Carbon-13 cross-polarization magic-angle spinning nuclear magnetic resonance spectra of anhydrous formoterol fumarate and the dihydrate are presented, together with some relaxation time measurements. The latter enabled quantitation of mixtures of the anhydrate and dihydrate to be made. Quantitative nuclear magnetic resonance measurements were then performed on mixtures of the two forms formulated in lactose. Relative amounts of the forms could be assessed at a total formulation level of 2%, whereas the dihydrate on its own in lactose was detectable at the 0.45% level. The optimum experiment involves dipolar dephasing, because that minimizes the intensity of signals from the lactose.