Method Optimization: Analysis of Benzbromarone and Tolfenamic Acid in Citrus Tissues and Soil Using Liquid Chromatography Coupled With Triple-Quadrupole Mass Spectrometry

Abstract

Herein, an analytical method was developed for extraction and quantification of benzbromarone and tolfenamic acid in citrus and soil matrices using liquidliquid extraction followed by liquid chromatography-triple quadrupole-tandem mass spectrometry analysis. The compounds were extracted using 0.1% formic acid in 6:4 ethyl acetate and n-hexane solution, and the analytes were separated using a mixture of 0.1% formic acid in ultrapure water and 0.1% formic acid in acetonitrile as mobile phase. A six-point in-matrix calibration curve was constructed providing good linearity with coefficients of determination R 2 ≥ 0.98. The limits of detection and quantification for benzbromarone and tolfenamic acid were 3.0 and 10.0 µg/kg in roots, peel, juice, and soil, and 4.0 and 12.0 µg/kg for leaves samples, respectively. The method yielded excellent recoveries between 81.3 and 101.2%, with relative standard deviation ≤9.5% in the matrices. The developed technique provides a simple and sensitive method for the determination of the chemicals and can be applied to agricultural practices.