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Article

Selective Extraction of Diazepam and Its Metabolites from Urine Samples by a Molecularly Imprinted Solid-Phase Extraction (MISPE) Method

by
Ana María Gil Tejedor
,
Juan Carlos Bravo Yagüe
*,
Gema Paniagua González
*,
Rosa María Garcinuño Martínez
and
Pilar Fernández Hernando
Department of Analytical Sciences, Faculty of Sciences, National Distance Education University (UNED), Urbanización Monte Rozas, Avda. Esparta s/n, 28232 Las Rozas, Madrid, Spain
*
Authors to whom correspondence should be addressed.
Polymers 2024, 16(5), 635; https://doi.org/10.3390/polym16050635
Submission received: 15 January 2024 / Revised: 15 February 2024 / Accepted: 19 February 2024 / Published: 27 February 2024
(This article belongs to the Special Issue Research and Application of Molecularly Imprinted Polymers)

Abstract

In this research, a molecularly imprinted polymer (MIP) was synthesized by precipitation polymerization using oxazepam (OZ) as a template molecule and was subsequently applied as a selective sorbent for the extraction of diazepam (DZP) and its metabolites in urine samples using an SPE cartridge. OZ, temazepam (TZ), nordiazepam (NZ) and DZP were analyzed in the final extracts by high-performance liquid chromatography with diode array detection (HPLC-DAD). The SPE extraction steps were optimized, and the evaluation of an imprinting factor was carried out. The selectivity of the method for OZ versus structurally related benzodiazepines (BZDs), such as bromazepam (BRZ), tetrazepam (TTZ) and halazepam (HZ), was investigated. Under the optimum conditions, the proposed methodology provided good linearity in the range of 10–1500 ng/mL, with limit of detection values between 13.5 and 21.1 ng/mL and recovery levels for DZP and its metabolites from 89.0 to 93.9% (RSD ≤ 8%) at a concentration level of 1000 ng/mL. The proposed method exhibited good selectivity, precision and accuracy and was applied to the analysis of urine samples from a real case of DZP intake.
Keywords: benzodiazepines; molecular imprinting solid-phase extraction; urine samples; HPLC-DAD benzodiazepines; molecular imprinting solid-phase extraction; urine samples; HPLC-DAD
Graphical Abstract

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MDPI and ACS Style

Gil Tejedor, A.M.; Bravo Yagüe, J.C.; Paniagua González, G.; Garcinuño Martínez, R.M.; Fernández Hernando, P. Selective Extraction of Diazepam and Its Metabolites from Urine Samples by a Molecularly Imprinted Solid-Phase Extraction (MISPE) Method. Polymers 2024, 16, 635. https://doi.org/10.3390/polym16050635

AMA Style

Gil Tejedor AM, Bravo Yagüe JC, Paniagua González G, Garcinuño Martínez RM, Fernández Hernando P. Selective Extraction of Diazepam and Its Metabolites from Urine Samples by a Molecularly Imprinted Solid-Phase Extraction (MISPE) Method. Polymers. 2024; 16(5):635. https://doi.org/10.3390/polym16050635

Chicago/Turabian Style

Gil Tejedor, Ana María, Juan Carlos Bravo Yagüe, Gema Paniagua González, Rosa María Garcinuño Martínez, and Pilar Fernández Hernando. 2024. "Selective Extraction of Diazepam and Its Metabolites from Urine Samples by a Molecularly Imprinted Solid-Phase Extraction (MISPE) Method" Polymers 16, no. 5: 635. https://doi.org/10.3390/polym16050635

APA Style

Gil Tejedor, A. M., Bravo Yagüe, J. C., Paniagua González, G., Garcinuño Martínez, R. M., & Fernández Hernando, P. (2024). Selective Extraction of Diazepam and Its Metabolites from Urine Samples by a Molecularly Imprinted Solid-Phase Extraction (MISPE) Method. Polymers, 16(5), 635. https://doi.org/10.3390/polym16050635

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