International Journal of Clinical Research

Objective To establish a method for the simultaneous determination of florfenicol and florfenicol amine residues in eggs and chicken by UPLC-MS/MS with automatic solid phase extraction. Methods The samples were diluted with water, extracted with ammonia-ethyl acetate (3:100), and the resulting extracts were clean-up on C18 solid phase extraction column,and then eluted with 100% methanol. The target components were separated on a ACQUITY UPLC ® Ben C18 column (2.1mm * 100mm, 1.7μm) , with 0.02% ammonia water and acetonitrile as mobile phase. Multiple reaction monitoring in positive and negative mode were used，and it quantified by the internal standard calibration curves. Results The target components could be well separated，with coefficients of determination higher than 0.999．The limits of detection and limits of quantification of florfenicol were 0.0057 and 0.0019μg/kg，The limits of detection and limits of quantification of florfenicol amine were 0.022 and 0.0074μg/kg．The recovery tests at high，medium，and low spiked levels: the recoveries were 91.9%-108.6%, and relative standard deviation (RSDs) were7.1%-14.2% in eggs; the recoveries were 94.2%-117.2%，and RSDs were 1.4%-7.6% in chicken. The method was used to detect 60 eggs and 60 chicken samples from Guangdong Province, and the result showed that florfenicol or florfenicol amine were detected in 14 chicken samples，they were detected simultaneously in one chicken sample, and the results were 320 μg/kg and 120μg/kg，which exceeded the limit value of 100μg/kg. It was not detected in egg samples. Conclusion The method was accurate and sensitive, and provides a more reliable analytical method for the simultaneous detection and monitoring of florfenicol and florfenicol amine residues in chicken and eggs.

UPLC-MS/MS; Florfenicol; Florfenicol amine; Egg; Chicken; Automated solid phase; Extraction; Residue