A new method, involving the application of PMR spectroscopy for the analysis of diloxanide furoate in authentic powder and in tablets form is proposed. The PMR spectrum of diloxanide shows singler peak at δ = 3.23 due to N-CH3protons which is chosen for quantitative measurement. Tetramethylsilane (TMS) was used as internal standard. Comparing of the integral of N-CH3singlet signal to that of the sharp singlet of TMS positioned at δ = 0.00 was adopted as the principal of the method.