Objective: A sensitive method based on isotope dilution gas chromatography tandem mass spectrometry is described for the determination of the antibiotic chloramphenicol (Cap) in shrimp tissue.
Methods: Homogenized shrimp samples spiked with an isotopically labeled internal standard (d5-Cap) were extracted with ethyl acetate extraction, defatted with hexane, followed by a clean-up step on a SPE C18 cartridge, and then the elute was evaporated and derivatized with Sylon BFT {N,O-bis (trimethylsily) trifluoroacetamide[BSTFA]-trimethylchlorosilane [TMCS] ,99 + 1}. Analyzes were determined by GC/MS-MS in MRM mode.
Results: Internal calibration curves obtained for Cap/ d5-Cap in the 5 to 500 pg range were linear with correlation coefficients of 0.9958. Limit of quantitation (LOQ) was 0.3ng/g. Shrimp tissues were fortified with Cap at 0.3, 0.5, 1.0 ng/g level, average recoveries were 104%, 111% and 95% , respectively.
Conclusion: The proposed method allows the detection, quantitation and confirmation of Cap in shrimps with high accuracy and sensitivity.