CN109499582B - 一种复合氧化物模拟酶材料及其制备方法和用途 - Google Patents
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Abstract
本发明涉及模拟酶技术，具体说是一种复合氧化物(CoV复合氧化物)模拟酶材料及其制备和应用。通过沉淀剂尿素沉淀法制备CoV的层状双羟基复合金属氢氧化物前体，然后通过焙烧处理得CoV的复合氧化物模拟酶材料。本发明提供的钴钒氧化物模拟酶同时具有氧化酶和过氧化物酶活性的多重特征。所得复合材料具有合成步骤易操作、成本小、效果显著等特点，在新型催化氧化分析中具有广阔的应用前景。
Description
技术领域
本发明涉及模拟酶技术，具体说是一种复合氧化物(CoV复合氧化物)模拟酶材料及其制备和应用。
背景技术
近年来，随着纳米技术的开发，越来越多的纳米材料或纳米复合材料被发现具有模拟酶的性质，极大扩展了酶的试用条件，如四氧化三铁纳米粒子、二氧化铈纳米材料[Asati A,Kaittanis C,Santra S,et al.pH-tunable oxidase-like activity ofcerium oxide nanoparticles achieving sensitive fluorigenic detection ofcancer biomarkers at neutral pH.Analytical Chemistry,2011,83(7):2547-2553]、碳纳米管、碳量子点、贵金属纳米颗粒金、银、铂[Jiang H,Chen Z,Cao H,et al.Peroxidase-like activity of chitosan stabilized silver nanoparticles for visual andcolorimetric detection of glucose.Analyst,2012,137(23):5560-5564；MoglianettiM,De Luca E,Pedone D,et al.Platinum nanozymes recover cellular ROShomeostasis in an oxidative stress-mediateddisease model.Nanoscale,2016,8(6):3739-3752]等、和双金属纳米材料。
但是纳米颗粒因尺寸小，具有高的表面能，则容易发生团聚。多功能复合材料纳米模拟酶不仅能控制纳米材料大小，统一形貌，还能使其保持高催化活性。这对纳米模拟酶深入发展研究具有重要的理论指导与实际意义。
发明内容
本发明的目的在于提供一种复合氧化物(CoV复合氧化物)模拟酶材料及其制备和应用。
为实现上述目的，本发明采用的技术方案为：
一种复合氧化物模拟酶材料的制备方法，通过沉淀剂尿素沉淀法制备CoV的层状双羟基复合金属氢氧化物前体，然后通过焙烧处理得CoV的复合氧化物模拟酶材料。
进一步的说，将Co2+可溶性盐与三氯化钒(VCl3)按物质的量4～2:1的比例为混合，再加入尿素(CO(NH2)2)，加入后一并溶于水中混匀直至澄清透明，而后置于水热反应釜中120-150℃(优选120℃)下晶化12h，晶化结束后自然冷却至室温后取出清洗、干燥，干燥后于300-800℃(优选300-500℃)下焙烧2h得到Co-V-MMO模拟酶材料；其中，尿素(CO(NH2)2)加量为Co源物质的量的1-3倍。
所述晶化处理后依次用超纯水、乙醇洗涤，洗涤后于4000转/min离心分离10min，离心后沉淀于80℃干燥6h，干燥后培烧得到Co-V MMO模拟酶材料。
所述Co2+可溶性盐为硝酸钴、氯化钴或草酸钴。
复合氧化物模拟酶材料，按所述方法制备获得Co-V复合氧化物模拟酶材料。
复合氧化物模拟酶材料的应用，所述Co-V的复合氧化物在作为模拟氧化物或过氧化物酶中的应用。
所述Co-V的复合氧化物作为氧化物或过氧化物模拟酶，在对底物进行催化氧化还原反应。
所述Co-V的复合氧化物作为氧化物或过氧化物模拟酶，在酸性条件下对底物进行催化氧化还原反应。
所述底物为TMB；或TMB和H2O2。
本发明与现有技术相比，具有以下优点及突出性效果：
本发明通过尿素沉淀法制备出CoV复合金属前体，然后通过焙烧处理得分散性高、具有活化性能的钴钒复合氧化物氧化物模拟酶和过氧化物模拟酶双酶活性材料；并且模拟酶材料在酸性条件下具有高的化学稳定性，同时本发明材料成本低、制备方法简单、重复性好；作为一种新颖模拟酶在免疫分析、生物检测和临床诊断等领域都有潜在的应用价值；同时模拟酶在新型催化氧化分析中具有广阔的应用前景。
附图说明：
图1为本发明实施案例提供的复合纳米材料TEM图；
图2为本发明实施案例提供的定性分析材料成分X-射线衍射图；
图3为本发明实施例提供的复合纳米模拟酶类似过氧化物酶催化活性时的比色照片图。
具体实施方式
以下通过具体的实施例对本发明作进一步说明，有助于本领域的普通技术人员更全面的理解本发明，但不以任何方式限制本发明。
实施例1：
2.4mmol六水氯化钴、0.8mmol三氯化钒(VCl3)和5mmol尿素(CO(NH2)2)溶于35mL水中搅拌至澄清透明，澄清透明液体置于40mL水热反应釜中120℃下晶化12h，晶化结束后自然冷却至室温，冷却至室温后取出依次用超纯水、无水乙醇分别超声清洗3次，清洗后于80℃干燥6h，然后用马弗炉400℃下焙烧2h得到Co-V-MMO模拟酶材料。Co-V-MMO模拟酶材料形貌TEM如图1所示。700℃XRD测试结果表明产物为Co3O4/Co3V2O8(见图2)。
由图1TEM图可见CoV-MMO为形貌均一的纳米片；由图2可看出合成钴钒复合纳米材料和成分通过与Co3O4和Co3V2O8标准的标准卡片Co3O4(43-1003)和Co3V2O8(16-0675)相吻合，另外图谱中没有出现其他任何杂质相。
实施例2-18
制备过程：
2.4mmol六水氯化钴与不同添加量的三氯化钒(VCl3)和5mmol尿素(CO(NH2)2)溶于35mL水中搅拌至澄清透明，澄清透明液体置于40mL水热反应釜中120℃下晶化12h，晶化结束后自然冷却至室温后取出依次用超纯水、无水乙醇分别超声清洗3次，清洗后80℃干燥6h，然后用马弗炉300-800℃下焙烧2h得到化学成分为Co3O4/Co3V2O8的Co-V-MMO模拟酶材料(参见表1)。各合成钴钒复合纳米材料和成分Co3O4和Co3V2O8标准的标准卡片(JCPDS No.47-1049和JCPDS No.74-1394)比对相吻合，没有出现其他任何杂质相。
表1
应用例
取100μL3mM H2O2，100μL 3mM TMB，750μL pH为4的醋酸钠缓冲液，再加入浓度为50μg/ml的上述实施例获得模拟酶材料；同时以未加入上述模拟酶材料的体系作为对照1，未加入过氧化氢和TMB的体系作为对照2，未加入TMB的体系作为对照3，未加入过氧化氢为对照4。室温下(25℃)下反应(测试波长范围内吸光度变化参见图3)，由图3可见未加入模拟酶水溶液的对照1，过氧化氢对TMB没有氧化活性；而当不加入过氧化氢和TMB对照2，溶液也是略显浅黄色；当不加入TMB对照3，溶液也是略显浅黄色；当不加入过氧化氢对照4，溶液变浅蓝色，说明复合纳米材料有氧化酶性质；当TMB和过氧化氢时加入模拟酶水溶液，溶液蓝色较对照组4更深，说明复合纳米材料具有过氧化物模拟酶活性。
经离心洗涤后，不补充模拟酶材料，循环6次，模拟酶性能基本保持稳定，说明模拟酶材料稳定性较好。
Claims (6)
1.一种复合氧化物模拟酶材料的制备方法，其特征在于：通过沉淀剂尿素沉淀法制备CoV的层状双羟基复合金属氢氧化物前体，然后通过焙烧处理得CoV的复合氧化物模拟氧化物酶或过氧化物酶；
将Co2+可溶性盐与三氯化钒VCl3按物质的量的比例为4~2:1混合，再加入尿素CO(NH2)2，加入后一并溶于水中混匀直至澄清透明，而后置于水热反应釜中120-150℃下晶化12 h，晶化结束后自然冷却至室温后取出清洗、干燥，干燥后于300-800℃下焙烧2h得到Co-V-MMO模拟酶材料；
所述晶化处理后依次用超纯水、乙醇洗涤，离心后，沉淀干燥后焙烧得到Co-V MMO模拟酶材料；
所述Co2+可溶性盐为硝酸钴、氯化钴或草酸钴。
2.按权利要求1所述方法制备的复合氧化物模拟酶材料，其特征在于：按权利要求1所述方法制备获得Co-V复合氧化物模拟酶材料。
3.按权利要求2所述的复合氧化物模拟酶材料的应用，其特征在于：所述Co-V的复合氧化物在作为模拟氧化物或过氧化物酶中的应用。
4.按权利要求3所述的复合氧化物模拟酶材料的应用，其特征在于：所述Co-V的复合氧化物作为氧化物或过氧化物模拟酶，在对底物进行催化氧化还原反应。
5.按权利要求4所述的复合氧化物模拟酶材料的应用，其特征在于：所述Co-V的复合氧化物作为氧化物或过氧化物模拟酶，在酸性条件下对底物进行催化氧化还原反应。
6.按权利要求5所述的复合氧化物模拟酶材料的应用，其特征在于：所述底物为TMB或TMB和H2O2。
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