Residue analysis of fungicides fenpicoxamid, isofetamid, and mandestrobin in cereals using zirconium oxide disposable pipette extraction clean-up and ultrahigh-performance liquid chromatography-tandem mass spectrometry.

Abstract In the present study, a fast multiresidue method determining three novel fungicides fenpicoxamid, isofetamid, and mandestrobin in cereals was developed and validated for the first time using ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Samples were extracted by QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) methodology, and cleaned up using the disposable pipette extraction (DPX) tips containing primary secondary amine (PSA) and silica gel modified with zirconium oxide (Z-Sep) in less than 1 min. Linearity (r > 0.99) of three fungicides in the calibration range of 0.001-0.1 µg mL−1 was satisfactory. Mean recoveries (n = 15) from all matrices were between 84.8% and 100.3% as the corresponding intra-day and inter-day relative standard deviations (RSDs) were less than 10.6%. Limits of quantitation (LOQs) of all analytes in different matrices were defined at 0.01 mg kg−1. The results indicate this method can serve as a sensitive and rapid approach to monitoring contents of fenpicoxamid, isofetamid, and mandestrobin in cereals.