Development of HPLC-DAD method for determination of neonicotinoids in honey

After the EU banned the use of the neonicotinoids in flowering crops that honeybees might visit, there has been an increased interest in determining the neonicotinoid residues in honeybee products such as honey. The aim of this study was to develop and optimize an HPLC-DAD analytical method with dispersive liquid-liquid microextraction (DLLME) and QuEChERS sample preparation procedures for the simultaneous analysis of seven neonicotinoids (dinotefuran, nitenpyram, thiametoxam, clothianidin, imidacloprid, acetamiprid and thiacloprid) in honey samples. The liquid chromatographic conditions were optimized by Response surface methodology with Box-Behnken design and Derringer's desirability. The optimized method was validated to fulfill the requirements of SANCO/12571/2013 standard for both sample pretreatment procedures providing results for accuracy (73.1-118.3%), repeatability (3.28-10.40%) and within-laboratory reproducibility (6.45-17.70%), limits of detection (1.5-2.5 μg kg−1) and quantification (5.0-10.0 μg kg−1) with the use of matrix-matched calibration to compensate the matrix effects. For the first time 104 honey samples from Vojvodina were analyzed. The presence of thiacloprid, imidacloprid and thiametoxam was found in a small number of samples implicating the usefulness of ongoing control of honey. Residues were confirmed by LC-MS/MS.