Simultaneous determination of three herbicides in wheat, wheat straw, and soil using a quick, easy, cheap, effective, rugged, and safe method with ultra high performance liquid chromatography and tandem mass spectrometry

Abstract

In this study, a sensitive and effective analytical method for the extraction and detection of three herbicide residues (florasulam, fluroxypyr, and halauxifen-methyl) in wheat and soil was developed. Samples were extracted with acetonitrile/water followed by salting out, dispersive solid-phase extraction cleanup, and detection using ultra high performance liquid chromatography coupled with tandem mass spectrometry. The target analytes were detected within a 5 min runtime using an ultra high performance liquid chromatography high-strength silica trifunctional column connected to an electrospray ionization source in positive mode. The method was validated in five replicates at three fortification concentrations in each matrix. Adequate pesticide quantification and identity confirmation were attained, even at the lowest concentration levels. The method showed very good accuracy and precision. Good recoveries were observed for the three herbicides and mostly ranged between 75.8 and 114.6%, with intraday relative standard deviations <6.01% and interday relative standard deviations <4.02%. The limits of quantification ranged between 0.14 and 7.68 μg/kg for each herbicide. The method was successfully applied for the simultaneous analysis of the three herbicides in actual trial samples, and the results proved that the proposed method was effective in detecting these three herbicides.