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Simultaneous Quantification of Antidepressants and Metabolites in Urine and Plasma Samples by GC–MS for Therapeutic Drug Monitoring

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Abstract

The aim of this work was the optimization and method validation for antidepressants (fluoxetine, venlafaxine, amitriptyline, mianserin, trimipramine, nortriptyline, mirtazapine, sertraline, dothiepin, citalopram, and paroxetine) and their metabolites in urine and plasma samples using gas chromatography–mass spectrometry (GC–MS). The antidepressants were extracted with a Strata™ X solid-phase extraction (SPE) cartridge prior to analysis. The method presented linearity within the studied ranges in both samples with quantification limits varying from 1 to 15 ng mL−1 and determination coefficients (R 2) higher than 0.99 for all analytes in all runs. The limits of detection ranged from 1 to 5 ng mL−1 for the compounds under study. The recovery for urine samples ranged from 40 to 89% and for plasma samples varied from 68 to 98%. Precision and accuracy analysis showed acceptable coefficients of variation and relative error, fulfilling the criteria normally accepted in bioanalytical method validation. The method developed proved to be suitable for screening of the studied drugs in urine and plasma samples, proving to be sensitive and presenting appropriate selectivity and sensitivity, allowing detection of small amounts of the analytes.

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Acknowledgements

The authors acknowledge the Programa Operacional Regional do Centro 20072013 “Mais Centro”—Project “Therapeutic drug monitoring on age-related diseases” (CENTRO-07-ST24-FEDER-002012), the program POCI—COMPETE 2020—Operational Programme Competitiveness and Internationalisation in Axis I—Strengthening research, technological development and innovation (Project POCI-01-0145-FEDER-007491) and National Funds by FCT—Foundation for Science and Technology (Project UID/Multi/00709/2013). The authors are grateful to MsC Ivo Moreno for his help in the sample preparation and data analysis.

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Authors and Affiliations

  1. CICS-UBI, Centro de Investigação em Ciências da Saúde, Universidade da Beira Interior, Av. Infante D. Henrique, 6201-506, Covilhã, Portugal

    Tiago Rosado, Alexandra Gonçalves, Ana Martinho, Gilberto Alves, Ana Paula Duarte, Fernanda Domingues, Samuel Silvestre, Luiza Breitenfeld Granadeiro & Eugenia Gallardo

  2. CNC, Centro de Neurociências e Biologia Celular, Universidade de Coimbra, Rua Larga Faculdade de Medicina, Pólo I, 1º andar, 3004-504, Coimbra, Portugal

    Gilberto Alves & Samuel Silvestre

  3. Departamento de Psiquiatria e Saúde Mental, Centro Hospitalar Cova da Beira, E.P.E., 6201-551, Covilhã, Portugal

    Víctor Oliveira & Carlos Leitão

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  1. Tiago Rosado
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Correspondence to Eugenia Gallardo.

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The authors have no relevant affiliations or financial involvement with any organization or entity with a financial interest in or financial conflict.

Ethical approval

Authentic samples are analyzed routinely by the laboratory, and therefore the ethical standards are guaranteed by the hospital where they are collected. All procedures performed in studies involving human participants were in accordance with the ethical standards of the institutional and/or national research committee and with the 1964 Helsinki Declaration and its later amendments or comparable ethical standards.

Research involving Human Participants and/or Animals

This article does not contain any study (clinical trials) involving human participants or animals.

Informed consent

Informed consent was obtained from all individual participants included in the study (Protocol: “Monitorização terapêutica de fármacos antipsicóticos em doentes do foro psiquiátrico: contribuição para o estabelecimento de relações entre as concentrações terapêuticas em amostras biológicas e avaliação da adesão terapêutica”- CHCB/March-2012).

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Rosado, T., Gonçalves, A., Martinho, A. et al. Simultaneous Quantification of Antidepressants and Metabolites in Urine and Plasma Samples by GC–MS for Therapeutic Drug Monitoring. Chromatographia 80, 301–328 (2017). https://doi.org/10.1007/s10337-017-3240-3

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