Simultaneous Determination of Spiramycin,Tilmicosin,Tylosin and Kitasamycin Residues in Fishery Products by UPLC-TUV Method

An ultra high performance liquid chromatographic(UPLC) method for simultaneous determination of residues of spiramycin(SPM),tilmicosin(TIL),tylosin(TYL) and kitasamycin(KIT) in fishery products has been developed.The muscle tissue sample was extracted by acetonitrile,and the extracts were evaporated to near dryness and redissolved in 4% NaCl water solution.The extracts were defatted with hexane,and cleaned up on a HLB SPE column.The analytes was separated on ACQUITY UPLC BEH C18 with acetonitrile-25 mmol/L NH4H2PO4 solution(pH 2.5,containing 10% acetonitrile) as mobile phase at flow rate of 0.3 mL/min and column temperature of 45 ℃.The TUV detector was set at the mode of wavelength events.The external standard was used for quantitation analysis.The standard curves were linear in the range of 0.100-20.0 mg/L for all analytes with correlation coefficients of 0.998 0-0.999 4.The detection limits for spiramycin,tilmicosin,tylosin and kitasamycin were 25,25,50,75 μg/kg,respectively.The average recoveries of four analytes at spiking levels of 0.10-1.0 mg/kg ranged from 70% to 102%.The relative standard deviations were between 2.9% and 11.2%.The method could meet the requirement for simultaneously determination of spiramycin,tilmicosin,tylosin and kitasamycin residues in fishery products muscle samples.