用于农药测定的芬顿试剂验证中的干扰建模、实验设计和预浓缩步骤。
Interference modelling, experimental design and pre-concentration steps in validation of the Fenton's reagent for pesticides determination.
作者信息
Ostra Miren, Ubide Carlos, Zuriarrain Juan
机构信息
Departamento de Química Aplicada, Facultad de Química, Universidad del País Vasco, Apdo. 1072, 20080-San Sebastián, Spain.
出版信息
Anal Chim Acta. 2007 Feb 12;584(1):228-35. doi: 10.1016/j.aca.2006.11.028. Epub 2006 Nov 12.
The determination of atrazine in real samples (commercial pesticide preparations and water matrices) shows how the Fenton's reagent can be used with analytical purposes when kinetic methodology and multivariate calibration methods are applied. Also, binary mixtures of atrazine-alachlor and atrazine-bentazone in pesticide preparations have been resolved. The work shows the way in which interferences and the matrix effect can be modelled. Experimental design has been used to optimize experimental conditions, including the effect of solvent (methanol) used for extraction of atrazine from the sample. The determination of pesticides in commercial preparations was accomplished without any pre-treatment of sample apart from evaporation of solvent; the calibration model was developed for concentration ranges between 0.46 and 11.6 x 10(-5) mol L(-1) with mean relative errors under 4%. Solid-phase extraction is used for pre-concentration of atrazine in water samples through C(18) disks, and the concentration range for determination was established between 4 and 115 microg L(-1) approximately. Satisfactory results for recuperation of atrazine were always obtained.
实际样品（商业农药制剂和水基质）中阿特拉津的测定表明，当应用动力学方法和多元校准方法时，芬顿试剂可用于分析目的。此外，农药制剂中阿特拉津 - 甲草胺和阿特拉津 - 苯达松的二元混合物也得到了分离。这项工作展示了干扰和基质效应的建模方法。实验设计已用于优化实验条件，包括用于从样品中提取阿特拉津的溶剂（甲醇）的影响。商业制剂中农药的测定除了溶剂蒸发外无需对样品进行任何预处理；校准模型针对0.46至11.6×10⁻⁵ mol L⁻¹的浓度范围建立，平均相对误差在4%以下。固相萃取用于通过C₁₈盘对水样中的阿特拉津进行预浓缩，测定的浓度范围约为4至115 μg L⁻¹。阿特拉津的回收率始终获得令人满意的结果。
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