Determination of fenobucarb residues in animal and aquatic food products using liquid chromatography-tandem mass spectrometry coupled with a QuEChERS extraction method

- Fenobucarb residues in animal and aquatic food products were determined by LC-MS/MS analysis.
- Samples were extracted with a modified QuEChERS method.
- Recovery was good when samples were extracted with 0.1% trifluoroacetic acid in acetonitrile.
- None of the market samples tested positive for fenobucarb residues.

A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method coupled with liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI+/MS-MS) was developed for quantification of fenobucarb residues in animal food products, such as porcine muscle, egg, and whole milk, and aquatic food products, such as eel, flatfish, and shrimp. Acetonitrile with the addition of 0.1% trifluoroacetic acid was employed as an extraction solvent and was compared with acetonitrile alone and 0.1% formic acid in acetonitrile. All extracted samples were purified using C18 sorbent. The best extraction efficiencies, expressed as recovery at two spiking levels equivalent to 1- and 2-times the limit of quantification (LOQ = 2 μg/kg) were achieved using 0.1% trifluoroacetic acid in acetonitrile and ranged from 61.38 to 102.21% in all matrices, with relative standard deviations (RSDs) < 13% (except for the low spiking of porcine muscle and the high spiking of whole milk, for which the RSDs were > 20%). Six-point matrix-matched calibration was used for quantification and the determination coefficients were good (R2 ≥ 0.9865). The method was verified by application to samples purchased from local markets and none of the samples tested positive. In conclusion, the developed method is simple and versatile and can be used for the routine detection of fenobucarb in different animal food products having varying protein and fat contents with satisfactory accuracy and precision.

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