CN112425711A - 一种橡子壳提取物涂膜保鲜剂及其制备方法 - Google Patents
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Abstract
一种橡子壳提取物涂膜保鲜剂及其制备方法,它涉及涂膜保鲜剂及其制备方法。本发明的目是提供一种橡子壳提取物涂膜保鲜剂及其制备方法。本发明的橡子壳提取物涂膜保鲜剂是由橡子壳提取物、橡实淀粉酯、壳聚糖、海藻酸钠、单甘酯和水制成的。制法:将橡实淀粉酯、壳聚糖、海藻酸钠、单甘酯加入到部分水中,得到混合液;再将橡子壳提取物加入到剩余的水中,混合均匀后倒入混合液中,再进行高速剪切处理,得到橡子壳提取物涂膜保鲜剂。它对大肠杆菌、金黄色葡萄球菌和的沙门氏菌的抑菌圈直径分别达到12~14mm、12~13mm、15~17mm,抑菌效果良好,可用于食品保鲜领域。
Description
技术领域
本发明涉及涂膜保鲜剂的制备方法。
背景技术
食品保鲜剂是指用于防止食品在储存、流通过程中,由于微生物繁殖引起的变质,或由于储存销售条件不当,食品内在品质发生劣变、色泽下降,为提高保存期,延长食用价值而在食品中使用的食品添加剂。现阶段主要采用化学合成物质和天然物质作为食品保鲜剂。化学合成保鲜剂主要分为吸附型防腐保鲜剂、溶液浸泡型防腐保鲜剂、熏蒸型防腐剂等几类,这类防腐保鲜剂发展迅速,应用较多,但是由于人工合成的保鲜剂存在毒性残留的问题。天然保鲜剂主要指植物源保鲜剂,来源广泛,安全无毒且实用性强,可从果蔬、中草药、香辛料等多种植物中收集,并且很多成分都具有明显防腐保鲜功能,现阶段已广泛应用于果蔬保鲜研究中。在人们长期食用的食品中,天然保鲜剂成分的毒性远远低于人工合成的保鲜剂。因此,从自然界寻求天然保鲜剂的研究已引起各国科学家的高度重视。
发明内容
本发明的目是提供一种橡子壳提取物涂膜保鲜剂及其制备方法。
本发明的橡子壳提取物涂膜保鲜剂按质量份数由5~8份橡子壳提取物、30~35份橡实淀粉酯、5~8份壳聚糖、6~10份的海藻酸钠、2~3份的单甘酯和1000份蒸馏水制成的。
上述的橡子壳提取物涂膜保鲜剂的制备方法,按以下步骤进行:
一、按质量份数称取5~8份橡子壳提取物、30~35份橡实淀粉酯、5~8份壳聚糖、6~10份的海藻酸钠、2~3份的单甘酯和1000份蒸馏水;
二、将称取的橡实淀粉酯、壳聚糖、海藻酸钠、单甘酯加入到四分之三的蒸馏水中,搅拌并加热到70~75℃使其完全溶解,得到混合液;
三、将称取的橡子壳提取物加入到剩余的蒸馏水中,混合均匀,再将其倒入混合液中,用高剪切乳化机进行高速剪切处理,得到橡子壳提取物涂膜保鲜剂。
更进一步地,橡子壳提取物的制备方法如下:
(1)将橡子壳在50~60℃下烘干后,粉碎,过80目筛,得到橡子壳粉;
(2)将橡子壳粉加入到萃取瓶中,以料液比1:(18~20)添加质量百分浓度为40%~80%的乙醇溶液作为提取溶剂,在55~60℃的条件下超声波提取2~2.5h;将混合液以4000~5000r/min转速离心分离10~15min,收集上清液;橡子壳残渣再复提2次,合并三次上清液;
(3)将上清液在40~50℃的条件下真空旋转浓缩,浓缩液再放在-18~-20℃的条件下下预冷冻,最后真空冷冻干燥,得到橡子壳提取物。
更进一步地,橡实淀粉酯的制备方法如下:
(1)称取橡实淀粉、辛酸、异丙醇、吐温-80;其中辛酸与异丙醇的体积比为1:(5~6);吐温-80的质量为辛酸的质量的2%~3%;辛酸与异丙醇的质量之和为橡实淀粉质量的25%~30%;
(2)按橡实淀粉的质量百分浓度为30%~35%将橡实淀粉分散在蒸馏水中,再用0.1M NaOH溶液调节pH值在8.2~8.6,得到橡实淀粉悬浮液;
(3)将辛酸和异丙醇混合,得到异丙醇辛酸溶液;
(4)称将橡实淀粉悬浮液加入到高速剪切均质机中,在高速剪切均质条件下,将异丙醇辛酸溶液和吐温-80加入到橡实淀粉悬浮液中,异丙醇辛酸溶液和吐温-80在2小时内加入完成;然后在温度为30~35℃的条件下酯化反应5~6h,再用1M HCl溶液将pH调至7.0,得到混合物;
(5)将混合物离心处理,固相物依次用蒸馏水和无水乙醇洗,放入烘箱中在温度为40~45℃的条件下干燥18~30小时,研磨并通过100目筛,得到橡实淀粉酯。
更进一步地,步骤(5)中混合物离心处理的转速为4000~5000r/min,离心处理时间为15~20min;
更进一步地,步骤三中所述的高速剪切处理是在在14000~16000r/min的条件下进行高速剪切10~15min。
本发明的橡子壳提取物涂膜保鲜剂的使用方法是通过将橡子壳提取物涂膜保鲜剂喷洒在产品上在其表面瞬间形成保鲜膜层的方式进行保鲜抑菌。橡子壳提取物中含有儿茶酚、花黄素、花色素连有糖基的化合物等多种活性成分,是一种优良的天然食品保鲜剂。不仅安全性高,而且色调柔和,具有一定的生理活性。橡实淀粉酯是利用中短链脂肪酸辛酸和橡实淀粉进行酯化反应制备的,橡实淀粉酯即具有中链碳链的亲油性,又具有橡实淀粉羟基的亲水性,使得改良后的液膜对食源性细菌细胞膜的吸附性的增强,大大提高橡子壳提取物中的有效抑菌成分对细菌的作用。同时也使液膜在肉制品上的吸附力与稳定性增强,延缓产品的脱水速率,保证产品的品质。
本发明橡子壳提取物涂膜保鲜剂通过充分发挥橡子壳中多酚和黄酮等天然物质对食源性微生物的抑菌效果。在涂膜保鲜剂配方中首次采用了橡实淀粉酯作为乳化剂,提高保鲜剂的对细菌的靶向性和在产品表面的粘附性,同时采用高速剪切技术进行处理和加工,不仅改善了橡子壳提取物涂膜保鲜剂抑菌效果,而且在产品表面形成稳定的抑菌膜,延缓了产品的脱水速率,保证了产品的品质,是一种高效绿色环保的涂膜保鲜剂。
本发明的橡子壳提取物涂膜保鲜剂对大肠杆菌的抑菌圈直径是12~14mm,金黄色葡萄球菌的抑菌圈直径为12~13mm,对于沙门氏菌的抑菌圈直径为15~17mm。抑菌效果较好。本发明的橡子壳提取物涂膜保鲜剂可用于食品保鲜领域。
具体实施方式
用下面的实施例验证本发明的有益效果。
实施例1:本实施例的橡子壳提取物涂膜保鲜剂的制备方法,按以下步骤进行:
一、称取5g橡子壳提取物、30g橡实淀粉酯、5g壳聚糖、6g的海藻酸钠、2g的单甘酯和1000mL蒸馏水;
二、将称取的橡实淀粉酯、壳聚糖、海藻酸钠、单甘酯加入到750mL的蒸馏水中,搅拌并加热到75℃使其完全溶解,得到混合液;
三、将称取的橡子壳提取物加入到剩余的250mL蒸馏水中,混合均匀,再将其倒入混合液中,用高剪切乳化机在15000r/min的条件下进行高速剪切10min,得到橡子壳提取物涂膜保鲜剂。
其中橡子壳提取物的制备方法如下:
(1)将橡子壳在60℃下烘干后,粉碎,过80目筛,得到橡子壳粉;
(2)将橡子壳粉加入到萃取瓶中,以料液比1:20添加质量百分浓度为60%的乙醇溶液作为提取溶剂,在60℃的条件下超声波提取2h;将混合液以4000r/min转速离心分离10min,收集上清液;橡子壳残渣再复提取2次,合并三次上清液;
(3)将上清液在40℃的条件下真空旋转浓缩至体积减少到原来的五分之一,浓缩液再放在-18℃的条件下下预冷冻,最后真空冷冻干燥,得到橡子壳提取物。
其中橡实淀粉酯的制备方法如下:
(1)称取30g橡实淀粉、1.25g辛酸、6.25g异丙醇、25mg吐温-80;其中辛酸与异丙醇的体积比为1:5;吐温-80的质量为辛酸的质量的2%;辛酸与异丙醇的质量之和为橡实淀粉质量的25%;
(2)按橡实淀粉的质量百分浓度为30%将橡实淀粉分散在蒸馏水中,再用0.1MNaOH溶液调节pH值在8.5,得到橡实淀粉悬浮液;
(3)将辛酸和异丙醇混合,得到异丙醇辛酸溶液;
(4)称将橡实淀粉悬浮液加入到高速剪切均质机中,在高速剪切均质条件下,将异丙醇辛酸溶液和吐温-80加入到橡实淀粉悬浮液中,异丙醇辛酸溶液和吐温-80在2小时内加入完成;然后在温度为35℃的条件下酯化反应5h,再用1M HCl溶液将pH调至7.0,得到混合物;
(5)将混合物在4000r/min的条件下离心处理15分钟,固相物先用无水乙醇洗涤两次,再用蒸馏水洗涤三次,放入烘箱中在温度为45℃的条件下干燥24小时,研磨并通过100目筛,得到橡实淀粉酯。
对比实施例1:本对比实施例为不加橡实淀粉酯的保鲜液,该保鲜液制备方法如下:
一、准确称取5g橡子壳提取物、5g壳聚糖、6g海藻酸钠、2g单甘酯和蒸馏水至1000mL;其中橡子壳提取物与实施例1中的相同。
二、将壳聚糖、海藻酸钠和单甘酯加入至750mL蒸馏水中,搅拌加热到75℃使其完全溶解,得到混合液;
三、将称取的橡子壳提取物,溶解到剩余的250mL蒸馏水中,将其缓慢倒入混合液中;用高剪切乳化机在15000r/min的条件下进行高速剪切10min,得到作为对比的不加橡实淀粉酯的保鲜剂。
对比实施例2:本对比实施例为制备橡实淀粉酯时不加吐温-80的保鲜液,该保鲜液制备方法如下:
先制备橡实淀粉酯,具体的方法如下:
(1)称取30g橡实淀粉、1.25g辛酸、6.25g异丙醇;
(2)按橡实淀粉的质量百分浓度为30%将橡实淀粉分散在蒸馏水中,再用0.1MNaOH溶液调节pH值在8.5,得到橡实淀粉悬浮液;
(3)将辛酸和异丙醇混合,得到异丙醇辛酸溶液;
(4)称将橡实淀粉悬浮液加入到高速剪切均质机中,在高速剪切均质条件下,将异丙醇辛酸溶液加入到橡实淀粉悬浮液中,异丙醇辛酸溶液在2小时内加入完成;然后在温度为35℃的条件下酯化反应5h,再用1M HCl溶液将pH调至7.0,得到混合物;
(5)将混合物在4000r/min的条件下离心处理15分钟,固相物先用无水乙醇洗涤两次,再用蒸馏水洗涤三次,放入烘箱中在温度为45℃的条件下干燥24小时,研磨并通过100目筛,得到作为对比的橡实淀粉酯;
利用该作为对比的橡实淀粉酯,制备保鲜液,具体的方法如下:
一、称取5g橡子壳提取物、30g作为对比的橡实淀粉酯、5g壳聚糖、6g的海藻酸钠、2g的单甘酯和1000mL蒸馏水;
二、将称取的作为对比的橡实淀粉酯、壳聚糖、海藻酸钠、单甘酯加入到750mL的蒸馏水中,搅拌并加热到75℃使其完全溶解,得到混合液;
三、将称取的橡子壳提取物加入到剩余的250mL蒸馏水中,混合均匀,再将其倒入混合液中,用高剪切乳化机在15000r/min的条件下进行高速剪切10min,得到作为对比的不加吐温-80的橡子壳提取物涂膜保鲜剂。
将实施例1制备的橡子壳提取物涂膜保鲜剂、对比实施例1制备的作为对比的不加橡实淀粉酯的保鲜剂、对比实施例2制备的作为对比的不加吐温-80的橡子壳提取物涂膜保鲜剂和0.5%的橡子壳提取物溶液同时进行抑菌试验,得到的结果如表1所示。
表1抑菌试验结果
通过表1的对比可知,本实施例1的橡子壳提取物涂膜保鲜剂对大肠杆菌的抑菌圈直径是0.5%的橡子壳提取物溶液的2.5倍,对金黄色葡萄球菌的抑菌圈直径是0.5%的橡子壳提取物溶液的2.8倍,对沙门氏菌的抑菌圈直径是0.5%的橡子壳提取物溶液的3.09倍。通过与对比实施例1的对比可知,采用橡实淀粉酯作为乳化剂,可以提高保鲜剂中的活性成分对细菌的靶向性和在产品表面的粘附性,在产品表面形成稳定的抑菌膜,同时提高了橡子壳提取物的抑菌效果。通过与对比实施例2的对比可知,在制备橡实淀粉酯时加入吐温-80也对提高保鲜剂的抑菌效果起了重要的作用,在制备橡实淀粉酯时加入吐温-8,吐温-80是一种有效的表面活性剂,分析表明在橡实淀粉酯制备过程中吐温-80有效增加了橡实淀粉与辛酸酯化反应效率,提高了酯化度,进而提高了橡实淀粉酯的乳化性能和黏附性能,最终有益于橡子壳提取物涂膜保鲜剂成膜性和对菌体的粘附性,提高了抑菌效果。
实施例2:本实施例的橡子壳提取物涂膜保鲜剂的制备方法,按以下步骤进行:
一、称取8g橡子壳提取物、35g橡实淀粉酯、6g壳聚糖、8g的海藻酸钠、3g的单甘酯和1000mL蒸馏水;
二、将称取的橡实淀粉酯、壳聚糖、海藻酸钠、单甘酯加入到750mL的蒸馏水中,搅拌并加热到75℃使其完全溶解,得到混合液;
三、将称取的橡子壳提取物加入到剩余的250mL蒸馏水中,混合均匀,再将其倒入混合液中,用高剪切乳化机在14000r/min的条件下进行高速剪切15min,得到橡子壳提取物涂膜保鲜剂。
其中橡子壳提取物的制备方法如下:
(1)将橡子壳在60℃下烘干后,粉碎,过80目筛,得到橡子壳粉;
(2)将橡子壳粉加入到萃取瓶中,以料液比1:25添加质量百分浓度为80%的乙醇溶液作为提取溶剂,在60℃的条件下超声波提取2h;将混合液以4000r/min转速离心分离10min,收集上清液;橡子壳残渣再重复提取2次,合并三次上清液;
(3)将上清液在40℃的条件下真空旋转浓缩至体积减少到原来的五分之一,浓缩液再放在-18℃的条件下下预冷冻,最后真空冷冻干燥,得到橡子壳提取物。
其中橡实淀粉酯的制备方法如下:
(1)称取30g橡实淀粉、1.5g辛酸、7.5g异丙醇、45mg吐温-80;其中辛酸与异丙醇的体积比为1:5;吐温-80的质量为辛酸的质量的3%;辛酸与异丙醇的质量之和为橡实淀粉质量的30%;
(2)按橡实淀粉的质量百分浓度为30%将橡实淀粉分散在蒸馏水中,再用0.1MNaOH溶液调节pH值在8.5,得到橡实淀粉悬浮液;
(3)将辛酸和异丙醇混合,得到异丙醇辛酸溶液;
(4)称将橡实淀粉悬浮液加入到高速剪切均质机中,在高速剪切均质条件下,将异丙醇辛酸溶液和吐温-80加入到橡实淀粉悬浮液中,异丙醇辛酸溶液和吐温-80在2小时内加入完成;然后在温度为35℃的条件下酯化反应5h,再用1M HCl溶液将pH调至7.0,得到混合物;
(5)将混合物在4000r/min的条件下离心处理15分钟,固相物先用无水乙醇洗涤两次,再用蒸馏水洗涤三次,放入烘箱中在温度为45℃的条件下干燥24小时,研磨并通过100目筛,得到橡实淀粉酯。
本实施例2的橡子壳提取物涂膜保鲜剂对大肠杆菌的抑菌圈直径是13.94±0.29mm,金黄色葡萄球菌的抑菌圈直径为12.76±0.24mm,对于沙门氏菌的抑菌圈直径为16.83±0.42mm。抑菌效果较好。
Claims (6)
1.一种橡子壳提取物涂膜保鲜剂,其特征在于该涂膜保鲜剂是按质量份数由5~8份橡子壳提取物、30~35份橡实淀粉酯、5~8份壳聚糖、6~10份的海藻酸钠、2~3份的单甘酯和1000份蒸馏水制成的。
2.制备权利要求1所述的一种橡子壳提取物涂膜保鲜剂的方法,其特征在于该方法按以下步骤进行:
一、按质量份数称取5~8份橡子壳提取物、30~35份橡实淀粉酯、5~8份壳聚糖、6~10份的海藻酸钠、2~3份的单甘酯和1000份蒸馏水;
二、将称取的橡实淀粉酯、壳聚糖、海藻酸钠、单甘酯加入到四分之三的蒸馏水中,搅拌并加热到70~75℃使其完全溶解,得到混合液;
三、将称取的橡子壳提取物加入到剩余的蒸馏水中,混合均匀,再将其倒入混合液中,用高剪切乳化机高速剪切处理,得到橡子壳提取物涂膜保鲜剂。
3.根据权利要求2所述的一种橡子壳提取物涂膜保鲜剂的制备方法,其特征在于步骤一中所述的橡子壳提取物的制备方法如下:
(1)将橡子壳在50~60℃下烘干后,粉碎,过80目筛,得到橡子壳粉;
(2)将橡子壳粉加入到萃取瓶中,以料液比1:(18~20)添加质量百分浓度为40%~80%的乙醇溶液作为提取溶剂,在55~60℃的条件下超声波提取2~2.5h;将混合液以4000~5000r/min转速离心分离10~15min,收集上清液;橡子壳残渣再复提2次,合并三次上清液;
(3)将上清液在40~50℃的条件下真空旋转浓缩,浓缩液再放在-18~-20℃的条件下下预冷冻,最后真空冷冻干燥,得到橡子壳提取物。
4.根据权利要求2或3所述的一种橡子壳提取物涂膜保鲜剂的制备方法,其特征在于步骤一中所述的橡实淀粉酯的制备方法如下:
(1)称取橡实淀粉、辛酸、异丙醇、吐温-80;其中辛酸与异丙醇的体积比为1:(5~6);吐温-80的质量为辛酸的质量的2%~3%;辛酸与异丙醇的质量之和为橡实淀粉质量的25%~30%;
(2)按橡实淀粉的质量百分浓度为30%~35%将橡实淀粉分散在蒸馏水中,再用0.1MNaOH溶液调节pH值在8.2~8.6,得到橡实淀粉悬浮液;
(3)将辛酸和异丙醇混合,得到异丙醇辛酸溶液;
(4)称将橡实淀粉悬浮液加入到高速剪切均质机中,在高速剪切均质条件下,将异丙醇辛酸溶液和吐温-80加入到橡实淀粉悬浮液中,异丙醇辛酸溶液和吐温-80在2小时内加入完成;然后在温度为30~35℃的条件下酯化反应5~6h,再用1M HCl溶液将pH调至7.0,得到混合物;
(5)将混合物离心处理,固相物依次用蒸馏水和无水乙醇洗,放入烘箱中在温度为40~45℃的条件下干燥18~30小时,研磨并通过100目筛,得到橡实淀粉酯。
5.根据权利要求4所述的一种橡子壳提取物涂膜保鲜剂的制备方法,其特征在于步骤(5)中混合物离心处理的转速为4000~5000r/min,离心处理时间为15~20min。
6.根据权利要求2所述的一种橡子壳提取物涂膜保鲜剂的制备方法,其特征在于步骤三中所述的高速剪切处理是在在14000~16000r/min的条件下进行高速剪切10~15min。
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