Recovery of volatile fatty acids from fermentation broth has been investigated by adopting an intensified approach using extractants tri-noctylamine 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 K D and %E. The statistical analysis indicated that the degree of influence on K D by experimental variables follows the following trend: extractant type (X 2 ) > pH (X 5 ) > diluent type (X 1 ) > temperature (X 4 ) > extractant concentration (X 1 ). The trend for %E observed is as follows: extractant type (X 2 ) > pH (X 5 ) > temperature (X 4 ) > extractant concentration (X 1 ) > diluent type (X 1 ). The combination of optimum parameters were obtained as X 1 ¼ 1-decanol, X 2 ¼ tri-n-octylamine, X 3 ¼ 20 %, X 4 ¼ 293.15 K, and X 5 ¼ 3.5. A confirmation run was conducted using these parameters and K D 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 K D ¼ 10.36 and %E ¼ 91.26 %.