CN112179960B - 一种基于五苯基吡咯的水相电化学发光体系的构建方法 - Google Patents

一种基于五苯基吡咯的水相电化学发光体系的构建方法 Download PDF

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CN112179960B
CN112179960B CN202010845517.6A CN202010845517A CN112179960B CN 112179960 B CN112179960 B CN 112179960B CN 202010845517 A CN202010845517 A CN 202010845517A CN 112179960 B CN112179960 B CN 112179960B
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卢小泉
邓彦芳
吴艳霞
韩振刚
白蕾
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Abstract

本发明公开了一种基于五苯基吡咯的水相电化学发光体系的构建方法，将电化学发光试剂五苯基吡咯溶解于N,N‑二甲基甲酰胺中，得五苯基吡咯溶液，以K2S2O8作为体系的共反应剂，将五苯基吡咯溶液加入含有K2S2O8的磷酸盐缓冲溶液中，得电化学发光试剂溶液，然后将裸的玻碳电极、铂柱电极和Ag/AgCl电极分别作为工作电极、对电极与参比电极浸入到电化学发光试剂溶液中。该方法构建的水相电化学发光体系相比其他有机物发光体在水相的电化学性能，五苯基吡咯水相电化学发光体系具有良好的发光性能以及高的稳定性和重现性；五苯基吡咯可作为一种新型的聚集诱导发光试剂用于电化学发光体系的构建。

Description

一种基于五苯基吡咯的水相电化学发光体系的构建方法
技术领域
本发明属于水相电化学发光体系构建技术领域，具体涉及一种基于五苯基吡咯的水相电化学发光体系的构建方法。
背景技术
电化学发光体系中最早涉及的有机物发光体是多环芳烃(PAHs)，如蒽(anthracene)、9,10-二苯基蒽(DPA)等，以及其他一些发光体，如卟啉类化合物。但是由于绝大多数有机化合物为疏水性平面分子，在水相体系中溶解性差且容易发生Π-Π堆积从而导致荧光猝灭，使得其在固态以及聚集态的荧光强度大大减弱，从而在很大程度上限制了有机发光体在水相电化学发光体系中的应用。虽然也有研究报道，通过物理方法或化学方法修饰改善大多数因Π-Π堆积而引起的荧光淬灭问题，使其适用于水相电化学发光体系，但是操作过程复杂，并且不具有普适性。
发明内容
本发明的目的是为了解决上述问题，提供一种基于五苯基吡咯的水相电化学发光体系的构建方法，该体系易于构建，发光剂用量少，重现性好，能够在水相中产生强而稳定的电化学发光信号。
本发明的目的通过以下技术方案来具体实现：
一种基于五苯基吡咯(PentaPP)的水相电化学发光体系的构建方法，将电化学发光试剂五苯基吡咯溶解于N,N-二甲基甲酰胺(DMF)中，得五苯基吡咯溶液，以K2S2O8作为体系的共反应剂，将五苯基吡咯溶液加入含有K2S2O8的磷酸盐缓冲溶液中，得电化学发光试剂溶液，然后将裸的玻碳电极、铂柱电极和Ag/AgCl电极分别作为工作电极、对电极与参比电极浸入到电化学发光试剂溶液中。
作为优选的，所述五苯基吡咯溶液中五苯基吡咯的浓度为10mmol/L，所述磷酸盐缓冲液的pH值为7.0，含有0.1mol/L的K2S2O8，五苯基吡咯在磷酸盐缓冲液中的浓度为2×10-5mmol/L。
更进一步的，体系构建好后用毛细管电泳-电化学发光分析仪进行检测，电化学发光分析仪的光电倍增管偏压设置为800V，扫速为0.1V·s-1，电势窗为-1.7～-0.1V。
五苯基吡咯(PentaPP)是一种非平面分子，具有聚集诱导发光增强(AIEE)活性。本发明将其应用于水相电化学发光性能研究，该体系不良溶剂水与良溶剂DMF的比例远大于99:1，由于其聚集诱导发光增强活性可实现水相介质中强的发光信号。
本发明具有以下有益效果：
本发明提供的基于五苯基吡咯的水相电化学发光体系的构建方法，相比其他有机物发光体在水相的电化学性能，五苯基吡咯水相电化学发光体系具有良好的发光性能以及高的稳定性和重现性；五苯基吡咯可作为一种新型的聚集诱导发光试剂用于电化学发光体系的构建。
附图说明
图1是PentaPP的制备示意图。
图2中的(a)、(b)分别表示PentaPP的紫外荧光表征和不同含水量的PentaPP荧光谱图。
图3中的(a)表示K2S2O8、PentaPP、PentaPP/K2S2O8分别在水相电化学发光体系中的CV图；(b)表示与(a)相对应的ECL信号强度-电位图。
图4中的(a)、(b)、(c)、(d)分别表示PentaPP/K2S2O8水相电化学发光体系的电位窗、扫描速率、pH、K2S2O8浓度等实验条件的优化图。
图5中的(a)、(b)分别表示PentaPP/K2S2O8水相电化学发光体系中PentaPP用量的浓度优化和连续扫描30圈该体系的ECL稳定性测试。
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
一种基于五苯基吡咯的水相电化学发光体系的构建方法，步骤如下：
1)PentaPP的制备
取二苯乙炔(0.5mmol)，苯胺(0.25mmol)，氯化亚铜(1mmol)，碳酸钠(0.25mmol)和氯化钯(0.025mmol)置于10mL的圆底烧瓶中，加入2mL干燥的1,4-二氧六环。首先，抽真空通氮气三次，将其密封回流6h，通过点板观察反应是否完全，完全反应后将残渣溶于***中，用水洗(3×15mL)后用无水硫酸钠干燥，之后过滤将滤液旋干后过柱纯化(二氯甲烷/正己烷，1:20)，最终获得白色固体粉末。
(2)将裸的玻碳电极依次用0.3μm和0.05μm的三氧化二铝粉打磨抛光，然后用二次蒸馏水冲洗，最后用氮气吹干后待用。
(3)称取PentaPP 4.47mg，溶解于1mL的DMF中，配制成10mmol/L的储备液。
(4)取步骤(3)配制的PentaPP储备液10uL，将其加入到5mLpH＝7.0的磷酸盐缓冲液(含0.1mol/L的K2S2O8)中，最后将裸的玻碳电极、铂柱电极和Ag/AgCl电极分别作为工作电极、对电极与参比电极浸入到磷酸盐缓冲溶液中。
体系构建好后用MPI-A型毛细管电泳-电化学发光分析仪(购买于西安瑞迈分析仪器有限责任公司)进行检测。电化学发光分析仪的光电倍增管偏压设置为800V，扫速为0.1V·s-1，电势窗为-1.7～-0.1V。
由图3可知，PentaPP/K2S2O8体系的还原峰电位更低其更易于发生氧化还原反应，具有良好的电致化学发光性能。
由图5可知，PentaPP/K2S2O8水相电化学发光体系连续扫描30圈稳定性测试中其相对标准偏差为0.03％，表明其具有优良的稳定性。
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 (3)

1.一种基于五苯基吡咯的水相电化学发光体系的构建方法，其特征在于，将电化学发光试剂五苯基吡咯溶解于N,N-二甲基甲酰胺中，得五苯基吡咯溶液，以K2S2O8作为体系的共反应剂，将五苯基吡咯溶液加入含有K2S2O8的磷酸盐缓冲溶液中，得电化学发光试剂溶液，然后将裸的玻碳电极、铂柱电极和Ag/AgCl电极分别作为工作电极、对电极与参比电极浸入到电化学发光试剂溶液中。
2.根据权利要求1所述的基于五苯基吡咯的水相电化学发光体系的构建方法，其特征在于，所述五苯基吡咯溶液中五苯基吡咯的浓度为10mmol/L，所述磷酸盐缓冲溶液的pH值为7.0，含有0.1mol/L的K2S2O8，五苯基吡咯在磷酸盐缓冲溶液中的浓度为2×10-5mmol/L。
3.根据权利要求1或2所述的基于五苯基吡咯的水相电化学发光体系的构建方法，其特征在于，体系构建好后用毛细管电泳-电化学发光分析仪进行检测，电化学发光分析仪的光电倍增管偏压设置为800V，扫速为0.1V·s-1，电势窗为-1.7～-0.1V。
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