Rapid determination of nitrofuran metabolites residues in honey by ultrasonic assisted derivatization - QuEChERS - high performance liquid chromatography / tandem mass spectrometry

In this study, a method of ultrasonic assisted derivatization combined with improved QuEChERS scheme and high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was developed for the analysis of nitrofuran metabolite residues in honey samples. The optimized conditions such as ultrasonic assisted derivatization conditions, extraction methods and purification materials quantitatively obtained by matrix standard curve external standard method had finally been proved to be effective in the determination of nitrofuran metabolite residues in honey samples. In order to make the results more accurate, the matrix matched standard for isotope-labeled internal standard method was used for methodological verification. The concentration of all target substances ranged from were 0.25–20 ng/mL, with good linearity, and the correlation coefficient were 0.9999. The LOD and LOQ of the target analyte were 0.15 and 0.5 μg/kg respectively. The average recoveries of the three standards were between 1.89 % and 107.9 %. The recoveries of inter-day and intra-day tests were 96.0–100.2 % and 93.2–98.7 % respectively. The precisions of inter-day(n = 6) and intra-day(n = 6) analysis were 3.56–5.29 % and 3.09–5.13 % respectively. 85 honey samples obtained from the market were analyzed by our optimized method, of which 4 SEM and 1 AOZ were detected in 5 samples.