CN113712072B - 一种丁香精油皮克林乳液涂膜保鲜剂及其制备方法和应用 - Google Patents
一种丁香精油皮克林乳液涂膜保鲜剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于食品领域,具体涉及一种丁香精油皮克林乳液涂膜保鲜剂及其制备方法和应用。该制备方法,包括以下步骤,用乙醇和玉米醇溶蛋白粉末配置20mg/ml的玉米醇溶蛋白溶液,超纯水和酪蛋白酸钠配置0.4‑6mg/ml的酪蛋白酸钠溶液,磁力搅拌过夜;将的20mg/ml玉米醇溶蛋白溶液逐滴滴入的0.4‑6mg/ml的酪蛋白酸钠溶液中,在500rpm磁力搅拌30min;再使用旋转蒸发仪在40℃蒸发掉溶液中的乙醇,蒸发掉的乙醇用超纯水替代;然后加入丁香精油,高速均质3min,得到丁香精油皮克林乳液;1%v/v乙酸和壳聚糖配置1.5%‑2%w/v壳聚糖溶液,在壳聚糖溶液中加入丁香精油皮克林乳液,高速均质3min,超声30min消泡,得到丁香精油皮克林乳液涂膜保鲜剂。
Description
技术领域
本发明属于食品领域,具体涉及一种丁香精油皮克林乳液涂膜保鲜剂及其制备方法和应用。
背景技术
植物精油是植物产生的具有芳香味的疏水性化合物,具有安全性、广谱抗菌性和抗氧化活性。迄今,已有诸多植物精油作为食品防腐剂代替合成防腐剂应用于食品保鲜,丁香精油是一种极具潜力的食品保鲜天然植物精油。丁香精油是从丁香树干花蕾中提取,由于高浓度的丁香酚和其它酚类化合物的存在,使其具有生物活性和抗菌活性,它能使细胞蛋白变性,并与细胞膜磷脂发生化学反应,从而改变细胞膜磷脂的通透性。丁香精油能够杀死一些重要的食源性病原菌,包括金黄色葡萄球菌、大肠杆菌、单核增生李斯特菌和伤寒沙门氏菌,并具有抗自由基和金属螯合活性。此外丁香精油对其它革兰氏阳性细菌、革兰氏阴性细菌和真菌都有较强的抑制作用。目前,丁香精油常被广泛应用在食品防腐保鲜领域。有研究将丁香精油通过浸泡法直接应用在火腿肠上,接种金黄色葡萄球菌ATCC和大肠杆菌O157:H7,结果显示丁香精油能够很好地延缓了火腿肠腐败程度;将丁香精油、芥末精油、桂皮精油复配,发现其对生鲜调理鸡肉的保鲜效果具有协同增效作用,使生鲜调理鸡肉的货架期延长至21天。
虽然将丁香精油直接应用到食品上,可以起到抗菌和抗氧化作用,但是其自身的易挥发性会降低它的利用率,并且高浓度的丁香精油导致食品具有强烈的丁香精油特殊风味。反之,低浓度的精油却达不到理想的杀菌效果。此外,在食品冷藏期间,随着时间增加,丁香精油的抑菌和抗氧化活性下降趋势较快。因此采取包封技术抑制丁香精油挥发,提高水溶性,从而提高精油在食品防腐保鲜方面的利用率和抗菌性。水包油型纳米乳液具有高稳定性、较强的物理化学性质、较好的控释性和良好的生物活性。到目前为止,常见的乳化剂都是表面活性剂,如吐温20、吐温80,于是学者们开始研究天然化合物制成固体颗粒稳定活性物质。与表面活性剂不同的是,在油水相界面,纳米颗粒吸附后可形成致密的界面层,有效防止液滴堆积。同时它具有更好的稳定性,优越的包埋率,更低的电解率,在一定程度上更好的保护活性小分子。由于蛋白质和多糖具有增稠性和凝胶性,常被用作乳化剂和稳定剂。将抗菌性和抗氧化性的活性小分子乳化、成膜,然后采用包裹、喷涂、浸泡等方式使之覆盖于在食品表面,用来阻隔氧气的透过,减少风味物质挥发、水分散失,增加食品表面的光泽,防止食品中组分的迁移和扩散降低脂肪氧化,减少微生物的生长,从而延缓食品的腐败变质、延长食品货架期。
发明内容
为此,需要提供一种丁香精油皮克林乳液涂膜保鲜剂及其制备方法和应用。本发明采用抗溶剂法制备玉米醇溶蛋白/酪蛋白酸钠纳米颗粒包埋丁香精油,研究不同含量丁香精油皮克林乳液对壳聚糖膜的机械性能、阻水性、微观结构、抗菌性和释放率的影响。
为实现上述目的,本发明采用如下技术方案:
一种丁香精油皮克林乳液涂膜保鲜剂的制备方法,包括以下步骤,
步骤S1、用乙醇和玉米醇溶蛋白粉末配置20mg/ml的玉米醇溶蛋白溶液,超纯水和酪蛋白酸钠配置0.4-6mg/ml的酪蛋白酸钠溶液,磁力搅拌6-12h;
步骤S2、将的20mg/ml玉米醇溶蛋白溶液逐滴滴入的0.4-6mg/ml的酪蛋白酸钠溶液中,在500rpm磁力搅拌30min;
步骤S3、再使用旋转蒸发仪在40℃蒸发掉溶液中的乙醇,蒸发掉的乙醇用超纯水替代,使溶液体积不变;
步骤S4、然后加入丁香精油,高速均质3min,得到丁香精油皮克林乳液;
步骤S5、1%v/v乙酸和壳聚糖配置1.5%-2%w/v壳聚糖溶液,在壳聚糖溶液中加入20%w/w甘油,然后在壳聚糖溶液中加入丁香精油皮克林乳液,高速均质3min,超声30min消泡,得到丁香精油皮克林乳液涂膜保鲜剂。
本技术方案进一步的优化,所述乙醇的浓度为70%-80%。
本技术方案进一步的优化,所述步骤S2中玉米醇溶蛋白溶液与酪蛋白酸钠溶液的比例为1:10。
本技术方案进一步的优化,所述步骤S4中丁香精油浓度为0.5%-2%v/v。
本技术方案进一步的优化,所述步骤S5中在壳聚糖溶液中加入丁香精油皮克林乳液后,使丁香精油在总溶液中浓度为0.2%-0.6%v/v。
本技术方案进一步的优化,所述步骤S4和S5中高速均质的速度为15000-20000rpm。
由上述任意一项技术方案所述的方法制备得到的丁香精油皮克林乳液涂膜保鲜剂。
丁香精油皮克林乳液涂膜保鲜剂作为食品保鲜剂的应用。应用于果蔬、肉制品。
丁香精油皮克林乳液涂膜保鲜剂保鲜烧鸡的方法,包括如下步骤,
步骤S1、将鲜烧鸡浸泡到0℃~4℃的丁香精油皮克林乳液涂膜保鲜剂中,浸泡20-60s;
步骤S2、鲜烧鸡从丁香精油皮克林乳液涂膜保鲜剂浸泡池中提出,在4℃冷藏室沥干处理,装入保鲜袋中4℃冷藏。
区别于现有技术,上述技术方案具有如下有益效果:
1.玉米醇溶蛋白-酪蛋白酸钠纳米颗粒乳化包埋丁香精油,减少丁香精油的挥发损失,对丁香精油的包埋率达62.91%。
2.与纯壳聚糖涂膜相比,添加了丁香精油皮克林乳液的壳聚糖复合膜的抗张强度从26.15MPa提升至38.67MPa。
3.丁香精油皮克林乳液涂膜保鲜剂对大肠杆菌和金黄色葡萄球菌均表现出强抑菌性,对大肠杆菌的抑菌圈直径达3.29mm,对金黄色葡萄球菌抑菌圈直径达6.15mm。
4.应用范围广,果蔬、肉制品均可使用丁香精油皮克林乳液涂膜保鲜剂保鲜。
附图说明
图1为丁香精油皮克林乳液涂膜保鲜剂制备技术路线图;
图2为不同添加量丁香精油皮克林乳液涂膜保鲜剂的机械强度图;
图3为不同添加量丁香精油皮克林乳液涂膜保鲜剂的扫描电镜图;
图4为不同添加量丁香精油皮克林乳液涂膜保鲜剂的傅里叶红外光谱图;
图5为不同添加量丁香精油皮克林乳液涂膜保鲜剂的对大肠杆菌(E.coli)和金黄色葡萄球菌(S.aureus)的抑菌圈直径图;
图6为固定传送带示意图;
图7为对照组—实施例1和实施例3成品展示图;
图8为符离集烧鸡贮藏期间菌落总数图。
具体实施方式
为详细说明技术方案的技术内容、构造特征、所实现目的及效果,以下结合具体实施例并配合附图详予说明。
请参阅图1所示,为丁香精油皮克林乳液涂膜保鲜剂制备技术路线图,本发明提出了一种丁香精油皮克林乳液涂膜保鲜剂的制备方法,包括以下步骤,
步骤S1、用70%-80%乙醇和玉米醇溶蛋白粉末配置20mg/ml的玉米醇溶蛋白溶液,超纯水和酪蛋白酸钠配置0.4-6mg/ml的酪蛋白酸钠溶液,磁力搅拌6-12h;
步骤S2、将1ml的20mg/ml玉米醇溶蛋白溶液逐滴滴入10ml的0.4-6mg/ml的酪蛋白酸钠溶液中,在500rpm磁力搅拌30min;
步骤S3、再使用旋转蒸发仪在40℃蒸发掉溶液中的乙醇,蒸发掉的乙醇用超纯水替代,使溶液体积不变;
步骤S4、然后加入0.5%-2%v/v丁香精油,15000-20000rpm高速均质3min,得到丁香精油皮克林乳液。
步骤S5、1%v/v乙酸和壳聚糖配置1.5%-2%w/v壳聚糖溶液,在壳聚糖溶液中加入丁香精油皮克林乳液,使丁香精油在总溶液中浓度为0.2%-0.6%v/v,在15000-20000rpm高速均质3min,超声30min消泡,得到丁香精油皮克林乳液涂膜保鲜剂。
由上述任意一项技术方案所述的方法制备得到的丁香精油皮克林乳液涂膜保鲜剂。
丁香精油皮克林乳液涂膜保鲜剂作为食品保鲜剂的应用。应用于果蔬、肉制品。
实施例1—对照组:
丁香精油皮克林乳液涂膜保鲜剂的制备方法:
步骤S1、1%v/v乙酸和壳聚糖配置1.5%w/v壳聚糖溶液,在壳聚糖溶液中加入20%w/w甘油。15000rpm均质3min,超声30min消泡,得到纯壳聚糖膜(对照组)保鲜剂。
实施例2:
丁香精油皮克林乳液涂膜保鲜剂的制备方法:
步骤S1、用75%乙醇和玉米醇溶蛋白配置20mg/ml的玉米醇溶蛋白溶液;超纯水和酪蛋白酸钠配置4mg/ml的酪蛋白酸钠溶液,磁力搅拌12h。
步骤S2、将1ml的20mg/ml玉米醇溶蛋白溶液逐滴滴入10ml的4mg/ml的酪蛋白酸钠溶液中,在500rpm磁力搅拌30min。
步骤S3、再使用旋转蒸发仪在40℃蒸发掉溶液中的乙醇,蒸发掉的乙醇用超纯水替代,使溶液体积不变。
步骤S4、然后加入1%v/v丁香精油,15000rpm均质3min,得到丁香精油皮克林乳液。
步骤S5、1%v/v乙酸和壳聚糖配置1.5%w/v壳聚糖溶液,在壳聚糖溶液中加入20%w/w甘油。然后在壳聚糖溶液中加入丁香精油皮克林乳液,使丁香精油在总溶液中浓度为0.2%v/v。15000rpm均质3min,超声30min消泡,得到丁香精油皮克林乳液涂膜保鲜剂。
实施例3:
丁香精油皮克林乳液涂膜保鲜剂的制备方法:
步骤S1、用75%乙醇和玉米醇溶蛋白配置20mg/ml的玉米醇溶蛋白溶液;超纯水和酪蛋白酸钠配置4mg/ml的酪蛋白酸钠溶液,磁力搅拌12h。
步骤S2、将1ml的20mg/ml玉米醇溶蛋白溶液逐滴滴入10ml的4mg/ml的酪蛋白酸钠溶液中,在500rpm磁力搅拌30min。
步骤S3、再使用旋转蒸发仪在40℃蒸发掉溶液中的乙醇,蒸发掉的乙醇用超纯水替代,使溶液体积不变。
步骤S4、然后加入1%v/v丁香精油,15000rpm均质3min,得到丁香精油皮克林乳液。
步骤S5、1%v/v乙酸和壳聚糖配置1.5%w/v壳聚糖溶液,在壳聚糖溶液中加入20%w/w甘油。然后在壳聚糖溶液中加入丁香精油皮克林乳液,使丁香精油在总溶液中浓度为0.4%v/v。15000rpm均质3min,超声30min消泡,得到丁香精油皮克林乳液涂膜保鲜剂。
实施例4:
丁香精油皮克林乳液涂膜保鲜剂的制备方法:
步骤S1、用75%乙醇和玉米醇溶蛋白配置20mg/ml的玉米醇溶蛋白溶液;超纯水和酪蛋白酸钠配置4mg/ml的酪蛋白酸钠溶液,磁力搅拌12h。
步骤S2、将1ml的20mg/ml玉米醇溶蛋白溶液逐滴滴入10ml的4mg/ml的酪蛋白酸钠溶液中,在500rpm磁力搅拌30min。
步骤S3、再使用旋转蒸发仪在40℃蒸发掉溶液中的乙醇,蒸发掉的乙醇用超纯水替代,使溶液体积不变。
步骤S4、然后加入1%v/v丁香精油,15000rpm均质3min,得到丁香精油皮克林乳液。
步骤S5、1%v/v乙酸和壳聚糖配置1.5%w/v壳聚糖溶液,在壳聚糖溶液中加入20%w/w甘油。然后在壳聚糖溶液中加入丁香精油皮克林乳液,使丁香精油在总溶液中浓度为0.6%v/v。15000rpm均质3min,超声30min消泡,得到丁香精油皮克林乳液涂膜保鲜剂。
所用的设备名称和型号:
设备名称1:IKA高速剪切分散机;型号:T18
设备名称2:紫外分光光度计;型号:UV-6000
设备名称3:质构仪;型号:TA-XTplus
设备名称4:恒温恒湿箱;型号:JC-100-SE
设备名称5:冷场扫描电子显微镜;型号:SU8920
设备名称6:傅里叶红外光谱分析仪
设备名称7:无菌均质机;型号:SCIENTZ-09
将步骤S4制备得到的丁香精油皮克林乳液在3500rpm下离心10min以去除任何大颗粒,然后再经10000rpm离心30min。采用无水乙醇稀释上清液,采用UV-6000紫外可见分光光度计在280nm的波长处测定丁香精油的吸光度。对照丁香精油的标准曲线(y=0.0129x-0.0157,R2=0.9992),计算皮克林乳液对丁香精油的包埋率。实验结果得到玉米醇溶蛋白-酪蛋白酸钠纳米颗粒乳化包埋丁香精油,减少丁香精油的挥发损失,对丁香精油的包埋率达62.91%。
将步骤S5制备的样品做设备3质构仪的拉伸测试,测膜的抗张强度和断裂伸长率。如图2所示,为不同添加量丁香精油皮克林乳液涂膜保鲜剂的机械强度图,得到与纯壳聚糖涂膜(对照租)--实施例1相比,添加了丁香精油皮克林乳液的壳聚糖复合膜(从左到右依次为0.2%--实施例2、0.4%--实施例3、0.6%--实施例4)的抗张强度从26.15MPa提升至38.67MPa,断裂伸长率从1%提升至1.56%。
在液氮里将膜弄碎,粘在导电胶上,喷金,通过扫描电镜观察膜的表面和横截面。如图3所示,为不同添加量丁香精油皮克林乳液涂膜保鲜剂的扫描电镜图,A1-D1依次为实施例1、实施例2、实施例3、实施例4的表面,A2-D2依次为实施例1、实施例2、实施例3、实施例4的横截面。通过电镜图观察到,丁香精油皮克林乳液嵌入壳聚糖网络状结构中,有圆形凸起在表面。
通过傅里叶红外光谱分析仪测试丁香精油皮克林乳液涂膜内部分子结构变化。如图4所示,为不同添加量丁香精油皮克林乳液涂膜保鲜剂的傅里叶红外光谱图,丁香精油皮克林乳液的添加使壳聚糖膜在3200cm-1处的吸收峰发生红移,这意味着丁香精油皮克林乳液已经与壳聚糖紧密结合。
根据制片扩散法,以革兰氏阴性菌—大肠杆菌和革兰氏阳性菌—金黄色葡萄球菌为受试菌,测试丁香精油皮克林乳液涂膜保鲜剂对这两种食源性致病菌的抑菌性。将100μL培养的106cfu/g的受试菌注射到LB平板中,涂布均匀。待平板略微干燥后,将6mm无菌空白药敏纸片浸泡在丁香精油皮克林乳液涂膜保鲜剂溶液中,均匀贴在涂有受试菌的平板。将平板放置在37℃恒温培养箱24-48h。通过游标卡尺,测量抑菌圈的直径。如图5所示,为为不同添加量丁香精油皮克林乳液涂膜保鲜剂的对大肠杆菌(E.coli)和金黄色葡萄球菌(S.aureus)的抑菌圈直径图,对大肠杆菌和金黄色葡萄球菌均表现出强抑菌性,0.4%组的丁香精油皮克林乳液涂膜保鲜剂对大肠杆菌的抑菌圈直径达3.29mm,对金黄色葡萄球菌抑菌圈直径达6.15mm。
丁香精油皮克林乳液涂膜保鲜剂保鲜烧鸡的方法,选取宿州徽香源工厂里卤制好的符离集烧鸡,将符离集烧鸡倒挂在图6所示的固定传送带上。通过传送带将烧鸡移至保鲜液浸泡池上方,竖直驱动机构的升降端外伸以使鲜烧鸡整体浸泡到0℃~4℃的保鲜液中,浸泡20-60s。然后竖直驱动机构的升降端回缩以将鲜烧鸡从保鲜液浸泡池中提出,在4℃冷藏室沥干处理,装入保鲜袋中4℃冷藏。
如图7所示,为对照组和实施例3成品展示图。A0:贮藏第0天未涂膜烧鸡,A6:贮藏第6天未涂膜烧鸡,B0:贮藏第0天涂膜烧鸡,B6:贮藏第6天涂膜烧鸡成品展示图。本发明采用丁香精油乳液涂膜对符离集鲜烧鸡进行保鲜贮藏,在没有大面积接触烧鸡的基础上,安全无毒、无二次污染、绿色环保,既保持了烧鸡原有品质,又显著延长了烧鸡的货架期。
解决了符离集鲜烧鸡的保鲜问题。通过GB4789.2-2016食品微生物菌落总数的测定。实施3制备的成品,8天内每2天取一次样品。在无菌工作台内取10g肉样,加入90mL生理盐水,通过设备1无菌均质机拍打2min均质。通过10倍系列稀释,取100μL涂在PCA平板上,涂布均匀。然后倒置在37℃恒温培养箱内培养24-48h。如图8所示,为符离集烧鸡贮藏期间菌落总数图。市场上售卖的符离集鲜烧鸡只能贮藏到第2天,细菌总数达4.7log cfu/g,即将超过国标5log cfu/g的要求;丁香精油乳液涂膜后的符离集鲜烧鸡可贮藏到第4-5天,第6天细菌总数达5.71log cfu/g。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者终端设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者终端设备所固有的要素。在没有更多限制的情况下,由语句“包括……”或“包含……”限定的要素,并不排除在包括所述要素的过程、方法、物品或者终端设备中还存在另外的要素。此外,在本文中,“大于”、“小于”、“超过”等理解为不包括本数;“以上”、“以下”、“以内”等理解为包括本数。
尽管已经对上述各实施例进行了描述,但本领域内的技术人员一旦得知了基本创造性概念,则可对这些实施例做出另外的变更和修改,所以以上所述仅为本发明的实施例,并非因此限制本发明的专利保护范围,凡是利用本发明说明书及附图内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围之内。
Claims (8)
1.一种丁香精油皮克林乳液涂膜保鲜剂的制备方法,其特征在于,包括以下步骤,
步骤S1、用乙醇和玉米醇溶蛋白粉末配置20mg/ml的玉米醇溶蛋白溶液,超纯水和酪蛋白酸钠配置0.4-6mg/ml的酪蛋白酸钠溶液,磁力搅拌6-12h;
步骤S2、将的20mg/ml玉米醇溶蛋白溶液逐滴滴入的0.4-6mg/ml的酪蛋白酸钠溶液中,在500rpm磁力搅拌30min;
步骤S3、再使用旋转蒸发仪在40℃蒸发掉溶液中的乙醇,蒸发掉的乙醇用超纯水替代,使溶液体积不变;
步骤S4、然后加入丁香精油,高速均质3min,得到丁香精油皮克林乳液;
步骤S5、1%v/v乙酸和壳聚糖配置1.5%-2%w/v壳聚糖溶液,在壳聚糖溶液中加入20%w/w甘油,然后在壳聚糖溶液中加入丁香精油皮克林乳液,
使丁香精油在总溶液中浓度为0.2%-0.6%v/v;高速均质3min,超声30min消泡,得到丁香精油皮克林乳液涂膜保鲜剂。
2.如权利要求1所述的丁香精油皮克林乳液涂膜保鲜剂的制备方法,其特征在于,所述乙醇的浓度为70%-80%。
3.如权利要求1所述的丁香精油皮克林乳液涂膜保鲜剂的制备方法,其特征在于,所述步骤S2中玉米醇溶蛋白溶液与酪蛋白酸钠溶液的比例为1:10。
4.如权利要求1所述的丁香精油皮克林乳液涂膜保鲜剂的制备方法,其特征在于,所述步骤S4中丁香精油浓度为0.5%-2%v/v。
5.如权利要求1所述的丁香精油皮克林乳液涂膜保鲜剂的制备方法,其特征在于,所述步骤S4和S5中高速均质的速度为15000-20000rpm。
6.由权利要求1-5中任意一项所述的方法制备得到的丁香精油皮克林乳液涂膜保鲜剂。
7.由权利要求6所述的丁香精油皮克林乳液涂膜保鲜剂作为食品保鲜剂的应用。
8.采用权利要求6所述的丁香精油皮克林乳液涂膜保鲜剂保鲜烧鸡的方法,其特征在于:包括如下步骤,
步骤S1、将鲜烧鸡浸泡到0℃~4℃的丁香精油皮克林乳液涂膜保鲜剂中,浸泡20-60s;
步骤S2、鲜烧鸡从丁香精油皮克林乳液涂膜保鲜剂浸泡池中提出,在4℃冷藏室沥干处理,装入保鲜袋中4℃冷藏。
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