The novel method for straightforward determination of enantiomeric compositions, including the synthesis of enantiopure chemicals and biologically active substances was reported. This method is based on the transient spectroscopy, exploiting the differences in triplet lifetimes within serum albumins for chiral recognition. Laser flash photolysis(LFP) measurements were performed on (S)- and (R)-flurbiprofen methyl esters (FBPMe) in the presence of human serum albumin (HSA), where (FBPMe) is a prodrug of the nonsteroidal antiinflammatory drug flubiprofen (FBP). The chiral discrimination in the triplet lifetimes of the drug SA complexes has made application of LFP-based method successful. This method has proved to be fast and simple, and require only one measurement. Also it avoids substrate derivatization as well as chromatographic separation and do not depend on the specific rotation to the target compound. This LFP-based approach is a very complementary tool to all the techniques.