新型荧光试剂1-(8-喹啉)-3-(3,5-二溴-2-吡啶)-三氮烯的合成及其应用

Synthesis of a New Fluorescence Reagent-1-(8-Quinoline)-3-(3,5-Dibromo-pyridine)-Triazene and Its Analytical Application

将具有荧光特性的杂环8-氨基喹啉和吡啶类试剂结合,并引入三氮烯结构,合成了新型荧光试剂1-(8-喹啉)-3-(3,5-二溴-2-吡啶)-三氮烯(QBPyT)。其结构经元素分析、红外光谱、核磁共振波谱证实。研究结果表明,在pH 9.5硼酸-氢氧化钠缓冲溶液的介质存在下,该试剂在λex/λem=248nm/496nm处产生强荧光,并且能与铅(Ⅱ)形成配合物从而使荧光增强。据此建立了三氮烯测定铅(Ⅱ)的新型荧光分析法。铅的浓度在5.0×10-7～1.2×10-5 mol.L范围内与其荧光强度呈线性关系,检出限(3S/N)为9.5×10-8 mol.L。将其应用于水样中铅(Ⅱ)的测定,测得回收率在92.6%～94.0%之间,测定值的相对标准偏差(n=5)小于3.5%。

By connecting the triazene structure with the heterocyclic fluorescent reagents of quinoline and pyridine,a new fluorescence reagent of 1-（8-quinoline）-3-（3,5-dibromo-pyridine）-triazene（QBPyT） was synthesized and identified by elemental analysis,IRS and NMR.Strong fluorescence at the wavelengths of 248 nm（λex） and 496 nm（λem） was emitted by this reagent in a borate buffer medium of pH 9.5,and an enhancement of fluorescence was observed in the presence of Pb（Ⅱ） ion due to the formation of a coordination complex between Pb（Ⅱ） and QBPyT.Linear relationship between the magnitude of increase in fluorescence intensity and concentration of Pb（Ⅱ） was obtained in the range of 5.0×10-7-1.2×10-5mol·L with detection limit（3S/N） of 9.5×10-8mol·L.The proposed method was used in the analysis of water samples,giving RSD′s（n=5） less than 3.5%,and using these samples as matrixes,recovery was tested,the values of recovery found were ranged from 92.6% to 94.0%.