Simultaneous Determination of Chloramphenicol, Thiamphenicol, Florfenicol and Florfenicol Amine Residues in Aquatic Products with Gas Chromatography/Mass Spectrometry

Abstract:

In this study we used major aquatic products in china (Penaeus chinensis, turbot, carp, river eels, crabs and turtles) as the experimental materials to explore the simultaneous detection of multiple residues of chloramphenicol drugs [Chloramphenicol (CAP), Thiamphenicol (TAP), Florfenicol (FF) and its metabolites-Florfenicol amine (FFA)] in the muscle tissues of aquatic products, and the method of Gas chromatography-Mass spectrometry was established. Samples were extracted with ethyl acetate and ammonium hydroxide (v : v = 98 : 2), degreased with n-hexane, and further defatted with the Oasis MCX solid phase extraction cartridge. Then the samples were derivatized with the silanization reagent and negative chemical ionization (NCI). The selected ion monitoring mode (SIM) was applied in the experiments. The selected ions of the four drugs were as below: CAP m/z 376, 378, 466*, 468; TAP m/z 409*, 411, 499, 411; FF m/z 339*, 341, 429, 341; FFA m/z 209*, 194, 210, 194 (*quantitative ion). The matrix spiked calibration curve was established. There was a clear linear relationship in the ranges of 2−200 ng/ml for CAP and 5−200 ng/ml for TAP, FF and FFA, and the correlation coefficients were more than 0.990. The recovery was 75%−110%, and the relative standard deviation was 5.7%−13.9%. The detection limit was 0.2 μg/kg for CAP, and 1.0 μg/kg for TAP, FF and FFA. These results indicated that the GC/MS method could be accurate, efficient, sensitive and highly specific. Therefore it may satisfy the simultaneous determination of the four target compounds in aquatic products.