Procedures were developed for the synthesis, purification and analysis of propanediol (PD) esters of n-fatty acids (FA). Mono- (MAPD) and di-acylated (DAPD) species were synthesized from PD and FA using an immobilized lipase (Candida antarctica B) in tert-butanol. MAPD and DAPD were isolated using silica gel column chromatography as approximately 95% pure preparations. Normal phase gradient LC provided for resolution of MAPD, DAPD and FA. UV220 nm detection provided a detection limit of about 1 microgram, and a linear response range of up to 2000 micrograms. Response factors were determined for MAPD, DAPD and FA components comprised of n-fatty acyl lengths of 4-16.