Development of a simple method to quantify fipronil and its intermediates in soil.
Development of a simple method to quantify fipronil and its intermediates in soil.
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DOI：
10.1039/d0ay00924e
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发表时间：
2020-07
期刊：
影响因子：
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通讯作者：
Rafaella Tomazini;G. Grosseli;Diana Nara Ribeiro de Sousa;P. Fadini;Flávia Talarico Saia;A. Langenhoff;B. M. van der Zaan;A. A. Mozeto-A.
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文献类型：
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作者：
Rafaella Tomazini;G. Grosseli;Diana Nara Ribeiro de Sousa;P. Fadini;Flávia Talarico Saia;A. Langenhoff;B. M. van der Zaan;A. A. Mozeto-A.
建立了一种简便、重现性好的同时测定土壤中农药氟虫腈及其中间体氟虫腈、氟虫腈和氟虫腈硫化物的方法。采用超声波法提取样品，以三中心Box-Behnken设计优化溶剂比(己烷/丙酮)、循环次数和循环时间。通过响应面分析，确定了最佳提取条件。净化步骤由含有二氧化硅(Florisil®)和氧化铝的固相萃取柱(SPE)进行。采用气相色谱-电子捕获检测法(GC-ECD)对氟虫腈及其中间体进行分离，分离时间为20min。最佳定量条件为1：1(v/v)丙酮/正己烷，超声周期2次，每次15min。回收率在81~108%之间，相对标准偏差(RSD)小于6%，不受所用基质的影响。分析曲线的回归系数值在0.9908以上，浓度范围为0.005~0.6μg g-1。所有分析物的检出限均在0.002~0.006μg g-1之间，定量限在0.006~0.020μg g-1之间。该方法可用于土壤中氟虫腈及其中间体的监测和定量。
A simple and reproducible method was developed and validated for simultaneous quantification of the pesticide fipronil and its intermediates fipronil desulfinyl, fipronil sulfone and fipronil sulfide, in soil. The analytes were extracted by ultrasonic bath and the ratio of solvents (hexane/acetone), number and time of cycles were optimized by Box-Behnken design with a triplicate central point. The optimal extraction conditions were achieved through a response surface analysis. The clean-up step was conducted by cartridges of solid phase extraction (SPE) containing silica (Florisil®) and aluminum oxide. Gas chromatography with electron capture detection (GC-ECD) was employed for separating fipronil and its intermediates with a suitable resolution and runtime of 20 minutes. The best quantification was achieved with 1 : 1 (v/v) acetone/hexane and 2 ultrasound cycles of 15 minutes each. The recovery values were between 81 to 108%, with relative standard deviation (RSD) lower than 6%, with no effect of the used matrix. Analytical curves presented regression coefficients values above 0.9908 for a concentration range from 0.005 to 0.6 μg g-1. Limits of detection (LOD) from 0.002 to 0.006 μg g-1 and limits of quantification (LOQ) from 0.006 to 0.020 μg g-1 were reached for all analytes. This method can be used to monitor and quantify fipronil and its intermediates in soil.