Development and application of kinetic-spectrophotometric method for analysis of diflubenzuron in soil samples using SPE followed by HPLC method

Emilija T. Pecev-Marinković, Ana S. Miletić, A. Pavlović, V. Dekić
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Abstract

The purpose of this paper is to present a new sensitive and simple kinetic-spectrophotometric method for the determination of the insecticide diflubenzuron (DFB). The kinetic method is based on the inhibition effect of DFB on the oxidation of sulfanilic acid (SA) by potassium periodate in acetate buffer in the presence of Fe(III) ion as a catalyst and 1,10-phenantroline. The reaction was monitored spectrophotometrically by measuring the increase in absorbance with time of the reaction product at 368 nm. Diflubenzuron was determined with linear calibration graph in the interval from 0.0374 to 0.374 μg/cm3 and from 0.374 to 26.18 μg/cm3. The detection limit and quantification limit of the method with 3σ criteria were 0.0039 μg/cm3 and 0.0131 μg/cm3, respectively. The relative standard deviations for five replicate determinations of 0.0374, 0.188 and 0.374 μg/cm3 DFB were 2.24, 2.11 and 1.10%, respectively. The method was successfully applied to determine DFB residues in soil samples. Solid-phase extraction (SPE) was used for extraction of DFB from soil and samples with Chromabond® (Macherey-Nagel) C18 cartridges. The HPLC method was used as a comparative method to verify the results. The results obtained by two different methods showed good agreement.
固相萃取-高效液相色谱动力学分光光度法分析土壤样品中氟虫脲的建立及应用
建立了一种灵敏简便的动态分光光度法测定杀虫脲(DFB)的新方法。动力学方法是基于DFB对醋酸缓冲液中高碘酸钾在Fe(III)离子和1,10-phenantroline存在下氧化磺胺酸(SA)的抑制作用。用分光光度法测定了反应产物在368nm处吸光度随时间的增加。在0.0374 ~ 0.374 μg/cm3和0.374 ~ 26.18 μg/cm3范围内,采用线性标定图对氟苯脲进行测定。方法的检出限为0.0039 μg/cm3,定量限为0.0131 μg/cm3。0.0374、0.188和0.374 μg/cm3 DFB 5个重复测定的相对标准偏差分别为2.24、2.11和1.10%。该方法成功地应用于土壤样品中DFB残留量的测定。采用固相萃取(SPE)技术,用Chromabond®(machery - nagel) C18萃取筒从土壤和样品中提取DFB。采用高效液相色谱法对结果进行对比验证。两种方法的测定结果一致。
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