CN112903635B - 一种双发射CDs/R6G@ZIF-8比率荧光探针在检测Fe3+中的应用 - Google Patents
一种双发射CDs/R6G@ZIF-8比率荧光探针在检测Fe3+中的应用 Download PDFInfo
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Abstract
本发明公开了一种双发射CDs/R6G@ZIF‑8比率荧光探针在检测Fe3+中的应用，所述双发射CDs/R6G@ZIF‑8比率荧光探针包括蓝色发光碳点，以及绿色发光的罗丹明6G。比率荧光探针易于保存，稳定性很好，对Fe3+具有良好的选择性，可实现对水溶液中Fe3+的特异性识别检测，操作简单方便且灵敏度高，同时，这种比率荧光探针可以消除环境和人为因素的干扰，减小实验误差，增加实验结论的可靠性。
Description
技术领域
本发明属于化学检测方法技术领域，具体涉及一种双发射 CDs/R6G@ZIF-8比率荧光探针在检测Fe3+中的应用。
背景技术
铁是人体必需的微量营养素，大多数生物电子转移过程都依赖铁蛋白。而Fe3+是血红蛋白的主要成分，可以促进血液中的氧气运输。铁在新生婴儿的大脑发育，体温调节和肌肉功能中起着重要作用。此外，孕妇铁缺乏症会增加患贫血和败血症的风险，并伴有高死亡率和高发病率。另外，铁超载可能导致神经系统疾病，如阿尔茨海默氏病和帕金森氏病。
由于铁离子(Fe3+)是生物系统中重要的过渡金属离子，在许多重要的化学和生物学过程中起着至关重要的作用。同时，Fe3+也是水中常见的污染物，饮用水中过量的Fe3+也可能导致人体健康问题。因此，开发高灵敏度，高选择性的探针检测Fe3+具有相当重要的意义。到目前为止，已经开发出了几种用于Fe3+检测的方法，包括原子吸收光谱法，电化学方法、电感耦合等离子体质谱法(ICPMS)和等离子体解吸质谱法。但是，它们的成本很高且缺乏便携性。而荧光分析技术由于其高灵敏度，特异性和易操作性等在离子检测方面占独特优势。
双发射CDs/R6G@ZIF-8比率荧光探针因其多孔结构的ZIF-8具有可以富集目标分析物和放大荧光信号的功能，可调节的发射性以及良好的水分散性而受到关注，有广阔的应用前景。
发明内容
本发明的目的在于根据上述背景技术的现状，提供了一种双发射CDs/R6G@ZIF-8比率荧光探针在检测Fe3+中的应用。
本发明的目的通过以下技术方案来具体实现：
一种双发射CDs/R6G@ZIF-8比率荧光探针在检测Fe3+中的应用，所述双发射CDs/R6G@ZIF-8比率荧光探针包括ZIF-8包裹的蓝色发光碳点(CDs)，以及绿色发光的罗丹明6G(R6G)。
作为优选的，采用比率荧光分析法检测Fe3+，所述蓝色发光碳点的荧光为响应信号，绿色发光罗丹明6G的荧光为参考信号。
Fe3+对碳点的荧光具有猝灭作用，可作为荧光分析检测的响应信号。由于罗丹明6G的荧光强度不受Fe3+的影响，可作为稳定的参考信号。罗丹明6G的荧光强度和碳点的荧光强度的比值与Fe3+浓度呈线性关系。
作为优选的，所述蓝色发光碳点通过水热法由谷胱甘肽和柠檬酸钠反应制得。
作为优选的，所述双发射CDs/R6G@ZIF-8比率荧光探针通过以下步骤制得：
(1)将谷胱甘肽与柠檬酸钠通过水热法反应得到带酚羟基官能团的蓝色发光碳点；
(2)将步骤(1)得到的蓝色发光碳点、罗丹明6G、2-甲基咪唑和六水合硝酸锌进行一锅法室温自组装反应，即得所述双发射 CDs/R6G@ZIF-8比率荧光探针。
作为优选的，步骤(1)中，所述谷胱甘肽和柠檬酸钠的质量比为7.5:1，水热反应温度为200℃，时间为4h。
作为优选的，步骤(2)中，所述蓝色发光碳点为5mL、罗丹明 6G为40mg、2-甲基咪唑为160mmol，六水合硝酸锌为40mmol。
作为优选的，所述一锅法室温自组装反应的时间为24h。
进一步优选的，Fe3+的检测过程包括：
(1)将10mg的CDs/R6G@ZIF-8粉末分散在10mL的超纯水中，配制成1mg/mL的悬浮液，然后将20μL制备的CDs/R6G@ZIF-8悬浮液转移到石英池中，并添加1.98mL超纯水，保证总体积为2mL；
(2)将Fe3+的供试溶液加入步骤(1)的溶液中，用荧光光谱仪检测荧光信号强度。
更进一步优选的，步骤(2)中，荧光光谱仪的激发波长为351nm。
本发明具有以下有益效果：
本发明提供的双发射CDs/R6G@ZIF-8比率荧光探针在检测Fe3+中的应用，比率荧光探针易于保存，稳定性很好，对Fe3+具有良好的选择性，可实现对水溶液中Fe3+的特异性识别检测，操作简单方便且灵敏度高，同时，这种比率荧光探针可以消除环境和人为因素的干扰，减小实验误差，增加实验结论的可靠性。
附图说明
图1是本发明的双发射CDs/R6G@ZIF-8比率荧光探针的紫外可见吸收光谱图。
图2是双发射CDs/R6G@ZIF-8比率荧光探针对不同金属离子的选择性图。
图3是双发射CDs/R6G@ZIF-8比率荧光探针的时间响应图。
图4是不同浓度的Fe3+对双发射CDs/R6G@ZIF-8比率荧光探针荧光强度的影响图。
图5是不同浓度的Fe3+滴定的线性关系图。
具体实施方式
以下对本发明的优选实施例进行说明，应当理解，此处所描述的优选实施例仅用于说明和解释本发明，并不用于限定本发明。
实施例1
双发射CDs/R6G@ZIF-8比率荧光探针的合成：
1)蓝色发光碳点(CDs)的合成：将柠檬酸钠(0.3g)和谷胱甘肽(0.04g)与9mL超纯水混合，然后在衬有特氟龙的高压釜中将溶液在200℃下加热4h。所获得的黄色产物用500Da的透析袋纯化 12h，浓度约为0.12mg/mL。
2)ZIF-8的制备：将Zn(NO3)2·6H2O(40mmol)溶于20mL的去离子水中,得到溶液A。将2-甲基咪唑(160mmol)溶于20mL的去离子水中，得到溶液B。将溶液A加入到溶液B中，混合均匀后再磁力搅拌24小时,通过离心、干燥，最终获得白色的ZIF-8。
3)双发射CDs/R6G@ZIF-8比率荧光探针的合成：将 Zn(NO3)2·6H2O(40mmol)溶于20mL的去离子水中，得到溶液A。将2-甲基咪唑(160mmol)溶于20mL的去离子水中，得到溶液B。将溶液A加入到溶液B中，再加入5mL的步骤(1)制备的蓝色发光碳点(CDs)和40mg罗丹明6G(R6G)，将混合溶液超声均匀后，在磁力搅拌下室温自组装24h后，通过离心、干燥，最终获得粉色的CDs/R6G@ZIF-8复合材料。
CDs/R6G@ZIF-8的紫外吸收光谱如图1所示。在超纯水中测试了R6G、ZIF-8、蓝色发光碳点(CDs)(以及CDs/R6G@ZIF-8复合材料的紫外可见吸收光谱。在540nm处观察到R6G的紫外吸收，在 330nm处观察到蓝色碳点的紫外吸收。CDs/R6G@ZIF-8复合材料在 334nm和543nm处均有吸收，说明ZIF-8中存在R6G和CDs，证明了该复合材料的成功制备。
实施例2
荧光分析法检测Fe3+：
样品溶液：配制1mmol/L的Fe3+溶液以及其它金属阳离子溶液，待用。
将10mg的CDs/R6G@ZIF-8粉末分散在10mL的超纯水中，配制成1mg/mL的悬浮液。然后取20μL制备的CDs/R6G@ZIF-8悬浮液转移到石英池中，并添加1.98mL超纯水(保证总体积为2mL)。最后使用精密微量移液枪按从少到多的顺序添加不同浓度的Fe3+，检测Fe3+样品溶液对CDs/R6G@ZIF-8探针荧光信号的影响。荧光光谱仪的狭缝宽度设定为6nm，设置激发光波长为351nm，测出 CDs/R6G@ZIF-8的发射波长为438nm和548nm，438nm为碳点所发射的蓝色荧光峰，548nm为R6G所发射的绿色荧光峰。结果显示加入Fe3+后，随着Fe3+浓度的增加，438nm出现荧光减弱现象，548 nm处的峰基本无变化。
向荧光探针溶液中加入Fe3+溶液(5μmol/L)，其他可能共存的金属离子50μmol/L，证明CDs/R6G@ZIF-8探针对Fe3+的特异性，结果如图2所示，只有Fe3+对蓝色碳点的荧光强度有明显猝灭作用，其他的金属离子对荧光探针的强度几乎没有影响，表明 CDs/R6G@ZIF-8探针对Fe3+具有良好的选择性，可实现Fe3+的特异性识别检测。
分别对CDs/R6G@ZIF-8和滴加了Fe3+的CDs/R6G@ZIF-8进行了荧光强度随时间的变化，结果如图3所示，发现荧光强度随着时间几乎不会发生变化，说明该荧光探针稳定性良好。
向荧光探针溶液中加入一系列不同浓度(0-100μmol/L)Fe3+溶液，分别检测不同浓度Fe3+对探针荧光信号的影响，结果如图4所示，可以看出随着Fe3+浓度的增大，438nm处的荧光强度减弱的越来越明显，而548nm处的荧光基本无变化，并且呈良好的线性，结果如图5所示，线性方程：I548/I438＝0.0041x+0.37001、线性范围： 1-60μmol/L、检测限：94nmol/L，其中，x为Fe3+的浓度。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (9)
1.一种双发射CDs/R6G@ZIF-8比率荧光探针在检测Fe3+中的应用，其特征在于，所述双发射CDs/R6G@ZIF-8比率荧光探针包括蓝色发光碳点，以及绿色发光的罗丹明6G。
2.根据权利要求1所述的应用，其特征在于，采用比率荧光分析法检测Fe3+，所述蓝色发光碳点的荧光为响应信号，绿色发光罗丹明6G的荧光为参考信号。
3.根据权利要求1所述的应用，其特征在于，所述蓝色发光碳点通过水热法由谷胱甘肽和柠檬酸钠反应制得。
4.根据权利要求1所述的应用，其特征在于，所述双发射CDs/R6G@ZIF-8比率荧光探针通过以下步骤制得：
(1)将谷胱甘肽与柠檬酸钠通过水热法反应得到带酚羟基官能团的蓝色发光碳点；
(2)将步骤(1)得到的蓝色发光碳点、罗丹明6G、2-甲基咪唑和六水合硝酸锌进行一锅法室温自组装反应，即得所述双发射CDs/R6G@ZIF-8比率荧光探针。
5.根据权利要求4所述的应用，其特征在于，步骤(1)中，所述谷胱甘肽和柠檬酸钠的质量比为7.5:1，水热反应温度为200℃，时间为4h。
6.根据权利要求4所述的应用，其特征在于，步骤(2)中，所述蓝色发光碳点为5mL、罗丹明6G为40mg、2-甲基咪唑为160mmol，六水合硝酸锌为40mmol。
7.根据权利要求4所述的应用，其特征在于，步骤(2)中，所述一锅法室温自组装反应的时间为24h。
8.根据权利要求1-7任一项所述的应用，其特征在于，Fe3+的检测过程包括：
(1)将10mg的CDs/R6G@ZIF-8粉末分散在10mL的超纯水中，配制成1mg/mL的悬浮液，然后将20μL制备的CDs/R6G@ZIF-8悬浮液转移到石英池中，并添加1.98mL超纯水，保证总体积为2mL；
(2)将Fe3+的供试溶液加入步骤(1)的溶液中，用荧光光谱仪检测荧光信号强度。
9.根据权利要求8所述的应用，其特征在于，步骤(2)中，荧光光谱仪的激发波长为351nm。
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