Method validation, dissipation and residue status of fluopicolide and fosetyl-aluminium in citrus using a rapid extraction method coupled with ultra-performance liquid chromatography-tandem mass spectrometry.

Abstract

The dissipation and residue status of a combination of fluopicolide and fosetyl-aluminium (fosetyl-Al) in citrus were evaluated in an experimental field. An efficient and sensitive liquid chromatography-tandem mass spectrometry, with rapid extraction, was carried out according to the SANTE guidelines. During the method validation, the recovery was within the range of 106.1-117.5, 94.4-115 and 85.4-109.5%, for fluopicolide, its metabolite 2,6-dichlorobenzamide and fosetyl-Al, respectively, with a relative standard deviation (RSD) of 0.3-10.6%. As a result, accuracy and precision at the spiking concentrations of 0.01, 0.05 and 0.10mg/kg in citrus were within the acceptable range of 70-120% with an RSD of 20%. The amount of the deposits of fluopicolide, 2,6-dichlorobenzamide and fosetyl-Al was less than the limit of quantification (LOQ) at 0.01 mg/kg at 0 day, adhering to the application in standard [1.77 + 2.66 g of active ingredient (a.i.)/L] and double (3.54 + 5.32 g a.i./L) doses. The present study proposes that the utilisation of fluopicolide and fosetyl-Al in citrus and the soil may not pose a health or environmental hazard provided that good agricultural practices are followed.