CN115558136B - 一种抗氧化抑菌的红麻果胶可食用膜及其制备方法 - Google Patents
一种抗氧化抑菌的红麻果胶可食用膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种抗氧化抑菌的红麻果胶可食用膜及其制备方法。抗氧化抑菌的红麻果胶可食用膜是以红麻果胶和绿原酸进行包合,再复合甘油和氯化钙制备而成。本发明先采用超声萃取仪对红麻进行处理,改变红麻果胶的化学结构,获得抗氧化活性增强的红麻果胶;再利用具有良好抑菌活性的绿原酸与红麻果胶自组装包合,得到兼具抗氧化和抑菌功能的包合物,最后通过与甘油和氯化钙进行复合,提高膜的机械性能,制备出具有抗氧化抑菌功能的红麻果胶可食用膜。本发明制得的可食用膜制备方法简单,具有抗氧化、抑菌、可生物降解等特点,有较好的膜性能,可应用于食品的包装及保鲜。
Description
技术领域
本发明涉及食用膜技术领域,具体为一种抗氧化抑菌的红麻果胶可食用膜及其制备方法。
背景技术
目前,商业化果胶主要提取自柑橘皮和苹果渣,但这两种原料的供应远不能满足市场对提取果胶用量的需求。因此亟待开发新的果胶提取原料。红麻是一种传统纤维作物,其茎秆韧皮富含纤维素,可加工成红麻纤维。除纤维素外,红麻茎秆韧皮中还含有较多的果胶成分,其在食品工业和医用材料领域深具应用前景。但红麻中的果胶通常在生产纤维的脱胶过程被去除,没有得到开发利用,造成了资源浪费。如果能对红麻果胶进行深度开发,用于生产可食用膜,将会产生显著的经济效益和生态效益。
单一果胶成分制备的膜通常在膜性能方面有所不足,如机械性能欠佳,抑菌活性不强等,如能在果胶中加入具有改善膜性能的成分,开发出的高性能果胶可食用膜将具有更高的应用价值。绿原酸是金银花的主要药效成分,具有抗菌抗病毒等功效,其在食品工业天然抗菌剂方面也日益得到应用。甘油是一种可食用的增塑剂,可用于改善膜的机械性能。氯化钙中的钙离子可通过与果胶形成“蛋-盒”结构,促进果胶形成凝胶。
发明内容
本发明的目的在于提供一种抗氧化抑菌的红麻果胶可食用膜,用红麻果胶和绿原酸包合,再复合甘油制备而成。
本发明还提供了一种抗氧化抑菌的红麻果胶可食用膜的制备方法,包括如下步骤:
(1)将干燥的红麻韧皮用闸刀闸成段并用粉碎机粉碎得到红麻粉,用定性滤纸包好红麻粉,放入索氏提取瓶中,按质量体积比加入8~12倍量的95%乙醇,回流脱脂2~5h,抽提结束后,在通风橱中风干后得脱脂红麻粉;
(2)将步骤(1)获得的脱脂红麻粉放入提取瓶,按质量体积比加入10~15倍量浓度为3~8g/L的草酸铵水溶液,置于超声萃取仪中于300~600W功率下、90℃水浴中提取2~4h,冷却至室温后,离心,取上清液;
(3)将步骤(2)获得的上清液用稀盐酸调节pH值为3~5,于旋转蒸发仪中45℃~65℃下浓缩,浓缩液置于流水中降温冷却,在不断搅拌下向浓缩后的提取液中加入2~4倍量预冷的95%无水乙醇,静置12~18h,过滤,得沉淀;
(4)将步骤(3)所得沉淀用75%~95%乙醇洗涤2~4次,沉淀物置于玻璃皿中,于45℃~65℃烘至干燥,得到红麻果胶;
(5)将(4)所述红麻果胶和绿原酸混合,得到绿原酸的质量含量为1%~10%的混合物,加入去离子水,40℃~60℃下搅拌30~60分钟,得到红麻果胶-绿原酸包合物,所述混合物与去离子水的质量体积比为1:(20~50);
(6)向步骤(5)所述的包合物中加入甘油,60℃~80℃搅拌30~60分钟,得到稳定均匀的成膜液,超声脱气15~35分钟,静置2h,将成膜液均匀平铺在玻璃板上,置于烘箱中于30~60℃下干燥4~12小时,揭膜,在常温常压下放置24~48小时,获得果胶膜,所述的包合物和甘油的质量比为50:(1~3);
(7)将步骤(6)制得的果胶膜浸入浓度为2~5%的CaCl2溶液中20~40min,用去离子水清洗3次,于35℃~45℃干燥20~30h,即得一种抗氧化抑菌的红麻果胶可食用膜。
优选的,所述步骤(1)为:将干燥的红麻韧皮用闸刀闸成段并用粉碎机粉碎得到红麻粉,用定性滤纸包好红麻粉,放入索氏提取瓶中,按质量体积比加入10倍量的95%乙醇,回流脱脂3h,抽提结束后,在通风橱中风干脱脂后得红麻粉。
优选的,所述步骤(2)为:将步骤(1)获得的脱脂红麻粉放入提取瓶,按质量体积比加入12倍量浓度为4g/L的草酸铵水溶液,置于超声萃取仪中于450W功率下、90℃水浴中提取3h,冷却至室温后,离心,取上清液。
优选的,所述步骤(3)为:获得的上清液用稀盐酸调节pH值为4,于旋转蒸发仪中55℃下浓缩,浓缩液置于流水中降温冷却,在不断搅拌下向浓缩后的提取液中加入3倍量预冷的95%无水乙醇,静置14h,过滤,得沉淀。
优选的,所述步骤(4)为:将步骤(3)所得沉淀用95%乙醇洗涤3次,沉淀物置于玻璃皿中,于55℃烘至干燥,得到红麻果胶。
优选的,所述步骤(5)为:将(4)所述红麻果胶和绿原酸混合,得到绿原酸的质量含量为4%的混合物,加入去离子水,50℃下搅拌40分钟,得到红麻果胶-绿原酸包合物,所述混合物与去离子水的质量体积比为1:30。
优选的,所述步骤(6)为:向步骤(5)所述的包合物中加入甘油,65℃搅拌40分钟,得到稳定均匀的成膜液,超声脱气25分钟,静置2h,将成膜液均匀平铺在玻璃板上,置于烘箱中于45℃下干燥6小时,揭膜,在常温常压下放置36小时,获得果胶膜,所述的包合物和甘油的质量比为50:2。
优选的,所述步骤(7)为:将步骤(6)所述果胶膜浸入浓度为4%的CaCl2溶液中30min,用去离子水清洗3次,于40℃干燥24h,即得一种抗氧化抑菌的红麻果胶可食用膜。
与现有技术相比,本发明的有益效果是:
1.本发明先采用超声波萃取仪对红麻进行处理,改变红麻果胶的化学结构,获得抗氧化活性增强的红麻果胶可食用膜。
2.本发明利用具有良好抑菌活性的绿原酸与红麻果胶进行自组装包合,得到兼具抗氧化和抑菌功能的包合物,最后通过与甘油和氯化钙进行复合,提高膜的机械性能,制备出具有抗氧化抑菌功能的红麻果胶可食用膜,实现了红麻果胶的高值利用,同时可减少传统塑料保鲜膜使用所致的环境污染。
3.本发明制得的可食用膜制备方法简单,具有抗氧化、抑菌、可生物降解等特点,有利于延长食品货架期,有较好的膜性能,可应用于食品的包装及保鲜。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合具体实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
实施例1
一种抗氧化抑菌的红麻果胶可食用膜及其制备方法,包括如下步骤:
(1)将干燥的红麻韧皮用闸刀闸成段并用粉碎机粉碎得到红麻粉,用定性滤纸包好红麻粉,放入索氏提取瓶中,按质量体积比加入10倍量的95%乙醇,回流脱脂3h。抽提结束后,在通风橱中风干脱脂后得红麻粉。
(2)将步骤(1)获得的脱脂红麻粉放入提取瓶,按质量体积比加入12倍量浓度为4g/L的草酸铵水溶液,置于超声萃取仪中于450W功率下、90℃水浴中提取3h。冷却至室温后,离心,取上清液。
(3)获得的上清液用稀盐酸调节pH值为4,于旋转蒸发仪中55℃下浓缩,浓缩液置于流水中降温冷却。在不断搅拌下向浓缩后的提取液中加入3倍量预冷的95%无水乙醇,静置14h,过滤,得沉淀。
(4)将步骤(3)所得沉淀用95%乙醇洗涤3次,沉淀物置于玻璃皿中,于55℃烘至干燥,得到红麻果胶。
(5)将(4)所述红麻果胶和绿原酸混合,得到绿原酸的质量含量为4%的混合物,加入去离子水,50℃下搅拌40分钟,得到红麻果胶-绿原酸包合物。所述混合物与去离子水的质量体积比为1:30。
(6)向步骤(5)所述的包合物中加入甘油,65℃搅拌40分钟,得到稳定均匀的成膜液,超声脱气25分钟,静置2h。将成膜液均匀平铺在玻璃板上,置于烘箱中于45℃下干燥6小时,揭膜,在常温常压下放置36小时,获得果胶膜。所述的包合物和甘油的质量比为50:2。
(7)将步骤(6)制得的果胶膜浸入浓度为4%的CaCl2溶液中30min,用去离子水清洗3次,于40℃干燥24h,即得一种抗氧化抑菌的红麻果胶可食用膜。
实施例2
一种抗氧化抑菌的红麻果胶可食用膜及其制备方法,包括如下步骤:
(1)将干燥的红麻韧皮用闸刀闸成段并用粉碎机粉碎得到红麻粉,用定性滤纸包好红麻粉,放入索氏提取瓶中,按质量体积比加入8倍量的95%乙醇,回流脱脂4h。抽提结束后,在通风橱中风干脱脂后得红麻粉。
(2)将步骤(1)获得的脱脂红麻粉放入提取瓶,按质量体积比加入10倍量浓度为6g/L的草酸铵水溶液,置于超声萃取仪中于300W功率下、90℃水浴中提取4h。冷却至室温后,离心,取上清液。
(3)获得的上清液用稀盐酸调节pH值为3.5,于旋转蒸发仪中50℃下浓缩,浓缩液置于流水中降温冷却。在不断搅拌下向浓缩后的提取液中加入2倍量预冷的95%无水乙醇,静置18h,过滤,得沉淀。
(4)将步骤(3)所得沉淀用75%乙醇洗涤4次,沉淀物置于玻璃皿中,于45℃烘至干燥,得到红麻果胶。
(5)将(4)所述红麻果胶和绿原酸混合,得到绿原酸的质量含量为2%的混合物,加入去离子水,40℃下搅拌60分钟,得到红麻果胶-绿原酸包合物。所述混合物与去离子水的质量体积比为1:20。
(6)向步骤(5)所述的包合物中加入甘油,60℃搅拌50分钟,得到稳定均匀的成膜液,超声脱气35分钟,静置2h。将成膜液均匀平铺在玻璃板上,置于烘箱中于35℃下干燥10小时,揭膜,在常温常压下放置48小时,获得果胶膜。所述的包合物和甘油的质量比为50:1。
(7)将步骤(6)制得的果胶膜浸入浓度为2%的CaCl2溶液中40min,用去离子水清洗3次,于45℃干燥20h,即得一种抗氧化抑菌的红麻果胶可食用膜。
实施例3
一种抗氧化抑菌的红麻果胶可食用膜及其制备方法,包括如下步骤:
(1)将干燥的红麻韧皮用闸刀闸成段并用粉碎机粉碎得到红麻粉,用定性滤纸包好红麻粉,放入索氏提取瓶中,按质量体积比加入12倍量的95%乙醇,回流脱脂2h。抽提结束后,在通风橱中风干脱脂后得红麻粉。
(2)将步骤(1)获得的脱脂红麻粉放入提取瓶,按质量体积比加入15倍量浓度为3g/L的草酸铵水溶液,置于超声萃取仪中于600W功率下90℃水浴提取2h。冷却至室温后,离心,取上清液。
(3)获得的上清液用稀盐酸调节pH值为5,于旋转蒸发仪中60℃下浓缩,浓缩液置于流水中降温冷却。在不断搅拌下向浓缩后的提取液中加入4倍量预冷的95%无水乙醇,静置12h,过滤,得沉淀。
(4)将步骤(3)所得沉淀用85%乙醇洗涤3次,沉淀物置于玻璃皿中,于50℃烘至干燥,得到红麻果胶。
(5)将(4)所述红麻果胶和绿原酸混合,得到绿原酸的质量含量为8%的混合物,加入去离子水,50℃下搅拌40分钟,得到红麻果胶-绿原酸包合物。所述混合物与去离子水的质量体积比为1:40。
(6)向步骤(5)所述的包合物中加入甘油,80℃搅拌30分钟,得到稳定均匀的成膜液,超声脱气15分钟,静置2h。将成膜液均匀平铺在玻璃板上,置于烘箱中于60℃下干燥8小时,揭膜,在常温常压下放置24小时,获得果胶膜。所述的包合物和甘油的质量比为50:3。
(7)将步骤(6)制得的果胶膜浸入浓度为5%的CaCl2溶液中20min,用去离子水清洗3次,于35℃干燥30h,即得一种抗氧化抑菌的红麻果胶可食用膜。
实施例4
以清除DPPH自由基实验和清除ABTS自由基实验检测本发明食用膜的抗氧化能力。
在实施例1的基础上省去步骤(2)中的超声波萃取仪,直接90℃水浴提取红麻果胶,制备的可食用膜作为对照组1;在实施例1的基础上省去步骤(5)中绿原酸的添加,制备的可食用膜作为对照组2;在实施例1的基础上省去步骤(6)中甘油的添加,制备的可食用膜作为对照组3。实施例1至3、对照组1至3的抗氧化能力及膜性能检测结果对比见下表1。
表1
由上述实验结果可以看出,与未超声处理的红麻果胶可食用膜(对照组1)相比,实施例1经超声处理后的红麻果胶膜DPPH自由基和ABTS自由基清除能力得到了显著增强,即抗氧化活性得到了显著增强。
实验证明,与未添加甘油的红麻果胶可食用膜(对照组3)相比,实施例1添加了甘油的红麻果胶可食用膜的抗拉强度和断裂延伸率得到了显著增强。实施例2和3制备的膜对DPPH和ABTS自由基的清除能力、抗拉强度以及断裂延伸率与实施例1制备的膜相似。
实施例5
通过测定对大肠杆菌和金黄色葡萄球菌的抑菌圈直径来检测本发明可食用膜的的抑菌活性。实施例1至3、对照组1至3的抑菌圈直径测定结果见表2。
表2
由上述结果可以看出,与对照组2未添加绿原酸的膜相比,实施例1添加了绿原酸的可食用膜对大肠杆菌和金黄色葡萄球菌的抑菌圈直径更大,表明抑菌活性更强。
实施例2和3和抑菌圈直径与实施例1相似,抑菌活性接近。
从以上可以看出,和对照组相比,本发明制得的红麻果胶可食用膜具有更强的抗氧化及抑菌活性,且拉伸强度和断裂延伸率等膜性能更优。
本发明的原料可食用,制备的膜也可以食用。
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 (9)
1.一种抗氧化抑菌的红麻果胶可食用膜,其特征在于:用红麻果胶和绿原酸包合,再复合甘油制备而成;所述红麻果胶由以下步骤制成:
(1)将干燥的红麻韧皮用闸刀闸成段并用粉碎机粉碎得到红麻粉,用定性滤纸包好红麻粉,放入索氏提取瓶中,按质量体积比加入8~12倍量的95%乙醇,回流脱脂2~5h,抽提结束后,在通风橱中风干后得脱脂红麻粉;
(2)将步骤(1)获得的脱脂红麻粉放入提取瓶,按质量体积比加入10~15倍量浓度为3~8g/L的草酸铵水溶液,置于超声萃取仪中于300~600W功率下、90℃水浴中提取2~4h,冷却至室温后,离心,取上清液;
(3)将步骤(2)获得的上清液用稀盐酸调节pH值为3~5,于旋转蒸发仪中45℃~65℃下浓缩,浓缩液置于流水中降温冷却,在不断搅拌下向浓缩后的提取液中加入2~4倍量预冷的95%无水乙醇,静置12~18h,过滤,得沉淀;
(4)将步骤(3)所得沉淀用75%~95%乙醇洗涤2~4次,沉淀物置于玻璃皿中,于45℃~65℃烘至干燥,得到红麻果胶。
2.根据权利要求1所述的一种抗氧化抑菌的红麻果胶可食用膜,其特征在于:所述步骤(1)为:将干燥的红麻韧皮用闸刀闸成段并用粉碎机粉碎得到红麻粉,用定性滤纸包好红麻粉,放入索氏提取瓶中,按质量体积比加入10倍量的95%乙醇,回流脱脂3h,抽提结束后,在通风橱中风干脱脂后得红麻粉。
3.根据权利要求1所述的一种抗氧化抑菌的红麻果胶可食用膜,其特征在于:所述步骤(2)为:将步骤(1)获得的脱脂红麻粉放入提取瓶,按质量体积比加入12倍量浓度为4 g/L的草酸铵水溶液,置于超声萃取仪中于450W功率下、90℃水浴中提取3h,冷却至室温后,离心,取上清液。
4.根据权利要求1所述的一种抗氧化抑菌的红麻果胶可食用膜,其特征在于:所述步骤(3)为:获得的上清液用稀盐酸调节pH值为4,于旋转蒸发仪中55℃下浓缩,浓缩液置于流水中降温冷却,在不断搅拌下向浓缩后的提取液中加入3倍量预冷的95%无水乙醇,静置14h,过滤,得沉淀。
5.根据权利要求1所述的一种抗氧化抑菌的红麻果胶可食用膜,其特征在于:所述步骤(4)为:将步骤(3)所得沉淀用95%乙醇洗涤3次,沉淀物置于玻璃皿中,于55℃烘至干燥,得到红麻果胶。
6.根据权利要求1所述的一种抗氧化抑菌的红麻果胶可食用膜的制备方法,其特征在于:包括如下步骤:
(1)将干燥的红麻韧皮用闸刀闸成段并用粉碎机粉碎得到红麻粉,用定性滤纸包好红麻粉,放入索氏提取瓶中,按质量体积比加入8~12倍量的95%乙醇,回流脱脂2~5h,抽提结束后,在通风橱中风干后得脱脂红麻粉;
(2)将步骤(1)获得的脱脂红麻粉放入提取瓶,按质量体积比加入10~15倍量浓度为3~8g/L的草酸铵水溶液,置于超声萃取仪中于300~600W功率下、90℃水浴中提取2~4h,冷却至室温后,离心,取上清液;
(3)将步骤(2)获得的上清液用稀盐酸调节pH值为3~5,于旋转蒸发仪中45℃~65℃下浓缩,浓缩液置于流水中降温冷却,在不断搅拌下向浓缩后的提取液中加入2~4倍量预冷的95%无水乙醇,静置12~18h,过滤,得沉淀;
(4)将步骤(3)所得沉淀用75%~95%乙醇洗涤2~4次,沉淀物置于玻璃皿中,于45℃~65℃烘至干燥,得到红麻果胶;
(5)将步骤(4)所述红麻果胶和绿原酸混合,得到绿原酸的质量含量为1%~10%的混合物,加入去离子水,40℃~60℃下搅拌30~60分钟,得到红麻果胶-绿原酸包合物,所述混合物与去离子水的质量体积比为1:(20~50);
(6)向步骤(5)所述的包合物中加入甘油,60℃~80℃搅拌30~60分钟,得到稳定均匀的成膜液,超声脱气15~35分钟,静置2h,将成膜液均匀平铺在玻璃板上,置于烘箱中于30~60℃下干燥4~12小时,揭膜,在常温常压下放置24~48小时,获得果胶膜,所述的包合物和甘油的质量比为50:(1~3);
(7)将步骤(6)制得的果胶膜浸入浓度为2~5%的CaCl2溶液中20~40min,用去离子水清洗3次,于35℃~45℃干燥20~30h,即得一种抗氧化抑菌的红麻果胶可食用膜。
7.根据权利要求6所述的一种抗氧化抑菌的红麻果胶可食用膜的制备方法,其特征在于:所述步骤(5)为:将(4)所述红麻果胶和绿原酸混合,得到绿原酸的质量含量为4%的混合物,加入去离子水,50℃下搅拌40分钟,得到红麻果胶-绿原酸包合物,所述混合物与去离子水的质量体积比为1:30。
8.根据权利要求6所述的一种抗氧化抑菌的红麻果胶可食用膜的制备方法,其特征在于:所述步骤(6)为:向步骤(5)所述的包合物中加入甘油,65℃搅拌40分钟,得到稳定均匀的成膜液,超声脱气25分钟,静置2h,将成膜液均匀平铺在玻璃板上,置于烘箱中于45℃下干燥6小时,揭膜,在常温常压下放置36小时,获得果胶膜,所述的包合物和甘油的质量比为50:2。
9.根据权利要求6所述的一种抗氧化抑菌的红麻果胶可食用膜的制备方法,其特征在于:所述步骤(7)为:将步骤(6)所述果胶膜浸入浓度为4%的CaCl2溶液中30min,用去离子水清洗3次,于40℃干燥24h,即得一种抗氧化抑菌的红麻果胶可食用膜。
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