Simultaneous determination of carbamate insecticides and mycotoxins in cereals by reversed phase liquid chromatography tandem mass spectrometry using a quick, easy, cheap, effective, rugged and safe extraction procedure

A simple, sensitive and reliable analytical method was developed for the simultaneous determination of 22 carbamate insecticides and 17 mycotoxins in cereals by ultra high performance liquid chromatography electrospray ionization tandem mass spectrometry (UHPLC–ESI-MS/MS). Carbamates and mycotoxins were extracted from cereal samples using a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) procedure without any further clean-up step. The extract was diluted with water containing 0.1% formic acid and 5.0 mM ammonium acetate, and analyzed by LC–MS/MS on a Waters Acquity BEH C18 column with water (0.1% formic acid, 0.50 mM ammonium acetate)/methanol as mobile phase with gradient elution. Matrix-matched calibration was used for quantification. Blank samples (rice, wheat and corn) were fortified at 5, 10 and 50 μg/kg except for five zearalenonic compounds at 25, 50 and 250 μg/kg, and recoveries were in the range of 70–120%. Relative standard deviations were lower than 20% in all cases. The LOQ values were in the range of 0.20–29.7 μg/kg. The method is suitable for the simultaneous determination of carbamate insecticides and mycotoxins in cereals. The total time required for the analysis of one sample, including sample preparation, was about 35 min.

► A LC–MS/MS method was developed for 22 carbamates and 17 mycotoxins in cereals.
► A simple pretreatment procedure based on QuEChERS has been established.
► Selectivity, linearity, trueness, precision, LOD, and LOQ had been validated.
► The whole method was fast, reliable, convenient and sensitive.