Synthesis of 3-Mehoxy-4-hydroxybenzaldehyde-2-hydrazinobenzoic Acid and Its Fluorescence Quenching Reaction with Silver Ion
摘 要
合成了一种新的荧光试剂3-甲氧基-4-羟基苯甲醛-2-肼基苯甲酸(香草醛缩邻肼基苯甲酸),并用红外光谱法及元素分析法对其分子结构作了验证.试验发现:在pH 5.1的乙酸盐缓冲介质中,上述新试剂在激发波长为308.8 nm时,在476.8 nm波长处出现发射荧光峰,而当在此条件下加入银离子时,由于两者相互反应生成络合物而导致试剂发生荧光猝灭现象,其荧光强度的减弱程度(ΔF)与银离子的质量浓度在3.0~160 μg·L-1范围内呈线性关系.测得此反应对Ag+离子的检出限(3S/N)为0.28 μg·L-1.据此,提出了测定痕量银的新方法.用标准加入法测得方法的回收率在98.3%~103.3%之间.
Abstract
A new fluorescence reagent,3-mehoxy-4-hydroxybenzaldehyde-2-hydrazinobenzoic acid (MHBHBA) was synthesized and its molecular structure was identified by IR-spectrometry and elementary analysis.It was found that in an acetate buffer of pH 5.1,the new reagent,MHBHBA reacted with Ag+ ion to form a stable complex,leading to quenching of fluorescence of the reagent,and that the magnitude of fluorescence quenching of MHBHBA kept linear relationship with mass concentration of Ag+ ion in the range of 3.0-160 μg·L-1,when measured at the wavelengths of (λex) 308.8 nm and (λem) 476.8 nm.Detection limit (3S/N) found was 0.28 μg·L-1.Based on these facts,method for determination of trace amount of silver was proposed.Recovery of the method was tested by standard addition method,giving values of recovery ranged from 98.3% to 103.3%.
中图分类号 O657.31
所属栏目 工作简报
基金项目 甘肃省教育厅科研基金项目(No.0710B-03)
收稿日期 2008/10/29
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备注仵博万(1970-),男,甘肃庆阳人,副教授,从事新型偶氮试剂的合成与应用研究.
引用该论文: WU Bo-wan,LIU Jian-ning. Synthesis of 3-Mehoxy-4-hydroxybenzaldehyde-2-hydrazinobenzoic Acid and Its Fluorescence Quenching Reaction with Silver Ion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(11): 1336~1338
仵博万,刘建宁. 香草醛缩邻肼基苯甲酸的合成及其与银的荧光猝灭反应[J]. 理化检验-化学分册, 2009, 45(11): 1336~1338
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【2】江崇球,王敬政,许秀芳,等.β-环糊精增敏邻羟基萘醛水杨酰腙-锶荧光反应及其应用[J].分析化学,1998,26(2):129-132.
【3】刘建宁,张兵,仵博万,等.双-(2,4-二羟基苯乙酮)缩肼的合成及其与锶的荧光猝灭反应[J].分析化学,2004,32(5):652-656.
【4】刘建宁,张兵,仵博万,等.2,3,4-三羟基苯乙酮缩-2-羧基苯胺与铜的高灵敏度荧光反应及其应用[J].分析化学,2004,32(7):919-922.
【5】仵博万,李惠成,刘建宁.新试剂4-羟基苯乙酮缩-2-氨基苯甲酸高灵敏荧光猝灭测定食品中痕量锌[J].食品工业科技,2007,28(9):201-202.
【6】陈国珍,黄贤智,许金钩.荧光分析法[M].2版.北京:科学出版社,1990:115-119.
【7】李彬,魏新军.催化荧光法测定超痕量银的研究[J].分析试验室,1998,17(2):68-70.
【8】王亮,胡秋芬,杨光宇,等.在线固相萃取富集反相液相色谱法测定水中的铅、镉、汞、银[J].分析化学,2004,32(4):421-424.
【9】YE Ying-zhi,MAO Hong-yan,CHEN Ya-hua.Catalytic kinetic simultaneous determination of iron,silver and manganese with the Kalman filter by using flow injection analysis stopped-flow spectrophotometry[J].Talanta,1998,45(6):1123-1129.
【10】黄晓东,陈美珠.阴离子表面活性剂增溶催化光度法测定痕量银[J].分析化学,2004,32(2):268.
【11】刘传湘,廖力夫.亚硝酸-亚砷酸-碘体系阻抑动力学光度法测痕量银[J].南华大学学报:理工版,2002,16(3):67-72.
【12】林志芬,郑肇生.以Triton X-100作增敏剂催化光度法测定痕量银[J].分析化学,2000,28(3):326-329.
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