Determination of Thirteen Antibiotics Residues in Manure by Solid Phase Extraction and High Performance Liquid Chromatography

A method was developed for the determination of five sulfonamides, four tetracyclines, two quinolones, furazolidone and chloramphenicol in liquid manure and chicken dung using solid phase extraction with high performance liquid chromatographic detection. Acetonitrile and 0.01 mol/L oxalic acid were used as the mobile phase to seperate four tetracyclines and chloramphenicol. Five sulfonamides, two quinolones and furazolidone were separated by acetonitrile and 0.025 mol/L NH4OAc. Limit of detection and quantization fall into the range of 0.01 - 0.05 mg/L and 0.03 - 0.167 mg/L respectively. Thirteen antibiotics in liquid manure and chicken dung were extracted using a mixture of ACN acidified with acetate buffer and EDTA and McIlvaine buffer respectively, then they were cleaned-up and pre-concentrated by hydrophilic-liphophillic balance (HLB) cartridge. The recoveries are 54% - 103%. This method was successfully used in the detection of 13 antibiotics in 4 livestock husbandries in Tianjin. Results showed the above all antibiotics were detected, with concentrations of 0.3 - 173.2 mg/kg.