VALIDATION OF A METHOD FOR THE ANALYSIS OF 2-FURFURYLTHIOL, THIOPHENE AND DIMETHYL DISULFIDE BY GAS CHROMATOGRAPHY COUPLED WITH MASS SPECTROMETRY (GC-QMS)
UEKANE, T.M.1*, ROCHA-LEÃO, M.H.M.2, REZENDE, C.M.1
1 Universidade Federal do Rio de Janeiro, Instituto de Química, Cidade Universitária, CT, Bloco A, CEP 21941-909, Rio de Janeiro – RJ, Brazil.
2 Universidade Federal do Rio de Janeiro, Escola de Química, Cidade Universitária, CT, Bloco E, CEP 21941-909, Rio de Janeiro – RJ, Brazil.
Sulfur compounds are an important aromatic class present in various foods, known as character-impact compounds, identified in cheese, bread, meat, mushrooms, beverages like coffee, beer, wines, whiskey and other alcoholic drinks. A research using SciFinder Chemical Abstract Data Base with roasted coffee and sulfur compounds as key-words yield, 2-Furfurylthiol (2-FFT), Thiophene (THIO) and Dimethyl disulfide (DMDS) as the most cited compounds. Validation of analytical methods is important to assure reliability of results. The aim of this work is to perform a single-laboratory method validation for the analysis of 2-FFT, THIO and DMDS by GC-qMS. The performance criteria assessed were: specificity, working range, linearity, sensibility, limit of detection (LD), limit of quantification (LQ), trueness and precision. Specificity was ensured through the use of selective monitoring ion (SIM) for the GC-qMS. Linearity was confirmed with correlation coefficient, examination of residuals and testing homocedasticity from the linear regression plotted on a working range of 15-200 µg.mL-1 for 2-FFT, 20-300 µg.mL-1 for THIO and 30-200 µg.mL-1 for DMDS. Sensibility was indicated by the slope of the regression line. LD (S/N=3) was 10 µg.mL-1 for 2-FFT and 5 µg.mL-1 for both THIO and DMDS. LQ (S/N=10) was 15 µg.mL-1 for 2-FFT and 10 µg.mL-1 for both THIO and DMDS. Trueness assed by spiking and recovery experiments of three different concentration levels were an average of 110% for 2-FFT, 100% for THIO and 97% for DMDS. Precision assessed under repeatability (intraday), intermediate precision (interday) and reproducibility (different days of analysis and change of solvent) conditions were below 2% for the three compounds. All validation parameters obtained were within acceptance criteria established for the three analytes and/or are in agreement with the goal of the method proposed.
Financial Support: FAPERJ, CAPES E CNPq ; Area: Food Science.
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