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Volume 30
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This is an early access version, the complete PDF, HTML, and XML versions will be available soon.
Article

Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices

by
Joana R. P. Pereira
1,2,
Daniela C. Rocha
1,
Nuno R. Neng
1,2,*,
Paulo Maurício
3,
M. Edite Torres
1,
Samir M. Ahmad
1,2 and
Alexandre Quintas
1,*
1
Laboratório de Ciências Forenses e Psicológicas Egas Moniz, Molecular Pathology and Forensic Biochemistry Laboratory, Egas Moniz Center for Interdisciplinary Research, Egas Moniz School of Health and Science, Quinta da Granja, 2829-511 Caparica, Almada, Portugal
2
Centro de Química Estrutural, Institute of Molecular Sciences, Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal
3
Oral Rehabilitation Department, CiiEM, Instituto Universitário Egas Moniz, Quinta da Granja, Monte de Caparica, 2829-511 Caparica, Portugal
*
Authors to whom correspondence should be addressed.
Molecules 2025, 30(1), 68; https://doi.org/10.3390/molecules30010068 (registering DOI)
Submission received: 5 December 2024 / Revised: 24 December 2024 / Accepted: 26 December 2024 / Published: 27 December 2024
(This article belongs to the Section Analytical Chemistry)
Versions Notes

Abstract

The present work reports the development, optimization, and validation, of a methodology to determine lidocaine, procaine, tetracaine, and benzocaine in urine matrices. Two extractive preconcentration techniques, solid-phase microextraction (SPME) LC Tips and bar adsorptive microextraction (BAμE), were studied and applied to the four target anesthetics, followed by gas chromatography-mass spectrometry (GC-MS) analysis. Several parameters that could affect microextraction and back-extraction were optimized using two different designs of experiments (Box–Behnken and full-factorial) to maximize extraction efficiency from aqueous media. Under optimized experimental conditions, the BAμE technique showed better performance than SPME LC tips and was chosen for validation assays and urine sample analysis. In blank urine, the BAµE/GC-MS methodology revealed suitable sensitivity (LOD between 2 and 18 ng/mL), good linearity (r2 ≥ 0.9945) between 0.5 and 30.0 µg/mL and recovery yields of 30.3-97.9%. Good precision (% RSD ≤ 8.8%) and accuracy (bias % between −15.9 and 15.0%) values were achieved. The developed methodology was successfully applied to the target anesthetics analysis of volunteers’ urine matrices and proved to be an environmentally friendly alternative to monitor trace levels of local anesthetics in complex matrices compared to other extraction techniques.
Keywords: local anesthetics; urine matrices; bar adsorptive microextraction (BAµE); solid phase microextraction (SPME) LC Tips; GC-MS local anesthetics; urine matrices; bar adsorptive microextraction (BAµE); solid phase microextraction (SPME) LC Tips; GC-MS

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MDPI and ACS Style

Pereira, J.R.P.; Rocha, D.C.; Neng, N.R.; Maurício, P.; Torres, M.E.; Ahmad, S.M.; Quintas, A. Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices. Molecules 2025, 30, 68. https://doi.org/10.3390/molecules30010068

AMA Style

Pereira JRP, Rocha DC, Neng NR, Maurício P, Torres ME, Ahmad SM, Quintas A. Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices. Molecules. 2025; 30(1):68. https://doi.org/10.3390/molecules30010068

Chicago/Turabian Style

Pereira, Joana R. P., Daniela C. Rocha, Nuno R. Neng, Paulo Maurício, M. Edite Torres, Samir M. Ahmad, and Alexandre Quintas. 2025. "Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices" Molecules 30, no. 1: 68. https://doi.org/10.3390/molecules30010068

APA Style

Pereira, J. R. P., Rocha, D. C., Neng, N. R., Maurício, P., Torres, M. E., Ahmad, S. M., & Quintas, A. (2025). Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices. Molecules, 30(1), 68. https://doi.org/10.3390/molecules30010068

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