CN117343337B - 一种包载辣椒素类物质金属-有机框架材料的制备方法及应用 - Google Patents
一种包载辣椒素类物质金属-有机框架材料的制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种包载辣椒素类物质金属‑有机框架材料的制备方法及应用,包括以下步骤:将辣椒素类物质超声溶解在无水乙醇中形成辣椒素类物质溶液,富马酸和六水合三氯化铁分别溶解在超纯水中分别形成富马酸溶液和六水合三氯化铁溶液;将辣椒素类物质溶液与富马酸溶液混合,再向其中逐滴加入六水合三氯化铁溶液并搅拌反应一定时间,离心沉淀并洗涤干燥,得到负载有辣椒素类物质的金属‑有机框架材料。利用富马酸和FeCl3·6H2O合成的金属‑有机框架材料,同时将辣椒素类物质包埋其中,制得具有抑制金黄色葡萄球菌、单增李斯特菌、大肠杆菌和沙门氏菌能力的金属‑有机纳米复合材料,该材料制备方法简单,条件温和,是一种安全的、绿色的纳米材料。
Description
技术领域
本发明涉及食品抑菌保鲜技术领域,具体涉及一种包载辣椒素类物质金属-有机框架材料的制备方法及应用。
背景技术
辣椒素类物质是辣椒中产生辛辣感的一种具有香草基胺的酰胺类衍生物质,包含辣椒素、二氢辣椒素、去二氢辣椒素、同型辣椒素和同型二氢辣椒素五种天然辣椒素,其中辣椒素和二氢辣椒素是含量最多、最有效的辣椒素,占80%及以上。辣椒素类物质可发挥重要的食品功能活性,如抑制食源性致病菌、抗炎、改善消化性能等。但根据Wilbur Scoville的测定,辣椒素类物质的辣度高达1600万史高维尔热单位(SHU),具有极强的刺激性气味,水溶性较低,因此,其加工能力低,生物利用度低,刺激性和粘膜刺激性强,往往限制了其应用。为克服这些限制,有必要对辣椒素类物质进行有效的封装以提高其利用价值。
包埋是一种可以提升活性分子功能性的重要途径,可以提高和调控辣椒素类物质的功能应用。目前,常用包埋材料为淀粉、多糖、蛋白、乳液等,但这些包埋材料可设计性差,与大分子辣椒素类物质的构效关系不明确,装载控释效果较差。
金属-有机骨架(MOFs)是一类由金属离子或簇节点和有机连接剂作为桥梁组成的有机-无机杂化多孔材料。MOFs的独特性质如可设计易调控、稳定性较好、内部表面积大等优点使它们适合装载和释放具有不同物理化学性质的药物。近年来,逐步用于食品活性分子的递送。在不同的MOFs中,由铁和富马酸组成的生物相容性较好的MIL-88A具有价格低廉、合成简单、安全等优点。富马酸和铁都是内源性物质,富马酸是柠檬酸循环的代谢物,铁是人体内的微量元素,也是许多酶和蛋白质的必需辅助因子,利用这两种绿色原料合成的MIL-88A安全性高,尺寸小,拥有更大的比表面积,用其负载辣椒素类物质具有较高的负载率,且装载范围较广。
发明内容
针对上述问题,本发明提供一种包载辣椒素类物质金属-有机框架材料的制备方法,包括如下步骤:
步骤1:将辣椒素类物质超声溶解在无水乙醇中形成辣椒素类物质溶液,富马酸和六水合三氯化铁分别溶解在超纯水中分别形成富马酸溶液和六水合三氯化铁溶液;
步骤2:将辣椒素类物质溶液与富马酸溶液混合,再向其中逐滴加入六水合三氯化铁溶液并搅拌反应一定时间,离心沉淀并洗涤干燥,得到负载有辣椒素类物质的金属-有机框架材料;
所述辣椒素类物质、富马酸、六水合三氯化铁的摩尔比为1:2:2-1:8:8。
进一步的,所述步骤2中用于溶解辣椒素类物质的无水乙醇占整个反应体系的20%-80%。
进一步的,所述步骤2中反应时间为9h-15h。
进一步的,富马酸作为有机配体,Fe3+作为中心金属离子形成框架结构,框架结构中包载辣椒素类物质。
进一步的,所述金属-有机框架材料负载有辣椒素类物质的负载率为5.12%-10.17%。
进一步的,包载有辣椒素类物质的金属-有机框架材料在食品添加剂中的应用。
本发明的有益效果是:
1、从食品角度出发,选用绿色原料铁和富马酸制备可以包载辣椒素类物质的金属-有机纳米级材料,在室温下即可合成高效纳米复合材料,具有简单、绿色等优点,其中采用无水乙醇一是溶解辣椒素类物质,将其引入到MOF框架中,二是有机溶剂体系里面无水乙醇是一种比较温和的、绿色的溶剂。
2、本发明包载辣椒素类物质的包载效率可观,载量较高,反应时间为9h-15h,考虑到合成时间过短,包载辣椒素类的负载率不高,合成时间太长,材料制备的效率不高,综合选择在9h-15h时间内能负载更多的辣椒素类物质。
3、本发明通过MOF独特的框架结构包载辣椒素类物质,可有效发挥辣椒素类物质对食源性致病菌的抑制作用。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例的附图作简单地介绍,显而易见地,下面描述中的附图仅仅涉及本发明的一些实施例,而非对本发明的限制。
图1为本发明辣椒素类物质、富马酸、MOF、具有不同辣椒素类物质负载率的MOF-Cap复合材料的紫外扫描吸收光谱图示意图;
图2为本发明富马酸与三价铁离子形成的金属-有机框架包埋辣椒素类物质示意图;
图3为本发明辣椒素类物质、MOF和负载辣椒素类物质的MOF复合材料的X射线衍射光谱图示意图;
图4为本发明经负载辣椒素类物质的MOF复合材料处理3h后,金黄色葡萄球菌、单增李斯特菌、大肠杆菌和沙门氏菌的存活率。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例的附图,对本发明实施例的技术方案进行清楚、完整地描述。显然,所描述的实施例是本发明的一部分实施例,而不是全部的实施例。基于所描述的本发明的实施例,本领域普通技术人员在无需创造性劳动的前提下所获得的所有其他实施例,都属于本发明保护的范围。
下面结合附图和实施例对本发明进一步说明。
一种包载辣椒素类物质金属-有机框架材料的制备方法,包括以下步骤:
步骤1:将辣椒素类物质超声溶解在无水乙醇中形成辣椒素类物质溶液,富马酸和六水合三氯化铁分别溶解在超纯水中分别形成富马酸溶液和六水合三氯化铁溶液。
步骤2:将辣椒素溶液与富马酸溶液混合,再向其中逐滴加入六水合三氯化铁溶液并搅拌反应一定时间,离心沉淀并洗涤干燥,得到负载有辣椒素类物质的金属-有机框架材料。
其中,所述步骤2中用于溶解辣椒素类物质的无水乙醇占整个反应体系的20%-80%,采用无水乙醇一是溶解辣椒素类物质,将其引入到MOF框架中,二是有机溶剂体系里面无水乙醇是一种比较温和的、绿色的溶剂,综合两种原因选择无水乙醇。
其中,所述辣椒素类物质、富马酸、六水合三氯化铁的摩尔比为1:2:2-1:8:8;反应时间为9h-15h,考虑到合成时间过短,包载辣椒素类的负载率不高,合成时间太长,材料制备的效率不高,综合选择了在较短的时间内能负载更多的辣椒素类物质。
具体的,富马酸作为有机配体,Fe3+作为中心金属离子形成框架结构,框架结构中包载辣椒素类物质。如图2所示,球形是三价铁离子,杠杆为有机配体富马酸,三价铁离子和富马酸形成立体框架包裹辣椒素类物质;所述金属-有机框架材料包载有辣椒素类物质的负载率为5.12%-10.17%;另外,本发明提供了包载有辣椒素类物质的金属-有机框架材料在食品添加剂中的应用。
实施例1
将辣椒素类物质超声溶解在无水乙醇中,将富马酸和六水合三氯化铁各自溶解在超纯水中,辣椒素类物质与富马酸、六水合三氯化铁的摩尔比为1:2:2,无水乙醇占整个反应体系的50%,在50%乙醇环境下,能更多的溶解辣椒素类物质,同时能保证合成的材料产率更高,乙醇浓度过高,材料的产率较低,乙醇浓度过低,辣椒素类物质溶解量也相应减少,导致最终负载率较低,综合选择50%作为最终的反应环境。将辣椒素溶液与富马酸溶液混合,再向其中逐滴加入六水合三氯化铁溶液,搅拌反应12h,将反应溶液在7193rcf,20min离心,收集沉淀,并用无水乙醇洗涤三次,最后真空干燥得到的材料记为MOF-Cap-1。
实施例2
保持实施例1其他条件不变,仅将辣椒素类物质与富马酸、六水合三氯化铁的摩尔比分别调整为1:4:4,得到材料记为MOF-Cap-2。
实施例3
保持实施例1其他条件不变,仅将辣椒素类物质与富马酸、六水合三氯化铁的摩尔比分别调整为1:8:8,得到材料记为MOF-Cap-3。
对比例
保持实施例1其他条件不变,仅将辣椒素类物质与富马酸、六水合三氯化铁的摩尔比分别调整为0:1:1,得到MOF。
将上述MOF-Cap-1、MOF-Cap-2、MOF-Cap-3、MOF分别在柠檬酸缓冲液中溶解,再用乙酸乙酯多次萃取,合并萃取液,得到的萃取液通过紫外分光光度计扫描全谱(图1)并测其吸光度,得到MOF-Cap-1、MOF-Cap-2和MOF-Cap-3的辣椒素类物质负载率分别为10.17%、7.48%、5.12%,可知MOF-Cap-1材料中辣椒素负载率最高;测得MOF-Cap-1粒径为220nm,图3为空白MOF、MOF-Cap-1、辣椒素类物质的XRD图,可知空白MOF和MOF-Cap-1的晶体结构均符合MIL-88A。
实验例1
将MOF-Cap-1材料应用于金黄色葡萄球菌的抑制,其步骤如下:
将金黄色葡萄球菌以2%的比例接种于LB培养基中,37℃恒温震荡培养,活化12h,将活化一代的菌液以2%的比例接种于新的LB培养基中,再次活化12h,此时菌体已达到稳定期,对其活菌计数为109CFU/mL。
将培养至稳定期的菌液在4℃下7000rcf离心5min,去掉上清液,将沉淀下来的菌体用无菌生理盐水复溶,并用无菌生理盐水稀释至107CFU/mL,称取一定量的MOF-Cap-1材料分散于金黄色葡萄球菌悬液(浓度为107CFU/mL)中,抑菌材料终浓度为500μg/mL,对照组不加抑菌材料,将实验组菌液和对照组菌液在37℃恒温摇床上以150rpm的速度震荡,分别取处理3h后的菌液100μL,按照平板涂布法接种到PCA固体培养基,并将其置于37℃培养箱中培养18h,然后进行活菌菌落计数,按以下公式计算活菌率:
活菌率=实验组菌落数/对照组菌落数×100%。
实验例2
将MOF-Cap-1材料应用于单增李斯特菌的抑制,其步骤如下:
将单增李斯特菌以2%的比例接种于MH肉汤中,37℃恒温震荡培养,活化12h,将活化一代的菌液以2%的比例接种于新的MH肉汤中,再次活化12h,此时菌体已达到稳定期,在李斯特氏菌显色平板上进行活菌计数为107CFU/mL。
将培养至稳定期的菌液在4℃下7000rcf离心5min,去掉上清液,将沉淀下来的菌体用无菌生理盐水复溶,称取一定量的MOF-Cap-1材料分散于单增李斯特菌(浓度为107CFU/mL)中,抑菌材料浓终度为500μg/mL,对照组不加抑菌材料,将实验组菌液和对照组菌液在37℃恒温摇床上以150rpm的速度震荡,分别取处理3h后的菌液100μL,在李斯特氏菌显色平板上进行涂布计数,按以下公式计算活菌率:
活菌率=实验组菌落数/对照组菌落数×100%。
实验例3
将MOF-Cap-1材料应用于大肠杆菌抑制,操作同实施例1,按照实施例1中公式计算活菌率。
实验例4
将MOF-Cap-1材料应用于沙门氏菌的抑制,操作同实施例1,按照实施例1中公式计算活菌率。
结果如下,经MOF-Cap-1材料处理3h后,金黄色葡萄球菌、单增李斯特菌、大肠杆菌和沙门氏菌的活菌率如图4所示,可见MOF-Cap-1材料对实验所用的食源性致病菌均有较好的抑制效果。
另外,在室温下将辣椒素类物质及MOF-Cap-1复合材料分别溶解在水中,连续搅拌72h后,在紫分光光度计外下测得二者辣椒素类物质的溶解度分别为8±0.8ug/ml、51±1.1ug/mL,相比于未包埋前,MOF框架的引入有效提高了辣椒素类物质在水溶液中的溶解度和分散性。
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所做的任何简单修改、等同变化与修饰,均仍属于本发明技术方案的范围内。
Claims (6)
1.一种包载辣椒素类物质金属-有机框架材料的制备方法,其特征在于,包括如下步骤:
步骤1:将辣椒素类物质超声溶解在无水乙醇中形成辣椒素类物质溶液,富马酸和六水合三氯化铁分别溶解在超纯水中分别形成富马酸溶液和六水合三氯化铁溶液;
步骤2:将辣椒素类物质溶液与富马酸溶液混合,再向其中逐滴加入六水合三氯化铁溶液并搅拌反应一定时间,离心沉淀并洗涤干燥,得到负载有辣椒素类物质的金属-有机框架材料;
所述辣椒素类物质、富马酸、六水合三氯化铁的摩尔比为1:2:2-1:8:8。
2.根据权利要求1所述一种包载辣椒素类物质金属-有机框架材料的制备方法,其特征在于,所述步骤2中用于溶解辣椒素类物质的无水乙醇占整个反应体系的20%-80%。
3.根据权利要求1所述一种包载辣椒素类物质金属-有机框架材料的制备方法,其特征在于,所述步骤2中反应时间为9h-15h。
4.如权利要求1至3所述任一种制备方法得到的包载有辣椒素类物质的金属-有机框架材料,其特征在于,富马酸作为有机配体,Fe3+作为中心金属离子形成框架结构,框架结构中包载辣椒素类物质。
5.根据权利要求4所述一种包载有辣椒素类物质的金属-有机框架材料,其特征在于,所述金属-有机框架材料负载有辣椒素类物质的负载率为5.12%-10.17%。
6.如权利要求5所述一种包载有辣椒素类物质的金属-有机框架材料的应用,其特征在于,包载有辣椒素类物质的金属-有机框架材料在食品添加剂中的应用。
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