Microextração Líquido-Líquido Dispersiva (DLLME): proposição de método analítico por DLLME-GC/MS para quantificação de compostos voláteis em óleos essenciais

Abstract

Dispersive liquid–liquid microextraction (DLLME) is a sample preparation technique that combines high extraction efficiency with low solvent consumption, making it suitable for the analysis of volatile compounds in complex matrices. In this study, an analytical method based on DLLME coupled with gas chromatography–mass spectrometry (GC-MS) was proposed and developed for the quantification of eugenol and β-caryophyllene in essential oil samples. The technique is based on the rapid dispersion of a mixture of extraction solvent (dense and hydrophobic) and disperser solvent (miscible with both water and the extractant) into an aqueous solution containing the analytes. This process forms microdroplets that provide a high contact surface area, facilitating analyte transfer. Phase separation was performed by centrifugation, isolating the enriched organic phase. Critical parameters such as the type and volume of solvents, pH, ionic strength, and extraction time were optimized to maximize recovery, enrichment factor, and reproducibility. The method proved to be efficient, sensitive, and environmentally sustainable. Recent advances in the field, including the use of alternative solvents and chemometric optimization strategies, further highlight the potential of DLLME as a robust tool for the analysis of essential oils