In this work, acylglycerols rich in n-3 PUFA were prepared by enzymatic glycerolysis of sardine oil using immobilized C. antarctica Lipase B (Lipozyme 435) in TP. The MAG fraction was purified using SPD. Different evaporation temperatures were evaluated to maximize the MAG recovery at high purity in the distillate. The main purpose of this study was to develop an effective distillation process for concentration of n-3 PUFA in MAG form.