COMPARISON OF DIFFERENT EXTRACTION PHASES FOR SOLID-PHASE MICROEXTRACTION IN THIN FILM FORMAT FOR THE ANALYSIS OF HORMONES IN WATER USING HPLC-DAD-FLD

Alan Demarchi Jaccoud; Georgia Labuto; Maria de Lourdes Leite Moraes; Erica Aparecida Souza Silva

Título do Trabalho

Autores

Alan Demarchi Jaccoud
Georgia Labuto
Maria de Lourdes Leite Moraes
Erica Aparecida Souza Silva

Modalidade

Resumo

Área temática

Contaminantes emergentes e Agrotóxicos

Data de Publicação

15/04/2024

País da Publicação

Brasil

Idioma da Publicação

Português

Página do Trabalho

https://www.even3.com.br/anais/xv-laseac-x-enqamb-2024i/788131-comparison-of-different-extraction-phases-for-solid-phase-microextraction-in-thin-film-format-for-the-analysis-of

ISBN

978-65-272-0404-6

Palavras-Chave

TFME ,Hormones ,Endocrine Disruptors , HPLC-DAD-FLD ,Natural Waters

Resumo

Emerging contaminants (ECs) constitute a comprehensive category of compounds that have garnered increasing attention in recent decades due to the lack of established parameters to assess their deleterious impact on the environment. This class encompasses a variety of compounds essential to human quality of life, including personal care products, pharmaceuticals, fertilizers, pesticides, flame retardants, plasticizers, and hormones, among others. The growing detection of these contaminants in aquatic bodies raises concerns, particularly because some of them act as endocrine disruptors, increasing the risk of various diseases.Hormones, whether of natural or synthetic origin, play a crucial role in regulating the endocrine system in living organisms. Researchers are increasingly focusing on new strategies for the extraction, detection, and removal of these emerging contaminants from the environment. In this study, various types of extraction phases were tested for solid-phase microextraction in thin-film format (TFME) to evaluate the most effective preconcentration of samples. A separation method was developed and validated using high-performance liquid chromatography with diode array and fluorescence detectors (HPLC-DAD-FLD) for the analysis of key estrogen and progestogen hormones, both natural and synthetic.Optimized analysis conditions included a C18 5µm column (250 mm x 4.6 mm), a mobile phase of acetonitrile:acidified ultrapure water in a gradient mode, a flow rate of 1 mL/min, injection volume of 20 µL, and detection at 200 nm and 242 nm for DAD and at a wave length of Ex 200 nm and wave length of Em 315 nm for FLD. The analytical curve ranged from 0.005 to 5.0 ng/µL, with satisfactory coefficient of linearity (r2) results close to 1 (minimum of 0.99). Detection limits ranged from 0.029 to 0.335 ng/µL, and quantification limits ranged from 0.090 to 1.017 ng/µL.The selection of the best extraction phase was performed using ultrapure water spiked with analytes of interest at a concentration of 2 mg/L. The following extraction phases were tested: PAN/C18, PAN/PS-DVB, PAN/C18/SCX, and PAN/HLB. The extraction phases were conditioned with a methanol:water solution (50:50 v/v) for 30 minutes. Subsequently, analyte extraction was carried out for 60 minutes at 1200 rpm agitation. Finally, the fibers underwent desorption solvents for 60 minutes at 1200 rpm agitation. Three different solvents were used for desorption for each extraction phase: methanol:water (80:20 v/v), acetonitrile:water (80:20 v/v), and acetonitrile:methanol:water (40:40:20 v/v/v).Based on the quantification results of the extracts, PAN/C18/SCX was selected as the optimal extraction phase, using acetonitrile:water (80:20 v/v) as the desorption solvent. The recovery percentage using the PAN/C18/SCX extraction phase ranged from 47% for the most non-polar analyte up to 83% for the most polar analyte . The selection of extraction phase was based in the results showing the best recovery percentage for all target analytes , and in the percentage of the carry over ranging no further than 5%

Título do Evento: XV LASEAC - X ENQAmb 2024.
Cidade do Evento: Ouro Preto
Título dos Anais do Evento: Anais do XV LASEAC (Latin American Symposium on Environmental Analytical Chemistry) & X ENQAmb (Encontro Nacional de Química Ambiental)
Nome da Editora: Even3
Meio de Divulgação: Meio Digital

Como citar

JACCOUD, Alan Demarchi et al.. COMPARISON OF DIFFERENT EXTRACTION PHASES FOR SOLID-PHASE MICROEXTRACTION IN THIN FILM FORMAT FOR THE ANALYSIS OF HORMONES IN WATER USING HPLC-DAD-FLD.. In: . Disponível em: https//www.even3.com.br/anais/xv-laseac-x-enqamb-2024i/788131-COMPARISON-OF-DIFFERENT-EXTRACTION-PHASES-FOR-SOLID-PHASE-MICROEXTRACTION-IN-THIN-FILM-FORMAT-FOR-THE-ANALYSIS-OF. Acesso em: 24/06/2025