Determination of Nitroimidazoles and Their Metabolites Residues in Honey by TurboFlow Online Purification-Ultra Performance Liquid Chromatography-Tandem Mass Sepctrometry and Istopes Dilution Technique / 分析化学

ABSTRACT

A TurboFlow ( TF ) online purification-ultra performance liquid chromatography-tandem mass spectrometric method was developed for the determination of nitroimidazoles and their metabolites ( ornidazole, IPZ, MNZ, MNZOH, DMZ, RNZ, IPZOH and HMMNI) in honey. The honey sample was extracted by H2 O containing 0. 1% formic acid solution. Then, the extraction solution was analyzed by TF-UPLC-MS/MS. The main factors influencing the purification efficiency including TF column, mobile phases and elution solutions were optimized. The compounds were detected by selective reaction monitoring ( SRM) in positive ion mode electrospray ionization ( ESI+) . The linear range of the method ranged from 0 . 1 to 50μg/L for nitroimidazoles and their metabolites, with the correlation coefficient ( R2 ) of over 0. 997. The limits of quantification were 0. 1 μg/kg for ornidazole, IPZ, 0. 2 μg/kg for MNZ, MNZOH, DMZ, RNZ and IPZOH, and 1. 0 μg/kg for HMMNI, respectively. The recoveries were in the range of 73. 7% to 116. 4% at four spiked levels with the relative standard deviations ranged from 1. 1% to 9. 1% in honey samples. The results indicate that the developed method is simple, efficient and precise, and can be used for the determination of nitroimidazoles and their metabolites in the actual honey samples.