Liquid Chromatography with Diode Array Detection and Tandem Mass Spectrometry for the Determination of Neonicotinoid Insecticides in Honey Samples Using Dispersive Liquid-Liquid Microextraction

The combination of solid-phase extraction with dispersive liquid-liquid microextraction (SPE-DLLME) is proposed for the determination of five neonicotinoid insecticides in honey. After a cleanup stage, the analytes were eluted using acetonitrile. DLLME was performed by injecting rapidly the acetonitrile extract into 10 mL of water containing a 10% (w/v) NaCl and 100 mu L of CHCl3. The settled organic phase obtained after centrifugation was evaporated, reconstituted in acetonitrile (ACN), and submitted to liquid chromatography (LC) with photodiode array. detection (DAD) and atmospheric pressure chemical ionization-ion trap-tandem mass spectrometry (APCI-IT-MS/MS). The matrix effect was evaluated, and quantification was carried out using external aqueous calibrations when using DAD, the matrix-matched calibration method was applied for MS/MS. Detection limits in the 0.2-1.0 and 0.02-0.13 ng/g ranges were obtained when using DAD and MS/MS, respectively. The SPE-DLLME-LC-APCI-IT-MS/MS method was applied for the analysis of different honey samples, and none was found to contain residues.