Desenvolvimento de um cartucho microporoso hidrofílico para microextração verde e sua aplicação na análise de amostras ambientais e alimentares por cromatografia gasosa bidimensional abrangente

Abstract

This thesis presents the development and validation of a hydrophilic microporous cartridge (HMCart), an innovation in sample preparation for complex environmental and food analyses. Combined with the direct immersion solid-phase microextraction (DI-SPME) technique, the device serves as a selective filter, protecting the fiber and enabling direct contact with solid samples without the need for harsh pre-treatment steps. The robustness of the methodology was demonstrated through successful application to various complex matrices, including the detection of adulterants in herbal medicines, the determination of polycyclic aromatic hydrocarbons (PAHs) in soils, and the analysis of PAHs and pesticides in spices and herbs. Additionally, the method enabled the characterization of volatile organic compounds (VOCs) and semi-volatile organic compounds (SVOCs) in jabuticaba peels, unconventional edible plants (PANCs), and spices, with emphasis on identifying bioactive terpenes and calculating their odor activity values (OAVs). The combination of HMCart-DI-SPME with comprehensive two-dimensional gas chromatography (GCGC) was essential to address the complexity of the analyzed matrices. This synergistic approach provided high separation, identification, and quantification capacity, along with excellent analytical sensitivity, ensuring the robustness and reliability of the results. Evaluation of the method from a green analytical chemistry perspective, using the AGREE tool, confirmed its contribution to reducing solvent consumption, analysis time, and consumable wear. These advances demonstrate not only the analytical robustness and versatility of the system but also its high level of technological maturity, positioning it as a promising solution for implementation in laboratory routines and real-scale monitoring processes. Therefore, this thesis consolidates an original contribution to the field of sample preparation, offering an innovative and sustainable strategy with significant potential for application in quality control, environmental monitoring, and the exploration of bioactive compounds of food and sensory interest.