Abstract:

A method was established for the determination of nitrofuran metabolite residues in bee pollen by liquid
chromatography-tandem mass spectrometry (LC-MS-MS). After acidified, samples were purified through HLB solid phase
extraction columns, derivatized, and then extracted with ethyl acetate. The extracted residues were analyzed by mass
spectrometry. The recoveries of nitrofuran metabolites ranged from 89.5% to 100.9% at spiked concentrations of 1, 2 μg/kg.
and 5 μg/kg. The method showed good precisions for intra-day (RSD ＜ 10%) and inter-day assays (RSD ＜ 15%), and had
an excellent linearity in the range from 0.5 to 20 ng/mL (r ＞ 0.99). The detection limit and quantitation limit were 0.25 μg/kg.
and 1.0 μg/kg, respectively. This validated method is suitable for the determination and confirmation of nitrofuran metabolite
residues in bee pollen thanks to its excellent selectivity and strong anti-interference capability.

Key words: bee pollen, nitrofuran metabolites, liquid chromatography-tandem mass spectrometry (LC-MS-MS), solid phase extraction (SPE)