Confirmatory Analysis of Nitroimidazoles and Hydroxy Metabolites in Honey by Dispersive-Solid Phase Extraction and Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

• Main Authors: Xiaowei Li, Yuebin Ke, Yingyu Wang, Chengfei Wang, Dongyang Ye, Xue Hu, Lan Zhou, Xi Xia
• Format: Article
• Language: English
• Published: MDPI AG 2018-12-01
• Series: Molecules
• Subjects: nitroimidazole; honey; liquid chromatography; mass spectrometry; d-SPE
• Online Access: https://www.mdpi.com/1420-3049/23/12/3350

An ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry (UHPLC-MS/MS) method was developed and validated for confirmatory analysis of four nitroimidazoles and three hydroxy metabolites in honey. Honey samples were dissolved in 2% formic acid solution and nitroimidazoles and metabolites were isolated and enriched by dispersive-solid phase extraction using mixed-mode strong cation-exchange sorbent. The determination involves separation of analytes on an UHPLC C₁₈ column and detection by multiple reaction monitoring in positive ionization mode. The recovery of the method was ranged from 90.2 to 105.6% with inter-day relative standard deviations of less than 11.2%. The limits of detection and limits of quantification were in the ranges of 0.02⁻0.07 µg/kg and 0.05⁻0.2 µg/kg, respectively. Honey samples from the market were analyzed to demonstrate the applicability of the proposed method.