Despite the efforts of the pharmaceutical industry to reduce the ethanol content in medicines, many of these products are still commercially available. These medicines must be monitored by quality control techniques using accurate method. Therefore, this study proposes to develop and validate an analytical method for ethanol quantification in adult and pediatric syrups, in order to guarantee the safety of medication certificates. For this, headspace multidimensional gas chromatography (heart-cut) coupled to mass spectrometry (HS-MDGC/MS) was used. The method was validated according to the norm established by National Agency of Sanitary Surveillance (ANVISA) presenting limit of detection (LOD) of 0.03% (v/v) and limit of quantification (LOQ) of 0.06% (v/v) ethanol, excellent selectivity and the recovery values (accuracy) were between 96.71 and 101.38%. Ethanol concentrations in commercial medicines syrups varied from 0.06 to 8.83%, which makes evident the need to control the syrup producing industries.
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