Development of QuEChERS-based extraction and liquid chromatography-tandem mass spectrometry method for quantifying flumethasone residues in beef muscle

A rapid, specific, and sensitive method based on liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM) was developed and validated to quantify flumethasone residues in beef muscle. Methods were compared between the original as well as the EN quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based extraction. Good linearity was achieved at concentration levels of 5-30 μg/kg. Estimated recovery rates at spiking levels of 5 and 10 μg/kg ranged from 72.1 to 84.6%, with relative standard deviations (RSDs) < 7%. The results of the inter-day study, which was performed by fortifying beef muscle samples (n = 18) on 3 separate days, showed an accuracy of 93.4-94.4%. The precision (expressed as relative standard deviation values) for the inter-day variation at two levels of fortification (10 and 20 μg/kg) was 1.9-5.2%. The limit of detection (LOD) and limit of quantitation (LOQ) were 1.7 and 5 μg/kg, at signal-to-noise ratios (S/Ns) of 3 and 10, respectively. The method was successfully applied to analyze real samples obtained from large markets throughout the Korean Peninsula. The method proved to be sensitive and reliable and, thus, rendered an appropriate means for residue analysis studies.

► A specific method was developed for flumethasone in beef muscles. ► LC-ESI+-MS/MS using MRM was used for confirmation and quantification. ► The method provides an adequate sensitivity and performance in beef muscles. ► This is the first report for determination of flumethasone using QuEChERS method.