Synthesis of N-9-Acridinyl-α-aminoacetic Acid and Its Use as Probe in the Fluorospectrophotometric Determination of Traces of Copper
摘 要
对荧光探针N-9-吖啶-α-氨基乙酸的合成方法作了改进,使偶氮化反应时间由7 h缩短为3 h,产率由78.9%提高至85.2%.此试剂与铜(Ⅱ)反应使其荧光猝灭,并据此提出了以此试剂为探针的痕量铜的荧光光度测定法.在pH 7.0的缓冲介质中,在一定量的乙醇存在下,铜(Ⅱ)与荧光探针反应,通过测定样品溶液和空白溶液在激发波长(λex) 262.0 nm和发射波长(λem) 456.0 nm的荧光强度FA和FB,计算得反应液荧光强度猝灭程度ΔF,其荧光强度的猝灭程度与铜(Ⅱ)质量浓度在0.20~600.0 μg·L-1范围内呈线性关系,方法的检出限(3σ/b)为0.04 μg·L-1.按此方法分析了3个环境水样,测得其铜量值的相对标准偏差(n=6)均小于2.5%,回收率在96.0%~102.0%之间.
Abstract
Synthesis of the fluorescence reagent,N-9-acridinyl-α-aminoacetic acid,was improved,resulting a decrease of time for diazotization from 7 h to 3 h,and an increase of yield from 78.9% to 85.2%.Fluorescence quenching effect was observed when the new reagent was reacted with Cu(Ⅱ).The use of the reagent as a fluorescence probe in the determination of trace amounts of copper was proposed.In a buffer solution of pH 7.0,Cu(Ⅱ) was reacted with the fluorescence reagent in the presence of ethanol,the magnitude of derease in fluorescence intensity (ΔF) of the reaction solution was measured at the wavelengths of (λex) 262.0 nm and (λem) 456.0 nm by taking the difference between emission fluorescence intensity of the blank solution FB and the sample solution FA.Linear relationship between values of ΔF and concentration of Cu(Ⅱ) was found in the range of 0.20-600.0 μg·L-1,with its detection limit (3σ/b) of 0.04 μg·L-1.Values of RSD′s (n=6) and recovery found in the analysis of 3 samples of environmental water,were less than 2.5% and in the range of 96.0%-102.0%.
中图分类号 O657.3
所属栏目 试验与研究
基金项目 安徽省高校青年教师科研资助项目(No:2005jq1161)和皖西学院应用项目(No:WXZY0709)
收稿日期 2008/4/6
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备注严正权(1971-),男,安徽六安人,讲师,硕士,主要从事有机试剂合成及应用研究.
引用该论文: YAN Zheng-quan,HU Lei,ZHOU Yun-you. Synthesis of N-9-Acridinyl-α-aminoacetic Acid and Its Use as Probe in the Fluorospectrophotometric Determination of Traces of Copper[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(4): 387~389
严正权,胡蕾,周运友. 荧光探针N-9-吖啶-α-氨基乙酸的合成及荧光分光光度法测定环境水样中痕量铜[J]. 理化检验-化学分册, 2009, 45(4): 387~389
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【3】WANG R,HOSAKA M,HAN L,et al.Molecular probes for sensing the cholesterol composition of subcellular organelle membranes[J].Biochimica & Biophysica Acta (BBA)-Molecular and Cell Biology of Lipids,2006,61(10):1169-1181.
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