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

Abstract EN

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.