As an exemplary case study of enzymatically catalyzed liquidliquidsolid systems, the enzymatic hydrolysis of methyl octanoate using immobilized Candida antarctica lipase B as catalyst was studied. The reaction system included two liquid phases (aqueous and organic) and the solid catalyst phase. Experiments were performed in a new laboratory packed-bed reactor arrangement with continuous liquidliquid phase separation. The assembly allowed two operation modes in which either the organic phase (singular phase flow) or an emulsion (biphasic flow) was circulated through the packed bed. The previously published mathematical model was modified and extended. When the model was parameterized on the basis of biphasic flow experiments, the model could subsequently be used to analyze the singular phase flow experiments. A comparison of both operation modes was performed, and for the first time the influence of the packed-bed flow rate in singular phase flow mode on the reaction course was investigated.