Boosting miniaturization in clinical analysis: determination of bisphenols in human serum and urine by miniaturized stir bar sorptive dispersive microextraction

Autores de IIS La Fe

• Evelin Elsbiet Lara Molina

  Autor

Participantes ajenos a IIS La Fe

• Peris-Pastor, G
• Benedé, JL
• Chisvert, A

Grupos

• Endocrinología Reproductiva e Infertilidad

Abstract

In this work, a miniaturized and sustainable method for the determination of endocrine-disrupting bisphenols in human serum and urine employing the miniaturized stir bar sorptive dispersive microextraction (mSBSDME) approach has been developed. As bisphenols are conjugated in the human body to their glucorinated and sulfated forms, an enzymolysis employing a commercial mixture of beta-glucuronidase and arylsulfatase was carried out prior to the microextraction procedure to determine their total content. A magnetic covalent organic framework (COF) was employed as the sorbent to carry out the extraction of the analytes from the biological matrixes, showing good extraction performance due to its hydrophobic, pi-pi, and dipole-dipole interactions with the analytes. As instrumental detection, liquid chromatography-tandem mass spectrometry (LC-MS/MS) was employed to achieve good sensitivity and selectivity. The method was validated for both matrixes, showing good linearity at least up to 100 ng mL-1, limits of detection in the low ng mL-1 range, good precision values (relative standard deviations below 15%), and good accuracy (relative recoveries between 80 and 127%). In order to show the applicability of the developed method, five samples from female volunteers were analyzed with the final aim of offering a practical tool for monitoring the female population's exposure to these highly endocrine-disrupting compounds. This new procedure enhances the implementation of miniaturized sample preparation approaches in biological samples for clinical analysis, giving special relevance to the sustainability of the method.

© 2024. The Author(s), under exclusive licence to Springer-Verlag GmbH, DE part of Springer Nature.

Keywords

• Bioanalysis; Bisphenols; Low-volume samples; Magnetic covalent organic framework; Miniaturized stir bar sorptive dispersive microextraction