Molecularly imprinted solid phase extraction method for simultaneous determination of seven nitroimidazoles from honey by HPLC-MS/MS.

ABSTRACT

In this work, a selective sample cleanup procedure that combined molecular imprinting technique with solid phase extraction was developed for the simultaneous extraction of the seven nitroimidazoles (NMZs) from honey samples. The molecular imprinting polymers for NMZs were prepared through bulk polymerization method using 2-methyl-5-nitroimidazole as template molecule, methacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross linking agent. The obtained molecular imprinting polymers showed high affinity to template molecule and was used as selective sorbent for simultaneously selective extraction of the seven NMZs from honey matrix. An off-line molecularly imprinted solid phase extraction (MISPE) method followed by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) for simultaneous determination of the seven NMZs from honey samples was also established. The proposed method was validated at 1.0, 2.0 and 10.0µg/kg, obtaining recoveries in the range of 79.7-110%, with repeatability and interday precision values (expressed as relative standard deviation) ≤11.4% and ≤15.2%, respectively. Limits of quantification for different NMZs were 1.0µg/kg, which were always below the minimum required performance limits established by the European Community Reference Laboratories (Commission Decision 2002/657/EC). It was demonstrated that this proposed MISPE-HPLC-MS-MS method could be applied to direct determination of NMZs from honey samples.