Extração de contaminantes emergentes por sorção em fase de tecido com determinação por cromatografia líquida de alta eficiência

Abstract

The present work describes the development of an analytical sorption methodology to quantify the emerging contaminants 17α-ethinylestradiol (EE2), estrone (E1) and bisphenol-A (BPA) present in aqueous matrices. To extract them, a 100% cotton fabric was used, which was structurally modified, obtaining a sol-gel fabric. This analytical method is known as Fabric Phase Sorptive Extraction (FPSE). FPSE is a new sorptive extraction technique that integrates the advantages of permeable sol-gel derived organic-inorganic solvents with flexible and permeable tissue substrates, resulting in a highly efficient, fast, simple and sensitive extraction medium that can be introduced directly into any type of fluidic matrix. The detection and quantification of analytes were performed by High Performance Liquid Chromatography (HPLC) with UV-vis detection. The chromatographic conditions determined and used to analyze the optimization processes were: column chromatography (Shimadzu C18 Exsil ODS (4.6 x 250 mm, 5 μm)), mobile phase (MeOH:ACN:H2O (06:38:56 v/v/v)), flow (1 mL min-1 ), wavelengths (λ= 220 nm), injection volume (20 μL) and temperature (Tam (22-25 o C)). The developed method was validated according to the criteria of ANVISA resolution no. 166, of 07/24/2017 and the INMETRO DOQ-CGCRE-008/2020 validation guide. Under optimized conditions, the extraction method presented detection limits of 0.003 μg mL-1 (BPA) and 0.015 μg mL-1 (EE2 and E1), quantification limits of 0.01 μg mL-1 (BPA) and 0.05 μg mL-1 (EE2 and E1), linear range from 0.01 to 10 μg mL-1 for BPA and 0.05 to 10 μg mL-1 for EE2 and E1. The intra-day and inter-day precision (DPR%) obtained values between 2.08 and 8.53%, meeting the criteria established by regulatory agencies. The accuracy was evaluated through recovery tests in dam water samples collected within the city of Catalão-GO, presenting values in the range of 80.51- 98.24%. The proposed methodology was satisfactorily applied for determination of emerging contaminants.