Simultaneous Determination of Fourteen Verterinary Antibiotics in Animal Manure Using Solid Phase Extraction and Liquid Chromatography
A method for the simultaneous determination of fourteen antibiotics in animal manure was studied and the parameters of accelerated solvent extraction(ACE),programs of solid phase extraction(SPE) and HPLC detection conditions were optimized.Fourteen antibiotics had been separated at the baseline on a C18 column at the wavelength of 270 nm after eluted by 1% acetate solution(pH=2.6) and acetonitrile.The limits of detection for tetracyclines(TCs),sulfonamides(SAs),fluoroquinolones(FQs) and tylosin(TYL) were 35-90 μg/kg,12-28 μg/kg,9-17μg/kg and 19 μg/kg,respectively.After extracted by buffer solution of 50% methanol,then enriched and cleaned-up by HLB,the recoveries of antibiotics(at the concentration of 1 μg/g and 10 μg/g) in manure were 58%-75% and 66%-83%,4%-93% and 91%-101%,74%-80% and 80%-88%,85% and 68% for TCs,SAs,FQs and TYL,respectively.The method was applied to determine fourteen antibiotics in animal manure samples collected from Liaoning Province.TCs,SAs,FQs and TYL were all detected in these manure samples and the concentrations were in the range of 0.75-22.34 mg/kg,0.10-1.71 mg/kg,0.38-4.46 mg/kg and 0.23-0.35 mg/kg,respectively.