Determination of chloramphenicol, thiamphenicol, and florfenicol in fish muscle by matrix solid-phase dispersion extraction (MSPD) and ultra-high pressure liquid chromatography tandem mass spectrometry

摘要

An UPLC-MS/MS method based on matrix solid-phase dispersion (MSPD) was developed for the determination of chloramphenicol (CAP), thiamphenicol (TAP) and florfenicol (FF) in fish muscle. Muscle tissue was blended with octadecylsilyl-derivatized silica (C-18). A column made from the C-18/muscle tissue matrix was washed with n-hexane, after which CAP was eluted with acetonitrile/water (50:50, v/v) and partitioned into ethyl acetate. The final extract was evaporated, and reconstituted into methanol/water (10:90, v/v) for the analysis of UPLC-MS/MS. The correlation coefficient (r(2)) with each matrix-matched calibration curve is higher than 0.999. CC alpha and CC beta of the fenicols upon the method were ranged from 0.02 to 0.06 mu g kg(-1) and 0.11-0.16 mu g kg(-1) respectively. At the fortified levels, mean recoveries of the three compounds were ranged from 84.2% to 99.8%, and the RSDs were lower than 12%. The method was accurate and reproducible, being successfully applied to the monitoring of CAP, TAP and FF in fish samples obtained from the Chinese market. (C) 2014 Elsevier Ltd. All rights reserved.