This work aims at exploring the feasibility of a combined process bioflocculation to concentrate sewage organic matter and anaerobic fermentation to produce volatile fatty acids (VFA). Bioflocculation, using a high-loaded aerobic membrane bioreactor (HL-MBR), was operated at an HRT of 1 h and an SRT of 1 day. The HL-MBR process removed on average 83% of sewage COD, while only 10% of nitrogen and phosphorus was removed. During anaerobic fermentation of HL-MBR concentrate at an SRT of 5 days and 35 °C, specific VFA production rate of 282 mg VFA-COD/g VSS could be reached and consisted of 50% acetate, 40% propionate and 10% butyrate. More than 75% of sewage COD was diverted to the concentrate, but only 15% sewage COD was recovered as VFA, due to incomplete VSS degradation at the short treatment time applied. This shows that combined process for the VFA production is technologically feasible and needs further optimization.