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Two new methods are developed for simultaneous determination of dipyrone (Dip) and camylofin dihydrochloride (Cam) in bulk and in pharmaceutical formulation (Spasmopyralgin M ® tablet) using hyoscine butyl bromide as internal standard (I.S.) to further increase the applicability of the methods. The first method was based on HPLC separation of studied compounds using 250 x 4.6 mm (i.d.) phenomenex (5μm particle size) C18 column as stationary phase and mixture of 50 mM ammonium acetate (pH adjusted to 5.3 using acetic acid) and acetonitrile as mobile phase. The second one was HPTLC method where the separation was achieved on Merck HPTLC aluminium plates of silica gel 60 F254 using acetone: methanol: acetic acid (52: 28: 20, v/v/v) as mobile phase. Comparative study was performed to argue the advantage of each method and determine which one is better for routine analysis of studied drugs.