A high-performance liquid chromatographic method has been developed and validated for the fingerprinting (profiling) and quantitative determination of E- and Z-guggulsterones, the hypolipidemic agents in the gum-resin exudate of Commiphora mukul, currently marketed worldwide as hypocholesterolemic. The method involves extraction of the guggul-resin from either the raw exudate or compounded tablets (or capsules) with ethyl acetate, concentration of the combined extracts and chromatography on a reversed-phase C18 column using an acetonitrile-water gradient. The method has a validated quantitation range of 15-85 microg/ml for E-guggulsterone and 25-130 microg/ml for Z-guggulsterone with a precision of +/-2% S.D. and a recovery of >99.5%. Standard curve correlation coefficients of 0.992 or greater were obtained during validation experiments. The method was applied to six commercial (OTC) products, all of which were found to contain significantly less (in most cases very little or none) of the claimed guggulsterones.