Verificação de metodologia para quantificação de Carbamato de Etile em aguardentes através de cromatografia gasosa a espectrometria de massas (GC-MS)

Abstract

The manufacturing process of spirits (drinks that contains between 38 and 54 percent alcohol by volume), also called as distilled liquor, consist in distillation of sugarcane fermentation formed wine. Ethyl carbamate (EC) is a secondary compound of the spirits production process, whose reaction route between urea and ethanol under acid condition is the most frequent one. The distillation of sugarcane wine is a spirits manufacturing critical step due ease formation of EC associated to ethanol high content, high process temperature and catalysts presence (Cu2+). EC is a genotoxic carcinogen and its content control on distillate drinks is determined by Ministery of Agriculture, Livestock and Provisioning (MAPA) through June 29th, 2005, 13th Brazilian Ministery of Agriculture Normative Instruction, which 150μg/L is the upper limit allowed. EC quantification was proceed by analytical method using gas chromatography coupled with mass spectrometry (GC/MS) in selected ion monitoring (SIM) mode for the quantification. The analysis of eight concentration patterns was performed in triplicate and the resulting calibration curve presented average regression (R²) of 0,9993. Student T test showed no systematic errors, being the effectiveness of the method proven by the homogeneous coefficient of variation (CV) analyzed of different experiments. The method was submitted to MAPA's proficiency test, whose the analysis was satisfactory for the BEB.016.001 sample and questionable for the BEB.016.002, resulting in a z-score distribution of -0,12 e 2,24, respectively.