Coupling thin layer chromatography with mass spectrometry for detection and identification of sertraline and its metabolite in the urine

The aim of the study was to detect sertraline and its metabolites in urine under standardized thin layer chromatography (TLC) screening conditions and identify the metabolites using the mass spectrometry method. Materials and methods. Urine samples, collected within 30 hours in portions of 20–50...

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Main Authors: S. B. Baiurka, S. A. Karpushyna, N. M. Kosmina, L. V. Krichkovskaya, I. Ye. Bylov, O. O. Altukhov
Format: Article
Language:English
Published: Zaporizhzhia State Medical and Pharmaceutical University 2024-02-01
Series:Aktualʹnì Pitannâ Farmacevtičnoï ì Medičnoï Nauki ta Praktiki
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Online Access:http://pharmed.zsmu.edu.ua/article/view/293490/291617
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author S. B. Baiurka
S. A. Karpushyna
N. M. Kosmina
L. V. Krichkovskaya
I. Ye. Bylov
O. O. Altukhov
author_facet S. B. Baiurka
S. A. Karpushyna
N. M. Kosmina
L. V. Krichkovskaya
I. Ye. Bylov
O. O. Altukhov
author_sort S. B. Baiurka
collection DOAJ
description The aim of the study was to detect sertraline and its metabolites in urine under standardized thin layer chromatography (TLC) screening conditions and identify the metabolites using the mass spectrometry method. Materials and methods. Urine samples, collected within 30 hours in portions of 20–50 mL, commenced from the seventh hour after the administration of a single therapeutic dose of the drug. The sample preparation process involved dilute acid hydrolysis, followed by the extraction of the native compound and metabolites with chloroform at a pH of 8–9. Thin layer chromatography studies of the extracts were conducted using four unified TLC systems recommended by The International Association of Forensic Toxicologists for general drug screening. Chromatograms were subjected to color reactions with a variety of chromogenic reagents. For the analysis of eluates from chromatograms, a Varian 1200 L mass spectrometer (Netherlands) equipped with a dual quadrupole mass analyzer was employed. Identification was performed through direct sample introduction into the ion chamber, electron-impact ionization (70 eV), and full ion scanning mode. Results. The spot of the native drug on the chromatogram was identified by the Rf, value. Metabolite of sertraline was identified as N-desmethyltrihydroxysertraline by the molecular ion peak in the mass spectrum. Conclusions. The study demonstrated the ability of TLC to detect sertraline and its metabolite, N-desmethyltrihydroxysertraline, in urine after the administration of a single therapeutic dose of the drug. The chromatographic mobility of the native compound and N-desmethyltrihydroxysertraline in the unified TLC screening systems, along with the results of their visualization using chromogenic reagents for toxicological drug screening, was determined. Furthermore, the potential of coupling TLC with mass spectrometry for the separation, detection, and confirmatory identification of sertraline and its metabolic products in urine was established.
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issn 2306-8094
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language English
publishDate 2024-02-01
publisher Zaporizhzhia State Medical and Pharmaceutical University
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series Aktualʹnì Pitannâ Farmacevtičnoï ì Medičnoï Nauki ta Praktiki
spelling doaj-art-800539e35cb74bbd9f52753b38c070802025-08-20T03:14:58ZengZaporizhzhia State Medical and Pharmaceutical UniversityAktualʹnì Pitannâ Farmacevtičnoï ì Medičnoï Nauki ta Praktiki2306-80942409-29322024-02-01171212510.14739/2409-2932.2024.1.293490Coupling thin layer chromatography with mass spectrometry for detection and identification of sertraline and its metabolite in the urineS. B. Baiurka0https://orcid.org/0000-0001-7505-6322S. A. Karpushyna1https://orcid.org/0000-0001-8834-4286N. M. Kosmina2https://orcid.org/0000-0002-9334-1036L. V. Krichkovskaya3https://orcid.org/0000-0003-3136-3149I. Ye. Bylov4https://orcid.org/0000-0001-7685-465XO. O. Altukhov5https://orcid.org/0000-0001-6930-8917National University of Pharmacy, Kharkiv, UkraineNational University of Pharmacy, Kharkiv, UkraineKharkiv Scientific Research Forensic Center of the Ministry of Internal Affairs of UkraineNational University of Pharmacy, Kharkiv, UkraineNational University of Pharmacy, Kharkiv, UkraineKharkiv Scientific Research Forensic Center of the Ministry of Internal Affairs of UkraineThe aim of the study was to detect sertraline and its metabolites in urine under standardized thin layer chromatography (TLC) screening conditions and identify the metabolites using the mass spectrometry method. Materials and methods. Urine samples, collected within 30 hours in portions of 20–50 mL, commenced from the seventh hour after the administration of a single therapeutic dose of the drug. The sample preparation process involved dilute acid hydrolysis, followed by the extraction of the native compound and metabolites with chloroform at a pH of 8–9. Thin layer chromatography studies of the extracts were conducted using four unified TLC systems recommended by The International Association of Forensic Toxicologists for general drug screening. Chromatograms were subjected to color reactions with a variety of chromogenic reagents. For the analysis of eluates from chromatograms, a Varian 1200 L mass spectrometer (Netherlands) equipped with a dual quadrupole mass analyzer was employed. Identification was performed through direct sample introduction into the ion chamber, electron-impact ionization (70 eV), and full ion scanning mode. Results. The spot of the native drug on the chromatogram was identified by the Rf, value. Metabolite of sertraline was identified as N-desmethyltrihydroxysertraline by the molecular ion peak in the mass spectrum. Conclusions. The study demonstrated the ability of TLC to detect sertraline and its metabolite, N-desmethyltrihydroxysertraline, in urine after the administration of a single therapeutic dose of the drug. The chromatographic mobility of the native compound and N-desmethyltrihydroxysertraline in the unified TLC screening systems, along with the results of their visualization using chromogenic reagents for toxicological drug screening, was determined. Furthermore, the potential of coupling TLC with mass spectrometry for the separation, detection, and confirmatory identification of sertraline and its metabolic products in urine was established.http://pharmed.zsmu.edu.ua/article/view/293490/291617sertralinehydroxysertralinen-desmethyltrihydroxysertralineurinethin layer chromatographymass spectrometry
spellingShingle S. B. Baiurka
S. A. Karpushyna
N. M. Kosmina
L. V. Krichkovskaya
I. Ye. Bylov
O. O. Altukhov
Coupling thin layer chromatography with mass spectrometry for detection and identification of sertraline and its metabolite in the urine
Aktualʹnì Pitannâ Farmacevtičnoï ì Medičnoï Nauki ta Praktiki
sertraline
hydroxysertraline
n-desmethyltrihydroxysertraline
urine
thin layer chromatography
mass spectrometry
title Coupling thin layer chromatography with mass spectrometry for detection and identification of sertraline and its metabolite in the urine
title_full Coupling thin layer chromatography with mass spectrometry for detection and identification of sertraline and its metabolite in the urine
title_fullStr Coupling thin layer chromatography with mass spectrometry for detection and identification of sertraline and its metabolite in the urine
title_full_unstemmed Coupling thin layer chromatography with mass spectrometry for detection and identification of sertraline and its metabolite in the urine
title_short Coupling thin layer chromatography with mass spectrometry for detection and identification of sertraline and its metabolite in the urine
title_sort coupling thin layer chromatography with mass spectrometry for detection and identification of sertraline and its metabolite in the urine
topic sertraline
hydroxysertraline
n-desmethyltrihydroxysertraline
urine
thin layer chromatography
mass spectrometry
url http://pharmed.zsmu.edu.ua/article/view/293490/291617
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AT nmkosmina couplingthinlayerchromatographywithmassspectrometryfordetectionandidentificationofsertralineanditsmetaboliteintheurine
AT lvkrichkovskaya couplingthinlayerchromatographywithmassspectrometryfordetectionandidentificationofsertralineanditsmetaboliteintheurine
AT iyebylov couplingthinlayerchromatographywithmassspectrometryfordetectionandidentificationofsertralineanditsmetaboliteintheurine
AT ooaltukhov couplingthinlayerchromatographywithmassspectrometryfordetectionandidentificationofsertralineanditsmetaboliteintheurine