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

A method was developed for determination of 5 sulfonamides, 4 tetracyclines, 2 quinolones, furazolidone, and chloramphenicol in liquid manure and chicken dung using the solid phase extraction with the high performance liquid chromatography detection. Acetonitrile and 0.01 M of oxalic acid were used as the mobile phase to separate 4 tetracyclines and chloramphenicol. Five sulfonamides, two quinolones, and furazolidone were separated by acetonitrile and 0.025 M NH4OAc. The limit of detection and quantization fall into the range of 0.01–0.05 mg l−1 and 0.03–0.167 mg l−1, respectively. Thirteen antibiotics in liquid manure and chicken dung were extracted using a mixture of ACN acidified with citrate buffer and EDTA-McIlvaine buffer, respectively. Then, they were cleaned-up and preconcentrated by the hydrophilic-lipophilic balance (HLB) cartridge. The overall recovery was up to 54%–110%. This method was successfully used in the detection of 13 antibiotics from 4 livestock husbandries in Tianjin, China. Results showed that all the antibiotics could be detected, with the concentration ranges of 0.3–173.2 mg kg−1.