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Development of a simple method to quantify fipronil and its intermediates in soil.
Analytical Methods ( IF 2.7 ) Pub Date : 2020-06-08 , DOI: 10.1039/d0ay00924e Rafaella Tomazini 1 , Guilherme Martins Grosseli 1 , Diana Nara Ribeiro de Sousa 1 , Pedro Sergio Fadini 1 , Flávia Talarico Saia 2 , Alette Langenhoff 3 , Bas van der Zaan 4 , Antonio Aparecido Mozeto 1
Analytical Methods ( IF 2.7 ) Pub Date : 2020-06-08 , DOI: 10.1039/d0ay00924e Rafaella Tomazini 1 , Guilherme Martins Grosseli 1 , Diana Nara Ribeiro de Sousa 1 , Pedro Sergio Fadini 1 , Flávia Talarico Saia 2 , Alette Langenhoff 3 , Bas van der Zaan 4 , Antonio Aparecido Mozeto 1
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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.
中文翻译：
开发一种简单的方法来定量土壤中氟虫腈及其中间体。
开发了一种简单且可重现的方法，并验证了该方法可同时定量测定土壤中的农药氟虫腈及其中间体氟虫腈去亚磺酰基，氟虫腈砜和氟虫腈。通过超声浴提取分析物，并通过Box-Behnken设计以三重中心点优化溶剂的比例（己烷/丙酮），循环次数和循环时间。最佳提取条件是通过响应面分析获得的。净化步骤是通过固相萃取（SPE）滤筒进行的，该滤筒中含有二氧化硅（Florisil？）和氧化铝。气相色谱-电子捕获检测（GC-ECD）用于分离氟虫腈及其中间体，分离度合适，运行时间为20分钟。最佳定量是通过1进行的：1（v / v）丙酮/己烷和2个超声循环，每个循环15分钟。回收率在81％至108％之间，相对标准偏差（RSD）低于6％，对所用基质无影响。分析曲线显示浓度范围为0.005至0.6μgg时，回归系数值高于0.9908-1。所有分析物的检测限（LOD）为0.002至0.006μgg -1，定量限（LOQ）为0.006至0.020μgg -1。该方法可用于监测和定量土壤中氟虫腈及其中间体。
更新日期：2020-07-02
中文翻译：
开发一种简单的方法来定量土壤中氟虫腈及其中间体。
开发了一种简单且可重现的方法，并验证了该方法可同时定量测定土壤中的农药氟虫腈及其中间体氟虫腈去亚磺酰基，氟虫腈砜和氟虫腈。通过超声浴提取分析物，并通过Box-Behnken设计以三重中心点优化溶剂的比例（己烷/丙酮），循环次数和循环时间。最佳提取条件是通过响应面分析获得的。净化步骤是通过固相萃取（SPE）滤筒进行的，该滤筒中含有二氧化硅（Florisil？）和氧化铝。气相色谱-电子捕获检测（GC-ECD）用于分离氟虫腈及其中间体，分离度合适，运行时间为20分钟。最佳定量是通过1进行的：1（v / v）丙酮/己烷和2个超声循环，每个循环15分钟。回收率在81％至108％之间，相对标准偏差（RSD）低于6％，对所用基质无影响。分析曲线显示浓度范围为0.005至0.6μgg时，回归系数值高于0.9908-1。所有分析物的检测限（LOD）为0.002至0.006μgg -1，定量限（LOQ）为0.006至0.020μgg -1。该方法可用于监测和定量土壤中氟虫腈及其中间体。
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