Rapid quantitative and qualitative confirmatory method for the determination of monofluoroacetic acid in foods by liquid chromatography–mass spectrometry

Abstract

A rapid quantitative method and a qualitative confirmatory method for the determination of monofluoroacetic acid (MFA) in complex food matrices are presented. The quantitative method utilizes a water extraction, solid phase extraction clean-up and liquid chromatography–mass spectrometry (LC–MS) for determination of MFA. This method showed a high degree of specificity, detecting MFA in all of the spiked samples, while none of the unfortified samples tested positive for MFA. Spike recoveries were high in all matrices analyzed, varying from 85 to 110%, and comparable at low (2 mg/L) and high (20 mg/L) spiking levels. Repeatability tests at the low spiking levels yielded RSDs of less than 5% for all matrices analyzed. The qualitative confirmatory method developed is conceptually different from the quantitative method, ensuring that both methods would not be subject to the same interferences. The method uses the formation of the hydrazide of MFA through derivatization with 2-nitrophenylhydrazine. This derivatization is well established for the determination of carboxylic acids, but this is the first application to the determination of MFA. The derivatization yield was matrix dependent, however the limit of detection (LOD) (0.8 μg/L) was sufficient to confirm the presence of MFA in all spiked matrices. Repeatability tests at the low spiking levels yielded RSDs of approximately 7% for all matrices analyzed.