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采用胶束液相色谱法测定废水和土壤中的敌草隆、特丁津和特丁净。

Determination of diuron, terbuthylazine, and terbutryn in wastewater and soil by micellar liquid chromatography.

作者信息

Pitarch-Andrés Susana, Roca-Genovés Pasqual, Peris-Vicente Juan, Esteve-Romero Josep

机构信息

Departamento de Química Física i Analítica, ESTCE, Universitat Jaume I, Campus de Riu Sec, 12071, Castelló, Spain.

出版信息

Anal Bioanal Chem. 2017 Mar;409(8):2037-2049. doi: 10.1007/s00216-016-0151-3. Epub 2016 Dec 27.

Abstract

An analytical method for the quantification of the herbicides and algaecides diuron, terbuthylazine, and terbutryn in wastewater and soil by micellar liquid chromatography was developed. The sample preparation was expedited to reduce the number of intermediate steps and the use of chemicals. The analytes in soils were recovered by ultrasonication in the mobile phase. The obtained supernatant and the water samples were directly injected, thus avoiding intermediate steps. The chromatographic behavior of the analytes, depending on the surfactant and alcohol was studied, in order to optimize the chromatographic run, by a chemometrical approach. The herbicides were resolved in <16 min using a C18 column and a mobile phase of 0.07 M sodium dodecyl sulfate/6% 1-pentanol phosphate buffered at pH 3, running under isocratic mode at 1 mL/min. The detection absorbance wavelength was set to 240 nm. The method was successfully validated in terms of selectivity, detection limit (0.06 mg/L in water and 0.3 mg/kg in soil), quantitation range (0.2-2 mg/L in water and 1-10 mg/kg in soil), trueness (-6.1 to +5.0%), precision (<9.4%), and ruggedness (<8.3%). The procedure was reliable, practical, easy-to-handle, available, short-time and ecofriendly and useful for routine analysis. Its applicability to real samples was evaluated by analyzing several wastewater, decorative reservoir, and soil samples from agricultural and urban sources.

摘要

建立了一种胶束液相色谱法,用于定量分析废水和土壤中的除草剂及除藻剂敌草隆、特丁津和特丁净。加快了样品制备过程,以减少中间步骤的数量和化学试剂的使用。土壤中的分析物通过在流动相中超声处理进行回收。将获得的上清液和水样直接进样,从而避免中间步骤。通过化学计量学方法研究了分析物在不同表面活性剂和醇类条件下的色谱行为,以优化色谱分析。使用C18柱和pH值为3的0.07 M十二烷基硫酸钠/6% 1-戊醇的磷酸盐缓冲流动相,在等度模式下以1 mL/min的流速运行,除草剂在<16分钟内实现分离。检测吸光度波长设定为240 nm。该方法在选择性、检测限(水中0.06 mg/L,土壤中0.3 mg/kg)、定量范围(水中0.2 - 2 mg/L,土壤中1 - 10 mg/kg)、准确性(-6.1%至+5.0%)、精密度(<9.4%)和耐用性(<8.3%)方面均成功得到验证。该方法可靠、实用、易于操作、可行、耗时短且环保,适用于常规分析。通过分析来自农业和城市来源的多个废水、景观蓄水池及土壤样品,评估了该方法对实际样品的适用性。

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