CN108546551B - 一种识别水体中铁离子的荧光探针及其制备方法和应用 - Google Patents

一种识别水体中铁离子的荧光探针及其制备方法和应用 Download PDF

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CN108546551B
CN108546551B CN201810065723.8A CN201810065723A CN108546551B CN 108546551 B CN108546551 B CN 108546551B CN 201810065723 A CN201810065723 A CN 201810065723A CN 108546551 B CN108546551 B CN 108546551B
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张建勇
邓维
史军霞
谷荣彩
崔鹏辉
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Abstract

本发明公开了一种识别水体中铁离子的荧光探针及其制备方法和应用。本发明的制备方法包括以下步骤：1)将TPT，OH‑H2BDC与四水合硝酸镉分散于DMA和水组成的混合溶剂中，得到前驱体溶液；2)将前驱体溶液借助溶剂热反应制得Cd‑MOF材料；(3)将Cd‑MOF材料加入到Eu3+溶液中，搅拌，抽滤，干燥得到Eu2+负载的荧光探针，其中的Eu3+在功能化“后修饰”过程中被“原位还原”成具有特殊蓝光发射的Eu2+离子。本发明制备方法简单，产率高；本发明的荧光探针测试样品无须前处理或前处理简单，对Fe3+离子表现出灵敏的识别性，荧光淬灭率可达到99％，可用于水体中Fe3+离子的识别检测。

Description

一种识别水体中铁离子的荧光探针及其制备方法和应用
技术领域
本发明属于荧光传感器技术领域，涉及一种荧光探针，具体来说是一种识别水体中铁离子的荧光探针及其制备方法和应用。
背景技术
众所周知，金属有机骨架材料(MOFs)在分子储存、分离和催化等方面有广泛的应用。多种可选择而且均匀的孔隙度，高的比表面积以及可辨别的发光变化使荧光金属有机骨架材料成为检测金属离子的手段。金属离子具有高的络合亲和力，可以很好的链接荧光发光配体，使得合成荧光金属有机骨架材料简单易得。这些MOFs材料表现出高敏感性、检测速率快和回收循环利用的优良特性。
金属离子在环境、生物和医学领域扮演着重要的角色，其浓度、种类以及价态对生命活动和环境都有重要的影响。比如钾、铁、锌等金属离子是生命体维持正常生理活动的必需元素。而一些重金属离子，由于在环境中不能分解并会通过食物链逐渐在生物链上层富集，易造成慢性中毒。自然界中的过量金属离子，特别是Fe3+的过量存在对生命体存在着严重的影响。铁在人体内很多代谢方面发挥重要功能，其中参与氧的储存和运输是其功能之一。血红蛋白在红细胞内作为载体参与氧气的运输；其中，铁在血红蛋白组成部分中占重要位置，负责与氧气的结合，然后随血液向身体各处运输，供应与进行呼吸氧化作用，使能量得以参与食物消化，从而获取营养；铁本身毒性很低，但摄入量过多或误食铁制剂可能会导致铁元素中毒。除此之外，生活垃圾中存在大量的Fe3+，侵占土地城市的生活垃圾，如果不做及时的处理处置，将会侵害农田，使农业生产、自然景观、植被甚至地貌遭到破坏。因此，金属离子的检测尤其铁离子检测对自然界有着至关重要的意义。目前，对于金属离子检测主要使用原子发光和吸收光谱，该方法具有灵敏度高，准确度高等，但是需使用大型仪器，检测成本高，不利于广泛推广。
发明内容
为了克服现有技术的不足，本发明的目的在于提供一种识别水体中铁离子的荧光探针及其制备方法和应用。本发明的荧光探针合成步骤简单，用料少，能大量制备；本发明的荧光探针用于水体中铁离子检测操作简单，只需要稀土掺杂的探针分子和待测含金属离子的溶液混合，使用简单的荧光分光光度计检测即可；检测时间短，灵敏度高，选择性强。
本发明将2,4,6-三(4-吡啶基)-1,3,5-三嗪(TPT)和5-羟基间苯二甲酸(OH-H2BDC)混合配体与硝酸镉盐形成三维结构的多孔的金属有机框架材料，并通过“后修饰”法和“原位还原”反应将稀土Eu3+离子引入到配合物孔道内，增强了配合物本身的荧光特性，形成Eu2+掺杂的荧光探针，用于水体中三价铁离子的检测。
本发明解决技术问题的技术方案具体如下。
本发明提供一种识别水体中铁离子的荧光探针，其以Cd2+的金属有机框架材料Cd-MOF为基体，通过“原位还原”方法引入具有特殊蓝光发射的稀土金属离子Eu2+做荧光探针。
本发明中，二价镉的金属有机框架材料Cd-MOF是以2,4,6-三(4-吡啶基)-1,3,5-三嗪与5-羟基间苯二甲酸为混合配体，将混合配体和硝酸镉盐通过溶剂热反应制得。
本发明还提供一种上述的荧光探针的制备方法，包括以下步骤：
(1)将2,4,6-三(4-吡啶基)-1,3,5-三嗪、5-羟基间苯二甲酸和硝酸镉盐在N,N-二甲基乙酰胺(DMA)和水组成的混合溶剂中分散，形成前驱体溶液；
(2)将前驱体溶液在90～120℃的温度下进行溶剂热反应，反应48-120小时，之后抽滤、洗涤，得到三维结构Cd-MOF材料；
(3)将三维结构Cd-MOF材料加入到0.1mol/L的Eu(NO3)3的水溶液中，搅拌48小时，抽滤，洗涤，烘干得到荧光探针。
本发明中，步骤(1)中，N,N-二甲基乙酰胺和水的体积比为2:1～1：2；步骤(1)中，2,4,6-三(4-吡啶基)-1,3,5-三嗪和5-羟基间苯二甲酸的摩尔比在1:1～1:2之间，二价钴盐和2,4,6-三(4-吡啶基)-1,3,5-三嗪的摩尔比为1:1～3:1之间。
本发明进一步提供一种上述的识别水体中铁离子的荧光探针在检测水体中铁离子方面的应用。优选的，应用方法包括以下步骤：称取3mg Eu2+@Cd-MOF材料加入到3ml含各种金属离子的溶液中，超声分散后，进行荧光检测。
和现有技术相比，本发明的有益效果在于：
本发明材料合成工艺简单，材料结构可控组装，材料性能可控调变，得到的基于二价镉的金属有机框架材料作为稀土掺杂的基体，形成选择性极高的荧光探针。该荧光探针具有较高的荧光发射效率和荧光稳定性，对不同金属离子有不同的响应，但是对铁离子有特异性响应。该探针合成简单，易于生产，节省资本，对铁离子检测有更短的检测时间，更高的灵敏度，能检测铁离子浓度低至1×10-5mol/L的水体。
附图说明
图1为不同样品的X-射线粉末衍射图谱。
图2为荧光探针对浓度为1×10-2mol/L的不同金属离子的响应图。
图3为荧光探针对不同浓度的Fe3+离子的荧光滴定图。
具体实施方式
下面结合具体的实施实例对本发明做进一步详细完整的说明。以下实例中如无特殊说明均为常规方法，实例中所涉及的所有药品均来自商业途径。以下描述的内容是对本发明的技术方案作进一步的描述，但本发明并不限于下述实施例。
实施例1
(1)按照2,4,6-三(4-吡啶基)-1,3,5-三嗪(TPT)与5-羟基间苯二甲酸摩尔比例为1:1称量，混合后成为混配体；
(2)按照Cd(NO3)2.4H2O与(1)中TPT配体摩尔比1:1的比例称量Cd(NO3)2·4H2O；
(3)将(1)和(2)中称量的试剂在超声或者搅拌下在DMA/H2O(其中DMA和H2O的体积比为4：4)溶剂8毫升中混合溶解，配制成前驱体溶液；
(4)将(3)所得前驱体溶液转入水热釜中，在120℃下进行溶剂热反应72小时，抽滤、洗涤、干燥得到一种三维结构Cd-MOF材料。
(5)将(4)中Cd-MOF 3mg加入3ml 0.1mol/L的Eu(NO3)3溶液中，搅拌48小时，抽滤，干燥得到Eu2+@Cd-MOF探针材料。
通过X-射线粉末衍射，我们表征了材料的稳定性，如图1所示，在“后修饰”和“原位还原”反应后，材料的衍射峰位置和衍射强度跟原材料基本保持一致，说明材料的骨架结构在反应前后稳定存在。
我们测试了Eu2+@Cd-MOF材料对不同金属离子的响应作用。称取3mg新鲜制备的Eu2 +@Cd-MOF样品，经研磨后放入水中超声30分钟使其均匀分散，然后分别加入金属离子(Mg2+、Fe3+、Ba2+、Pb2+、Al3+、Na+、K+、Ca2+、Zn2+、Ag+、Cr3+、Cd2+、Co2+、Cu2+、Sr2+和Ni2+)的硝酸盐，使金属离子的浓度控制在1×10-2mol/L，混合均匀后测定其混合溶液荧光。测试结果如图2所示。通过荧光强度的变化我们可以看出加入不同的金属离子后，Eu2+@Cd-MOF样品的荧光光谱呈现出不同强度的荧光淬灭或增强，其中加入Fe3+离子后的荧光淬灭最为明显，基本上可实现完全淬灭，淬灭效率为99％，而加入其它金属离子的荧光变化相对不是很明显。由此可见，该Eu2+@Cd-MOF材料对Fe3+离子具有较专一的选择性，可用做Fe3+离子的荧光探针。
实施例2
Eu2+@Cd-MOF材料的合成及应用
(1)按照2,4,6-三(4-吡啶基)-1,3,5-三嗪(TPT)与5-羟基间苯二甲酸摩尔比例为1:1称量，混合后成为混配体；
(2)按照Cd(NO3)2.4H2O与(1)中TPT配体摩尔比2:1的比例称量Cd(NO3)2.4H2O；
(3)将(1)和(2)中称量的试剂在超声或者搅拌下在DMA/H2O(其体积比为4：4)溶剂8毫升中混合溶解，配制成前驱体溶液；
(4)将(3)所得前驱体溶液转入水热釜中，在120℃下进行溶剂热反应72小时，抽滤、洗涤、干燥得到一种棒状晶态材料Cd-MOF。
(5)将(4)中Cd-MOF材料3mg加入3ml 0.1mol/L的Eu(NO3)3溶液中，搅拌48小时，抽滤，干燥得到Eu2+@Cd-MOF探针材料。
通过X-射线粉末衍射，我们表征了材料的稳定性，如图1所示，在“后修饰”和“原位还原”反应后，材料的衍射峰位置和衍射强度跟原材料基本保持一致，说明材料的骨架结构在反应前后稳定存在。
由于该荧光探针对Fe3+的淬灭效率最高，选择性强。因此，研究了Eu2+@Cd-MOF对不同浓度Fe3+离子的响应作用。称取3mg新鲜制备的Eu2+@Cd-MOF样品，经研磨后放入水中超声30分钟使其均匀分散，配制不同Fe3+浓度的水溶液：5×10-5mol/L，1×10-5mol/L，5×10- 4mol/L，1×10-4mol/L,5×10-3mol/L，1×10-3mol/L，5×10-2mol/L，1×10-2mol/L，然后量取不同浓度的Fe3+离子溶液3ml加入到分散好的Eu2+@Cd-MOF样品溶液中，超声处理两者混合液30分钟，混合均匀后测定其混合溶液荧光。测试结果如图3所示。随着Fe3+离子浓度的增大，荧光强度显示出逐渐变小的趋势。在浓度达到1×10-2mol/L时，荧光几乎完全淬灭。

Claims (2)

1.一种识别水体中铁离子的荧光探针的制备方法，其特征在于：其以Cd2+的金属有机框架材料Cd-MOF为基体，通过“原位还原”方法引入具有特殊蓝光发射的稀土金属离子Eu2+做荧光探针；该荧光探针的制备方法，包括以下步骤：
(1)将2,4,6-三(4-吡啶基)-1,3,5-三嗪、5-羟基间苯二甲酸和硝酸镉Cd(NO3)2·4H2O在N,N-二甲基乙酰胺DMA和水组成的混合溶剂中分散，形成前驱体溶液；
(2)将前驱体溶液在90～120℃的温度下进行溶剂热反应，反应48～120小时，之后抽滤、洗涤，得到三维结构的Cd-MOF材料；
(3)将Cd-MOF材料加入到0.1mol/L的Eu(NO3)3水溶液中，搅拌24～48小时，抽滤，干燥得到荧光探针材料。
2.根据权利要求1所述的制备方法，其特征在于，步骤(1)中，2,4,6-三(4-吡啶基)-1,3,5-三嗪和5-羟基间苯二甲酸的摩尔比在1:1～1:2之间，硝酸镉和2,4,6-三(4-吡啶基)-1,3,5-三嗪的摩尔比为1:1～3:1之间。
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