Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices
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), w...
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MDPI AG
2024-12-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/30/1/68 |
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| author | Joana R. P. Pereira Daniela C. Rocha Nuno R. Neng Paulo Maurício M. Edite Torres Samir M. Ahmad Alexandre Quintas |
| author_facet | Joana R. P. Pereira Daniela C. Rocha Nuno R. Neng Paulo Maurício M. Edite Torres Samir M. Ahmad Alexandre Quintas |
| author_sort | Joana R. P. Pereira |
| collection | DOAJ |
| description | 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 (<i>r</i><sup>2</sup> ≥ 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. |
| format | Article |
| id | doaj-art-7d7d3734ad40409ab3ed3c66ac473251 |
| institution | Kabale University |
| issn | 1420-3049 |
| language | English |
| publishDate | 2024-12-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj-art-7d7d3734ad40409ab3ed3c66ac4732512025-01-10T13:18:46ZengMDPI AGMolecules1420-30492024-12-013016810.3390/molecules30010068Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine MatricesJoana R. P. Pereira0Daniela C. Rocha1Nuno R. Neng2Paulo Maurício3M. Edite Torres4Samir M. Ahmad5Alexandre Quintas6Laboratório 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 Almada, PortugalLaboratório 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 Almada, PortugalLaboratório 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 Almada, PortugalOral Rehabilitation Department, CiiEM, Instituto Universitário Egas Moniz, Quinta da Granja, Monte de Caparica, 2829-511 Caparica, PortugalLaboratório 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 Almada, PortugalLaboratório 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 Almada, PortugalLaboratório 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 Almada, PortugalThe 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 (<i>r</i><sup>2</sup> ≥ 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.https://www.mdpi.com/1420-3049/30/1/68local anestheticsurine matricesbar adsorptive microextraction (BAµE)solid phase microextraction (SPME) LC TipsGC-MS |
| spellingShingle | Joana R. P. Pereira Daniela C. Rocha Nuno R. Neng Paulo Maurício M. Edite Torres Samir M. Ahmad Alexandre Quintas Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices Molecules local anesthetics urine matrices bar adsorptive microextraction (BAµE) solid phase microextraction (SPME) LC Tips GC-MS |
| title | Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices |
| title_full | Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices |
| title_fullStr | Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices |
| title_full_unstemmed | Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices |
| title_short | Bar Adsorptive Microextraction Approach for Trace Determination of Local Anesthetics in Urine Matrices |
| title_sort | bar adsorptive microextraction approach for trace determination of local anesthetics in urine matrices |
| topic | local anesthetics urine matrices bar adsorptive microextraction (BAµE) solid phase microextraction (SPME) LC Tips GC-MS |
| url | https://www.mdpi.com/1420-3049/30/1/68 |
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