A partition chromatographic method is presented for the separation and quantitation of chlorpheniramine, methapyrilene, and pyrilamine in combination. A solution of p‐toluenesulfonic acid and potassium chloride on a column of diatomaceous earth is used to effect the separation. The isolated chlorpheniramine is determined by UV spectrophotometry. The methapyrilene and pyrilamine are separated and determined by GLC. Copyright © 1969 Wiley‐Liss, Inc., A Wiley Company