Development of novel reagent for Hantzsch reaction for the determination of formaldehyde by spectrophotometry and fluorometry

Development of novel reagent for Hantzsch reaction for the determination of formaldehyde by spectrophotometry and fluorometry
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DOI:
10.2116/analsci.23.413
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发表时间:
2007-04-01
影响因子:
1.6
通讯作者:
Motomizu, Shoji
Motomizu, Shoji
中科院分区:
化学4区
文献类型:
--
作者:
Li, Qiong;Sritharathikhun, Piyanete;Motomizu, Shoji

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一种新型试剂乙酰乙酰苯胺(AAA)被引入基于汉茨希反应的甲醛测定中。使用AAA实现了一种简单且高灵敏度的荧光法。使用这种试剂的主要优点是:反应在室温下进行,无需任何加热系统,基于汉茨希反应的环化产物可溶于水,并且该产物可通过分光光度法和荧光法检测。产物的最大吸收波长在368 nm处,最大激发波长和发射波长分别在370 nm和470 nm处。对该过程的几个重要实验变量进行了研究;特别是对反应温度、反应时间、试剂浓度和试剂溶液的pH进行了优化,以提高检测灵敏度。校准曲线在1×10⁻⁷ - 1×10⁻⁶ M或更高浓度范围内呈线性。基于试剂空白标准偏差的三倍计算,检测限(LOD)为2.0×10⁻⁸ M。所提出的方法被应用于环境水样中甲醛的测定。水样中常见的许多外来物质不干扰所提出方法中甲醛的测定。
A novel reagent, acetoacetanilide (AAA), was introduced to the determination of formaldehyde based on Hantzsch reaction. A simple and highly sensitive fluorometric method was achieved by using AAA. The main advantages in the use of this reagent are: the reaction is carried out at room temperature without any heating system, the cyclization product based on Hantzsch reaction is soluble in water, and the product can be detected by spectrophotometry and fluorometry. The maximum absorption wavelength of the product occurs at 368 nm, and the maximum excitation and emission wavelengths are found at 370 and 470 nm, respectively. Several important experimental variables of the procedures were examined; particularly, the reaction temperature, reaction time, concentrations of reagents, and pH of the reagent solution were optimized for improving the detecting sensitivity. The calibration graph was linear in the range of 1 x 10(-7) -1 X 10(-6) M or much higher concentrations. The limit of detection (LOD), based on three times of the standard deviation of the reagent blank, was 2.0 x 10(-8) M. The proposed method was applied to the determination of formaldehyde in environmental water samples. Many foreign species commonly existing in water samples did not interfere with the determination of formaldehyde in the proposed method.