UHPLC/MS-MS Analysis of Six Neonicotinoids in Honey by Modified QuEChERS: Method Development, Validation, and Uncertainty Measurement

Abstract

Rapid and reliable multiresidue analytical methods were developed and validated for the determination of 6 neonicotinoids pesticides (acetamiprid, clothianidin, imidacloprid, nitenpyram, thiacloprid, and thiamethoxam) in honey. A modified QuEChERS method has allowed a very rapid and efficient single-step extraction, while the detection was performed by UHPLC/MS-MS. The recovery studies were carried out by spiking the samples at two concentration levels (10 and 40 μg/kg). The methods were subjected to a thorough validation procedure. The mean recovery was in the range of 75 to 114% with repeatability below 20%. The limits of detection were below 2.5 μg/kg, while the limits of quantification did not exceed 4.0 μg/kg. The total uncertainty was evaluated taking the main independent uncertainty sources under consideration. The expanded uncertainty did not exceed 49% for the 10 μg/kg concentration level and was in the range of 16–19% for the 40 μg/kg fortification level.