Determination of 16 Benzimidazoles and 13 Nitroimidazoles Residues in Fish and Fishery Products by UPLC-Q-Orbitrap HRMS with QuEChERS

KeyWord:quadrupole/electrostatic field orbitrap high-resolution mass spectroscopy(Q-Orbitrap-HRMS)  QuEChERS  fish and fishery products  nitroimidazole  benzimidazoles

Abstract:

      A method was developed for the simultaneous determination of 16 benzimidazoles and 13 nitroimidazoles residues in fish and fishery products using ultrahigh performance liquid chromatography quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap HRMS).The samples were extracted with ethyl acetate,then concentrated and dissolved with 30%methanol aqueous solution,and cleaned up using hexane saturated with acetonitrile,amine(NH2) sorbent and MgSO4.The separation was performed on a Thermo fisher Accucore RP-MS(100 mm¡Á2ª±1 mm£¬2ª±6 ¦Ìm) column using acetonitrile and 0ª±1%formic acid as mobile phase by gradient elution.The analytes were analyzed in Full MS/dd-MS2(TopN£½1) mode with a heated electrospray ion source(HESI),and quantified by the external standard method.The calibration curves for the 29 analytes were linear in the range of 0ª±5-400 ¦Ìg/L with correlation coefficients not less than 0ª±996 7.The average recoveries at three spiked levels in 5 kinds of product matrixes ranged from 60ª±2%to 123ª±3%with relative standard deviations(RSDs,n=6)of 0ª±1%-21ª±7%.The limits of quantitation were 0ª±5-5ª±0 ¦Ìg/kg.With the advantages of simplicity,high precision and good accuracy,the method is suitable for the rapid detection of 29 veterinary drug residues in aquatic products.