A quality control procedure has been developed for the determination of diazepam in pharmaceuticals using Fourier transform infrared (FTIR) spectroscopy. The method involves the off-line extraction of diazepam with chloroform by sonication and direct determination in the extracts through peak area measurement in the interval between 1672 and 1682cm −1 using a baseline correction defined between 1850 and 1524cm −1 . For standardization it was used an external calibration line established from standard solutions of diazepam in chloroform. The method provides a limit of detection of 0.04mg per tablet (n=5), a relative standard deviation (R.S.D.) of 0.5% for 5 independent measurements of a standard solution at a concentration level of 0.76mgg −1 and a sampling frequency of the whole procedure of 4h −1 , being required only 45s for the measurement step. Results obtained by FTIR agree with those obtained by a reference methodology based on ultraviolet spectrometry and thus the developed procedure offers a good alternative for the determination of diazepam in pharmaceuticals.