Recovery of volatile fatty acids from fermentation broth has been investigated by adopting an intensified approach using extractants tri-n-octylamine and tri-butyl phosphate dissolved in 1-decanol and methyl isobutyl ketone. The effects on distribution coefficient (K-D) and extraction efficiency (%E) were studied by varying the operating conditions like temperature (293.15-323.15) K, pH (2.5, 3.5, and 4.5), and compositions of extractant (10, 20, and 30%). Taguchi (L-36) orthogonal design with five factors, namely diluents, extractant type, composition, temperature, and pH, was employed for the multivariate optimization of reactive extraction of volatile fatty acids. In the Taguchi approach, a larger is better criterion was adopted to maximize KD and %E. The statistical analysis indicated that the degree of influence on KD by experimental variables follows the following trend: extractant type (X2)>pH (X5)>diluent type (X1)>temperature (X4)>extractant concentration (X1). The trend for %E observed is as follows: extractant type (X2)>pH (X5)>temperature (X4)>extractant concentration (X1)>diluent type (X1). The combination of optimum parameters were obtained as X-1=1-decanol, X-2=tri-n-octylamine, X-3=20%, X-4=293.15K, and X-5=3.5. A confirmation run was conducted using these parameters and KD and %E values from this run were determined to be 8.65 and of 89.64%, respectively, which were very close to the predicted values KD=10.36 and %E =91.26%.