Abstract: The method for separation and identification of three pairs of agarofuran epimers(α-and β-dihydroagarofuran,α-and β-baimuxinol, α-and β-baimuxinol methyl ether) by HRGC andHRGC/MSD is described. The proportion of each pair of isomers was determined and the analyticalprocedure for isomers of sesquiterpenes was established. Thus, the correct synthetic route can be effc-tively guided and the study of agarofuran synthesis can be greatly accelerated. The method provides areliable basis for identifying the products. MS data given in Table 2 may be useful for the identifica-tion of agarofuran derivatives.