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A rapid and sensitive analytical gas chromatography-mass spectrometry (GC-MS) method for perfume analysis to determine the phthalates banned by the European Union Regulation on cosmetic samples is presented. This method has been tested in commercial alcoholic perfume samples for the determination of the following seven phthalates: dibutyl phthalate, bis(2-ethylhexyl) phthalate, bis(2-methoxyethyl) phthalate, n-pentyl-isopentylphthalate, di-n-pentyl phthalate, diisopentylphthalate and benzyl butyl phthalate. Sample evaporation and redissolution in ethanol is carried out before GC-MS analysis, with no dilution of the sample. External calibration and standard addition calibration are compared to detect possible matrix effects. External calibration could provide good results in some cases but standard addition calibration is recommended as matrix effects are observed in many cases in the determination of the target phthalates. The accuracy of the method has been proven by the analysis of quality control samples prepared from commercial free phthalate perfumes after spiking with known concentrations of the analytes. Accurate results were obtained with limits of detection in the ng mL−1 range and good repeatability (relative standard deviations lower than 6%). The method was satisfactorily applied to the analysis of commercial perfume samples, and the results revealed considerable amounts of dibutyl phthalate and bis(2-ethylhexyl) phthalate in some of the analyzed samples.