An eco-friendly sample preparation procedure based on air-assisted liquid-liquid microextraction for the rapid determination of phthalate metabolites in urine samples by liquid chromatography-tandem mass spectrometry

Autor(es)

Rocha, Bruno Alves ; Gallimberti, Matheus ; Ximenez, Joao Paulo Bianchi ; Basso, Carla Giovana ; Martino-Andrade, Anderson Joel ; Koch, Holger Martin ; Calixto, Leandro Augusto ; Barbosa, Fernando

• Tipo de documento: Artigo Científico
• Fonte: Talanta; v. 266, p. 10-pg., 2024-01-01.

Resumo

Urinary phthalate metabolite (mPAEs) analysis is a reliable tool for assessing human exposure to phthalates. With growing interest in urinary biomonitoring of these metabolites, there is a need for fast and sensitive analytical methods. Therefore, a simple, rapid procedure for simultaneous determination of fifteen phthalate metabolites in human urine samples by liquid chromatography-tandem mass spectrometry was developed. The novelty of the present procedure is based on the use of diethyl carbonate as a green biobased extraction solvent and air-assisted liquid-liquid microextraction (AALLME) as a sample preparation step. A Plackett-Burman design was used for screening the factors that influence the AALLME extraction efficiency of mPAEs. The effective factors were then optimized by response surface methodology using a central composite rotatable design. Under the optimized conditions, good linearity can be achieved in a concentration range of 1.0-20.0 ng mL-1 with correlation coefficients higher than 0.99. The repeatability and reproducibility precision were in the range of 2-12% and 1-10% respectively. Recoveries ranging from 90% to 110%. This, and the low limits of detection, ranging from 0.01 to 0.05 ng mL-1, make the proposed procedure sensitive and suitable for human biomonitoring of phthalate exposures. For proof-of-principle, the new method was used to measure the urinary concentrations of mPAEs in 20 urine samples from Brazilian women. The high frequency of detections and in part high con-centrations of mPAEs indicate to widespread exposure to several phthalates among Brazilian women. (AU)

• Processo FAPESP: 22/07979-1 - Metabolômica do expossoma por espectrometria de massas
• Beneficiário: Bruno Alves Rocha
• Modalidade de apoio: Bolsas no Brasil - Programa Capacitação - Treinamento Técnico
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• Modalidade de apoio: Bolsas no Brasil - Pós-Doutorado
• Processo FAPESP: 18/24069-3 - Do biomonitoramento ao reconhecimento de assinaturas do exposoma humano visando antecipar riscos para uma saúde contínua
• Beneficiário: Fernando Barbosa Júnior
• Modalidade de apoio: Auxílio à Pesquisa - Temático
• Processo FAPESP: 20/02939-6 - Análise sistemática da relação dinâmica entre ambiente, metabolismo e condição de saúde, aplicando uma abordagem de aprendizado de máquina
• Beneficiário: João Paulo Bianchi Ximenez
• Modalidade de apoio: Bolsas no Brasil - Pós-Doutorado