨酸乙酯盐酸盐(Nα-lauroyl-L-arginateethylester,简称LAE)是一种阳离子表面活性剂,同时对多种食源性病原菌有较高的抑制活性,但LAE由于其阳离子性质容易与食品中阴离子成分相互作用,导致抗菌防腐能力下降;LAE在高于约50 ppm的浓度下会产生苦味,可能会影响食品的接受度。上述这些问题使得植物精油和LAE在使用过程中仍然伴随着一些限制。
此外,现有食品保鲜工艺中,抗菌剂主要使用方法之一是将其制成抗菌膜,特别是环保可降解抗菌膜,但是目前抗菌膜的制备主要采用流延法,该法使用大量溶剂、产量低、不适合大规模生产,大部分停留在实验阶段。挤压吹塑热加工是廉价、成熟的生产薄膜材料的工业化生产方法。但这种方法加工温度高,会加大植物精油等抗菌剂的损耗,甚至导致失活,使薄膜抗菌效果下降。因此,提高抗菌剂耐热性和利用度是挤压吹塑制备抗菌包装需要解决的关键难题。
发明内容
本发明的目的在于克服植物精油和LAE在现有食品保鲜实际应用过程中的局限性,和在挤压吹塑制备抗菌膜时热稳定性低的问题,提出一种利用羟丙基-β-环糊精所具有的独特的外亲水内疏水的空腔结构及其与LAE协同乳化对LAE和植物精油进行包埋乳化,提高两种抗菌材料的热稳定性和利用度,并改善两者对食品气味的影响,进而与热加工温度较低的可降解材料通过挤压热加工法混合,并利用植物精油和LAE的协同抗菌作用,得到一种含安全且高效的复合抗菌剂的可降解抗菌包装薄膜的制备方法。
本发明的技术解决方案:一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,具体包括如下步骤:
1)在室温下将质量分数为1~10%的羟丙基-β-环糊精固体粉末溶解于纯水中,得到环糊精溶液;
2)称取质量分数为0.5~5%的LAE固体粉末,加入步骤1)制备的环糊精溶液中充分溶解,得到包埋乳化剂水溶液;
3)在步骤2)制备的包埋乳化剂水溶液中加入体积分数为0.5~5%的植物精油,经过高速分散12000-18000 r/min下处理5-15 min,超声200-750 W功率下处理5-10 min或高压均质20-100MPa下处理,1-3个循环,每个阶段持续1分钟,得到液体复合抗菌剂;
4)将步骤3)制备的液体复合抗菌剂进一步通过喷雾干燥得到复合抗菌剂固体粉末,喷雾干燥处理的进口温度最高为170℃,出口温度最高为100℃,雾化器转速为20~40Hz,进料速度为15~30 r/min,根据进料速度调节出口温度;
5)将步骤4)制备的质量分数为2-7%复合抗菌剂固体粉末与质量分数为68-82%的可降解材料(淀粉、PBAT、PLA、PHB和PCL中的一种或任意多种复合材料)、质量分数为15-20%甘油、质量分数为1-5%硬脂酸通过高速搅拌机混合得到粉料,将制备的粉料通过双螺杆挤出机熔融挤出后冷却切粒得到热塑性母粒,双螺杆挤出机熔融区温度设置为80-130℃;再通过挤压吹塑机制备挤压吹塑得到可降解包装薄膜,挤压吹塑机熔融区温度设置为80-130℃。
与现有技术相比,本发明的优点在于:
1)利用表面活性剂LAE和羟丙基-β-环糊精协同乳化增强包埋乳化的效果;
2)利用羟丙基-β-环糊精的空腔包埋,对LAE和植物精油均有较好的保护作用,进一步提高LAE和植物精油热稳定性和两种抗菌剂的利用度;
3)制备的复合抗菌剂与热加工温度较低的可降解材料混合,进一步提高挤压热加工生产抗菌包装中抗菌剂的利用度和抗菌效果;
4)利用羟丙基-β-环糊精的空腔包埋,对LAE和植物精油均有较好的保护作用降低了LAE和植物精油与食品中其他物质的相互作用,提高两种抗菌剂抗菌效果,降低高浓度下的强烈风味,对抗菌剂起到缓释作用;
5)两种抗菌剂的复合对微生物有协同增效作用,提高抗菌保鲜能力,且可以降低每种抗菌剂的添加量,提高使用安全性。
具体实施方式
下面根据多个实施例进一步说明本发明的技术方案。在本说明书的描述中,各实施例的内容意指结合其描述的具体技术特征包含于本发明的至少一个实施方式中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施方式或示例。而且,描述的具体技术特征可以在任何的一个或多个实施方式或示例中以合适的方式结合。
实施例1
室温下将羟丙基-β-环糊精粉末(3% w/v)溶解于100 mL纯水中,再添加Nα-月桂酰-L-精氨酸乙酯盐酸盐固体粉末(1% w/v)充分溶解后,逐滴加入肉桂精油(3% v/v),继续搅拌2 h,高速分散器18000 r/min条件下处理5 min,最后在450 W功率下,超声处理10min,得到羟丙基-β-环糊精/肉桂精油/Nα-月桂酰-L-精氨酸乙酯盐酸盐复合抗菌剂。
将所得的复合抗菌剂进行喷雾干燥,喷雾干燥器的进口温度为150℃,出口温度最高为100℃,雾化器转速为30 Hz,进料速度为25 r/min,得到复合抗菌剂固体粉末。
将淀粉置于高速搅拌机,再添加5% 的复合抗菌剂固体粉末、1%硬脂酸、20%的甘油(以混合粉料质量分数计),混合30 min,置于聚乙烯包装袋密封24 h,备用。
将制备的粉料均匀喂入双螺杆造粒机,挤出机熔融区温度设置为90℃,螺杆转动频率为18 Hz,粉料经双螺杆挤出机熔融挤出后,冷却切粒,密封包装备用。
将挤压吹塑机加热至设定的温度,平衡30 min,将制备的热塑性淀粉均匀喂入吹塑机,待吹塑机头出料后,将材料拉着上牵引夹棍处,夹紧,并以一定压力吹胀淀粉膜,冷却后制得淀粉挤压吹塑抗菌膜。该包装可以用于食品包装内包装,避免与水接触。
实施例2
室温下将羟丙基-β-环糊精粉末(5% w/v)溶解于100 mL纯水中,再添加Nα-月桂酰-L-精氨酸乙酯盐酸盐固体粉末(2% w/v)充分溶解后,逐滴加入丁香精油(4% v/v),继续搅拌2 h,高速分散器18000 r/min条件下处理5 min,最后在450 W功率下,超声处理10min,得到羟丙基-β-环糊精/丁香精油/Nα-月桂酰-L-精氨酸乙酯盐酸盐复合抗菌剂。
将所得的复合抗菌剂进行喷雾干燥,喷雾干燥器的进口温度为150℃,出口温度最高为100℃,雾化器转速为25 Hz,进料速度为25 r/min,得到复合抗菌剂固体粉末。
将PLA(聚乳酸)、PHB(聚-β-羟丁酸)按一定质量比(3∶1)置于高速搅拌机,再添加7% 的复合抗菌剂固体粉末、0.8%硬脂酸、25%的甘油(以混合粉料质量分数计),混合30min,置于聚乙烯包装袋密封24 h,备用。
将制备的粉料均匀喂入双螺杆造粒机,挤出机熔融区温度设置为140℃,螺杆转动频率为18 Hz,粉料经双螺杆挤出机熔融挤出后,冷却切粒,密封包装备用。
将挤压吹塑机加热至设定的温度,平衡30 min,将制备的热塑性淀粉均匀喂入吹塑机,待吹塑机头出料后,将材料拉着上牵引夹棍处,夹紧,并以一定压力吹胀PLA/PHB膜,冷却后制得PLA/PHB挤压吹塑抗菌膜。该包装可以用于食品的外包装,延长食品保鲜期。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。

Claims (10)

1.一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,利用LAE和植物精油的协同抗菌性,LAE和羟丙基-β-环糊精协同乳化作用,以及利用羟丙基-β-环糊精的空腔结构包埋LAE和植物精油制备复合抗菌剂,提高LAE和植物精油的热稳定性和抗菌性,并通过挤压热加工使复合抗菌剂与热加工温度较低的可降解材料混合完成可降解抗菌包装薄膜;其特征在于,该方法具体包括如下步骤:
1)在室温下将羟丙基-β-环糊精固体粉末溶解于纯水中,得到环糊精溶液;
2)称取LAE固体粉末,加入步骤1)制备的环糊精溶液中充分溶解,得到包埋乳化剂水溶液;
3)在步骤2)制备的包埋乳化剂水溶液中加入植物精油,经过高速分散和超声处理或高压均质后得到液体复合抗菌剂;
4)将步骤3)制备的液体复合抗菌剂进一步通过喷雾干燥得到复合抗菌剂固体粉末;
5)将步骤4)制备的复合抗菌剂固体粉末与可降解材料、甘油、硬脂酸通过高速搅拌机混合得到粉料,将制备的粉料通过双螺杆挤出机熔融挤出后冷却切粒得到热塑性母粒,再通过挤压吹塑机制备挤压吹塑得到可降解抗菌包装薄膜。
2.根据权利要求1所述的一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,其特征在于:所述步骤1)中羟丙基-β-环糊精的质量分数为1~10%。
3.根据权利要求1所述的一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,其特征在于:所述步骤2)中LAE固体粉末的质量分数为0.5~5%。
4.根据权利要求1所述的一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,其特征在于:所述步骤3)中植物精油的体积分数为0.5~5%。
5.根据权利要求1所述的一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,其特征在于:所述步骤3)中高速分散的具体条件为在12000-18000 r/min下处理5-15min,超声处理的具体条件为在200-750 W功率下处理5-10 min,或采用高压均质在20-100MPa下处理,1-3个循环,每个阶段持续1分钟。
6.根据权利要求1所述的一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,其特征在于:所述步骤4)中喷雾干燥处理的进口温度最高为170℃,出口温度最高为100℃,雾化器转速为20~40 Hz,进料速度为15~30 r/min,根据进料速度调节出口温度。
7.根据权利要求1所述的一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,其特征在于:所述步骤5)中复合抗菌剂固体粉末的质量分数为2-7%,可降解材料的质量分数为68-82%,甘油的质量分数为15-20%,硬脂酸的质量分数为1-5%。
8.根据权利要求1所述的一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,其特征在于:所述步骤5)中的可降解材料为淀粉、PBAT、PLA、PHB和PCL中的一种或任意多种复合材料。
9.根据权利要求1所述的一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,其特征在于:所述步骤5)中双螺杆挤出机熔融区温度设置为80-130℃。
10.根据权利要求1所述的一种LAE和植物精油复合抗菌剂及可降解包装薄膜的制备方法,其特征在于:所述步骤5)中挤压吹塑机熔融区温度设置为80-130℃。
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CN113881206A (zh) * 2021-10-15 2022-01-04 明新孟诺卡(江苏)新材料有限公司 一种具备天然抗菌功能色母粒及其制备工艺
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CN113881206A (zh) * 2021-10-15 2022-01-04 明新孟诺卡(江苏)新材料有限公司 一种具备天然抗菌功能色母粒及其制备工艺
CN115960446A (zh) * 2022-12-27 2023-04-14 浙江农林大学 一种精油/羧基化纳米纤维素/聚乳酸包装膜的制备方法

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