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

• Chloramphenicol, thiamphenicol and florfenicol were tested by UPLC–MS/MS.
• Matrix solid-phase dispersion was used for the preparation of fish samples.
• The developed method was accurate and reproducible.

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 (C18). A column made from the C18/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 (r2) with each matrix-matched calibration curve is higher than 0.999. CCα and CCβ of the fenicols upon the method were ranged from 0.02 to 0.06 μg kg−1 and 0.11–0.16 μg 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.