MICROWAVE-ASSISTED SOLVENT EXTRACTION OF MELAMINE FROM SEAFOOD AND DETERMINATION BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY: OPTIMIZATION BY FACTORIAL DESIGN

摘要

Melamine attracts considerable attention because of its toxicity. The determination of melamine in seafood was performed by gas-chromatography-mass spectrometry, using an optimized version of a method adopted by the U.S. Food and Drug Administration. The melamine was extracted by closed-vessel microwave-assisted solvent extraction (MAE), as a valid alternative in sample preparation, to reduce analysis time and provide less ambiguous data. The procedure was optimized by means of experimental factorial design considering the three main variables that affect this process: microwave oven power, the maximum temperature inside the extraction tube, and the hold time. The recovery of melamine in spiked samples was used as the elemental response value of the design. Temperature and hold time had a more positive effect on the response than the microwave power. A significant positive interaction was observed between oven power and hold time. A temperature of 70℃ and a hold time of 1 min gave a recovery of 92±5% for a microwave power of 600 W. Under these conditions, the total microwave extraction time was approximately 2 minutes, a much shorter time compared to the ultrasonic bath, which required a total time of 40 min. The repeatability of the method was approximately 3%. The limits of quantification were 0.55 mg kg~(-1) for MAE and 1.9 mg kg~(-1) for the ultrasonic bath; the linearity was confirmed up to 10 mg kg~(-1). In conclusion, the MAE procedure was shown to be an excellent alternative to the official method.