Simultaneous analysis of seven neonicotinoid pesticides in agricultural products involving solid-phase extraction and surrogate compensation using liquid chromatography-tandem mass spectrometry

This study proposes a practical and precise method for the simultaneous analysis of seven neonicotinoid pesticides in agricultural products using liquid chromatography-tandem mass spectrometry from two different approaches. First, the applicability of a cleanup cartridge, comprised of a polymer sorbent consisting of a styrene-divinylbenzene copolymer with N-containing polar groups and methacrylate, in food samples was demonstrated for the first time. Second, applying an internal standard (IS) calibration method at a lower cost was considered by changing the timing of the IS addition and selecting the minimum number of ISs by referring on the matrix effect. The proposed method resulted in excellent recoveries in all tested matrices (brown rice, grapes, and peanuts) at a spiked concentration of 0.01 mg/kg. Subsequently, a residue analysis of hagobou (young burdock) was conducted. Imidacloprid was detected at 0.02 mg/kg, and the recoveries calculated in parallel with the analysis were satisfactory.