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Determination of carbamates in soils by liquid chromatography coupled with on-line postcolumn UV irradiation and chemiluminescence detection
Arabian Journal of Chemistry ( IF 5.3 ) Pub Date : 2020-01-01 , DOI: 10.1016/j.arabjc.2018.07.008
José A. Murillo Pulgarín , Luisa F. García Bermejo , Armando Carrasquero Durán

Abstract In this study, high performance liquid chromatography (HPLC) coupled with a simple and fast sample pre-treatment based on the use of the UV-irradiation in a simple continuous flow system for the chemiluminescent quantification of pesticide carbamates in soils was developed and validated. HPLC was used to separate thiodicarb, bendiocarb and carbaryl in soil extracts. The eluates emerging from the column tail were mixed with an alkaline solution of Co2+ in EDTA and irradiated with UV light to induce photolysis of the carbamates, in order to obtain free radicals and other reactive species capable of oxidizing luminol and producing photoinduced chemiluminescence (PICL) as a result. Measurements of CL intensity were plotted as a function of time to obtain chromatographic peaks. Under the optimum operating conditions for the combined HPLC-PICL system, CL peak areas were linearly related to analyte concentrations. The limit of detection were 0.05 mg L−1 for thiodicarb, 0.09 mg L−1 for bendiocarb and 0.17 mg L−1 for carbaryl. A simple extraction procedure using 98% methanol as solvent ensured complete dissolution of the analytes in spiked soils with recoveries from 87 to 120%. The proposed method is a simple, fast, accurate choice for quantifying the target pesticides in soils.

中文翻译:

液相色谱-柱后紫外照射在线化学发光检测法测定土壤中的氨基甲酸酯

摘要 在本研究中,开发并验证了高效液相色谱 (HPLC) 与简单快速的样品前处理相结合,该方法基于在简单连续流动系统中使用紫外线照射进行土壤中农药氨基甲酸酯的化学发光定量。 . HPLC 用于分离土壤提取物中的硫双威、苯菌威和甲萘威。从柱尾流出的洗脱液与 EDTA 中的 Co2+ 碱性溶液混合,并用紫外线照射以诱导氨基甲酸酯的光解,以获得能够氧化鲁米诺并产生光致化学发光 (PICL) 的自由基和其他活性物质因此。CL 强度的测量被绘制为时间的函数以获得色谱峰。在组合 HPLC-PICL 系统的最佳操作条件下,CL 峰面积与分析物浓度呈线性相关。硫双威的检测限为 0.05 mg L-1,苯菌威为 0.09 mg L-1,西维因为 0.17 mg L-1。使用 98% 甲醇作为溶剂的简单萃取程序可确保分析物在加标土壤中完全溶解,回收率为 87% 至 120%。所提出的方法是量化土壤中目标农药的一种简单、快速、准确的选择。
更新日期:2020-01-01
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