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Esta dissertação descreve o trabalho desenvolvido no estágio realizado no âmbito da unidade curricular “Dissertação/Estágio” do Mestrado em Engenharia Química – Ramo Qualidade na Symington Family Estates Vinhos, S.A..
O presente trabalho teve como objetivo a implementação e validação de um método de análise de 2,4,6-tricloroanisol em vinhos de mesa tintos por microextração em fase sólida (SPME) no headspace (HS) e análise por cromatografia gasosa com deteção por captura de eletrões (GC-ECD).
Foram realizados estudos de otimização das condições de extração, comparando o comportamento da metodologia para diferentes tempos de extração e dessorção, e diferentes percentagens de álcool, nomeadamente, vinho sem diluição (13% (v/v)) ou com diluição 1:2 (6,5% (v/v)). Utilizando a fibra de SPME de polidimetilsiloxano (PDMS) de 100 μm, obtiveram-se resultados satisfatórios com 25 minutos de extração, 5 minutos de dessorção e um teor alcoólico de 6,5 % (v/v).
Para validar o método realizaram-se estudos de linearidade, gama de trabalho, limiares analíticos, precisão (repetibilidade), exatidão e incerteza. Os resultados obtidos demonstram boa linearidade do método, na gama de 1,0 ng/L a 8,0 ng/L, com coeficientes de determinação (R2) superiores a 0,995, limite de deteção de 0,47 ng/L e limite de quantificação 1,57 ng/L.
This dissertation describes the work carried out in the internship of the curricular unit "Dissertation/Internship" of the Master in Chemical Engineering – Quality at Symington Family Estates Vinhos, S.A.. The purpose of this work was to implement and validate a method for the analysis of 2,4,6-Trichloroanisol in red wines by headspace-solid phase microextraction (HSSPME) and analysis by gas chromatography with electron capture detection (GC-ECD). Studies on the optimization of the extraction conditions were performed, comparing the behavior of the methodology for different extraction and desorption times, and different percentages of alcohol, namely, wine without dilution (13% (v/v)) or with dilution 1:2 (6.5% (v/v)). Using the SPME fiber of Polydimethylsiloxane (PDMS) of 100 μm, satisfactory results were obtained with 25 minutes of extraction, 5 minutes of desorption and an alcoholic content of 6.5% (v/v). To validate the method, studies of linearity, concentration range, analytical thresholds, precision (repeatability), accuracy and uncertainty were performed. The results obtained demonstrate good linearity of the method, in the range of 1.0 ng/L to 8.0 ng/L, with coefficients of determination (R2) higher than 0.995, detection limit of 0.47 ng/L and limit of quantification of 1.57 ng/L.
This dissertation describes the work carried out in the internship of the curricular unit "Dissertation/Internship" of the Master in Chemical Engineering – Quality at Symington Family Estates Vinhos, S.A.. The purpose of this work was to implement and validate a method for the analysis of 2,4,6-Trichloroanisol in red wines by headspace-solid phase microextraction (HSSPME) and analysis by gas chromatography with electron capture detection (GC-ECD). Studies on the optimization of the extraction conditions were performed, comparing the behavior of the methodology for different extraction and desorption times, and different percentages of alcohol, namely, wine without dilution (13% (v/v)) or with dilution 1:2 (6.5% (v/v)). Using the SPME fiber of Polydimethylsiloxane (PDMS) of 100 μm, satisfactory results were obtained with 25 minutes of extraction, 5 minutes of desorption and an alcoholic content of 6.5% (v/v). To validate the method, studies of linearity, concentration range, analytical thresholds, precision (repeatability), accuracy and uncertainty were performed. The results obtained demonstrate good linearity of the method, in the range of 1.0 ng/L to 8.0 ng/L, with coefficients of determination (R2) higher than 0.995, detection limit of 0.47 ng/L and limit of quantification of 1.57 ng/L.
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Keywords
2,4,6-TCA Vinho SPME Otimização Validação Wine Optimization Validation