Determination of Antidepressants in Human Plasma by Modified Cloud-Point Extraction Coupled with Mass Spectrometry

Cloud-point extraction (CPE) is rarely combined with liquid chromatography coupled to mass spectrometry (LC–MS) in drug determination due to the matrix effect (ME). However, we have recently shown that ME is not a limiting factor in CPE. Low extraction efficiency may be improved by salt addition, bu...

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Main Authors: Elżbieta Gniazdowska, Natalia Korytowska, Grzegorz Kłudka, Joanna Giebułtowicz
Format: Article
Language:English
Published: MDPI AG 2020-12-01
Series:Pharmaceuticals
Subjects:
Online Access:https://www.mdpi.com/1424-8247/13/12/458
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author Elżbieta Gniazdowska
Natalia Korytowska
Grzegorz Kłudka
Joanna Giebułtowicz
author_facet Elżbieta Gniazdowska
Natalia Korytowska
Grzegorz Kłudka
Joanna Giebułtowicz
author_sort Elżbieta Gniazdowska
collection DOAJ
description Cloud-point extraction (CPE) is rarely combined with liquid chromatography coupled to mass spectrometry (LC–MS) in drug determination due to the matrix effect (ME). However, we have recently shown that ME is not a limiting factor in CPE. Low extraction efficiency may be improved by salt addition, but none of the salts used in CPE are suitable for LC–MS. It is the first time that the influences of a volatile salt—ammonium acetate (AA)—on the CPE extraction efficiency and ME have been studied. Our modification of CPE included also the use of ethanol instead of acetonitrile to reduce the sample viscosity and make the method more environmentally friendly. We developed and validated CPE–LC–MS for the simultaneous determination of 21 antidepressants in plasma that can be useful for clinical and forensic toxicology. The selected parameters included Triton X-114 concentration (1.5 and 6%, <i>w/v</i>), concentration of AA (0, 10, 20 and 30%, <i>w/v</i>), and pH (3.5, 6.8 and 10.2). The addition of 10% of AA increased recovery twice. For 20 and 30% (<i>w/v</i>) of AA, three phases were formed that prolonged the extraction process. The developed CPE method (6% Triton X-114, 10% AA, pH 10.2) was successfully validated through LC–MS/MS simultaneous determination of 21 antidepressants in human plasma. The linearity was in the range of 10–750 ng/mL (r<sup>2</sup> > 0.990).
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spelling doaj.art-2be21f4f62674e92aba5c05931d145e52023-11-21T00:34:29ZengMDPI AGPharmaceuticals1424-82472020-12-01131245810.3390/ph13120458Determination of Antidepressants in Human Plasma by Modified Cloud-Point Extraction Coupled with Mass SpectrometryElżbieta Gniazdowska0Natalia Korytowska1Grzegorz Kłudka2Joanna Giebułtowicz3Łukasiewicz Research Network, Industrial Chemistry Institute, 8 Rydygiera, 01-793 Warsaw, PolandDepartment of Bioanalysis and Drugs Analysis, Faculty of Pharmacy, Medical University of Warsaw, 1 Banacha, 02-097 Warsaw, PolandDepartment of Bioanalysis and Drugs Analysis, Faculty of Pharmacy, Medical University of Warsaw, 1 Banacha, 02-097 Warsaw, PolandDepartment of Bioanalysis and Drugs Analysis, Faculty of Pharmacy, Medical University of Warsaw, 1 Banacha, 02-097 Warsaw, PolandCloud-point extraction (CPE) is rarely combined with liquid chromatography coupled to mass spectrometry (LC–MS) in drug determination due to the matrix effect (ME). However, we have recently shown that ME is not a limiting factor in CPE. Low extraction efficiency may be improved by salt addition, but none of the salts used in CPE are suitable for LC–MS. It is the first time that the influences of a volatile salt—ammonium acetate (AA)—on the CPE extraction efficiency and ME have been studied. Our modification of CPE included also the use of ethanol instead of acetonitrile to reduce the sample viscosity and make the method more environmentally friendly. We developed and validated CPE–LC–MS for the simultaneous determination of 21 antidepressants in plasma that can be useful for clinical and forensic toxicology. The selected parameters included Triton X-114 concentration (1.5 and 6%, <i>w/v</i>), concentration of AA (0, 10, 20 and 30%, <i>w/v</i>), and pH (3.5, 6.8 and 10.2). The addition of 10% of AA increased recovery twice. For 20 and 30% (<i>w/v</i>) of AA, three phases were formed that prolonged the extraction process. The developed CPE method (6% Triton X-114, 10% AA, pH 10.2) was successfully validated through LC–MS/MS simultaneous determination of 21 antidepressants in human plasma. The linearity was in the range of 10–750 ng/mL (r<sup>2</sup> > 0.990).https://www.mdpi.com/1424-8247/13/12/458sample preparationLC–MS/MSantidepressantbioanalytical methods
spellingShingle Elżbieta Gniazdowska
Natalia Korytowska
Grzegorz Kłudka
Joanna Giebułtowicz
Determination of Antidepressants in Human Plasma by Modified Cloud-Point Extraction Coupled with Mass Spectrometry
Pharmaceuticals
sample preparation
LC–MS/MS
antidepressant
bioanalytical methods
title Determination of Antidepressants in Human Plasma by Modified Cloud-Point Extraction Coupled with Mass Spectrometry
title_full Determination of Antidepressants in Human Plasma by Modified Cloud-Point Extraction Coupled with Mass Spectrometry
title_fullStr Determination of Antidepressants in Human Plasma by Modified Cloud-Point Extraction Coupled with Mass Spectrometry
title_full_unstemmed Determination of Antidepressants in Human Plasma by Modified Cloud-Point Extraction Coupled with Mass Spectrometry
title_short Determination of Antidepressants in Human Plasma by Modified Cloud-Point Extraction Coupled with Mass Spectrometry
title_sort determination of antidepressants in human plasma by modified cloud point extraction coupled with mass spectrometry
topic sample preparation
LC–MS/MS
antidepressant
bioanalytical methods
url https://www.mdpi.com/1424-8247/13/12/458
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