A gas-chromatographic determination method of thiamin which use a quantitative cleavage of thiamin to 4-methyl-5-(2-hydroxyethyl)thiazol [I] and solvent extraction of the analyte prior to GC injection was modified. A column chromatographic procedure using a reversed phase, high capacity solid phase cartridge was applied to the clean-up of the analyte. Thiazol derivative[I] was quantitatively recovered upon the column method. Acetanilide, an internal standard, has a good recovery through the analytical procedure. The method has analytical precision of 2% or less in the coefficient of variation.