The extraction effects of fluoroquinolones(FQs) and tetracyclines (TCs) in manure were compared experimantally by using different extractions,and the method of mixed extractions of EDTA-McIlvaine and 50%Mg(NO3)2-2.5% NH3?H2O was developed.The proportion of two extractions was explored.The result indicated that when the volume ratio of EDTA-McIlvaine and 50% Mg(NO3)2-2.5% NH3?H2O was 3∶1,the extraction ratios for the six antibiotics,including tetracycline(TC),chlortetracy(CTC),enrofloxacin(ENR),pefloxacin(PEF),danofloxain(DAR) and sarafloxacin(SAR) were between 84% and 92%.Based on this,the methods of solid phase extraction and purification for the six residued drugs were optimized through the investigation on different elution-volume and extraction columns.At the same time,the concentration method was established by optimizing the conditions that using nitrogen concentration and rotation-evaporation.Eventually,the simultaneous extraction and determination of fluoroquinolones(FQs) and tetracyclines(TCs) in manure by high performance capillary electrophoresis(HPCE) was established.Under the optimal chromatographic conditions,the linear ranges were between 3.125 mg/L and 100 mg/L,the limit of quantitation for six antibiotics were less than 0.1 mg/kg.At the spiked concentrations of 10.0,20.0,40.0 mg/L，recoveries of six antibiotics in manure ranged from 54% to 93% with relative standard deviations(RSDs) of 6.3%-8.9%.This method was quite simple,rapid and low-cost,and was successfully used in the detection of six antibiotics in manure around the city of Hefei.