Simultaneous Determination Of Tetracyclines And Fluoroquinolones In Aquatic Food Product

Animal drug residue is the original drug or its metabolin cumulated or stored in the cell or organ of the animal fed with drug. Commonly used animal drugs are tetracyclines (TCs), fluoroquinolones (FQs) , macrolide (MALs) ,sulfonamides (SAs) ,nitrofurans (NIFs) and nitroimidazole(NIIs). And the mostly common used are TCs, FQs and MALs. There are several methods to detect animal drug residue such as radioimmunoassay, enzyme linked immunosorbent assay, microbiological assay,high performance liquid chromatography(HPLC) method and liquid chromatography tandem mass(LC-MS) method. For its high sensivity and good stability , HPLC method is chosed to be the normal or standard method. But the preparation for HPLC detection is fussy, so many researchers bend themselves to develop method for detection of multi-residues and multi-classes residues.This research aims at developing HPLC detection method to extract, clean-up and determine the TCs and FQs in aquatic food product.It focus on the research as follows:Firstly, chromatographic column and column temperature suitable for separation was selected. Effects of mobile phase such as its composition and their concentration and pH on the retention behaviors and separation results were examined.Then the conditions for extract and clean-up the analytes from samples were optimized.After the optimization mentioned above ,HPLC detection method was developed.With UV detector,the detective limits of TCs were 0.0355~0.0509 mg/kg;that of FQs were 0.0105~0.0138 mg/kg;the quantitative limits of TCs were 0.118~0.169 mg/kg with lineary range of 0.2~10mg/L and that of FQs were 0.0350~0.0460 mg/kg with lineary range of 0.1~10 mg/L. The spiked recoveries were in the range of 80.8～90.5%.Secondly,with the optimization of mobile phase and cone voltage,LC-MS detection method was developed. For mass detector,the detective limits of TCs were 0.0215~0.0426 mg/kg;that of FQs were 0.0100~0.0118 mg/kg;the quantitative limits of TCs were 0.0645~0.128 mg/kg with lineary range of 0.2~10mg/L and that of FQs were 0.0300~0.0354 mg/kg with lineary range of 0.1~10 mg/L.Thirdly,make primary studies on the residues and elimination of oxytetracycline enrofloxacin and ciprofloxacin in crucian with the method developed.In this research,we developed HPLC and LC-MS method to detect residues of TCs and FQs in marine product.And we look forward to making beneficial contribute to marine product safety and export.