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The HPLC technique with UV-Vis detection was employed in the analysis of cocaine content in apprehended samples of cocaine and crack. A peak signal for cocaine was obtained in 3.5 minutes run by using acetonitrile/water (95:5v/v) as a mobile phase. Optimized spectrophotometric signal was obtained at a wavelength of 224 nm. The analytical curve from 1.0 to 40.0 ppm of cocaine was obtained, showing a linear correlation coefficient of 0.9989, with detection and quantification limits of 0.75 ppm and 3.78 ppm, respectively. This methodology was employed at the dosage of confiscated samples of cocaine and crack in the Scientific Police Laboratory of Ribeirão Preto-SP city.