Determination of ramipril in human plasma and its fragmentation by UPLC-Q-TOF-MS with positive electrospray ionization

This report presents the application of ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry with positive electrospray ionization, to determine ramipril in human plasma. First, the proteins in human plasma were precipitated using acetonitrile, then the supe...

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Main Authors: Szpot Paweł, Buszewicz Grzegorz
Format: Article
Language:English
Published: Sciendo 2015-06-01
Series:Acta Pharmaceutica
Subjects:
Online Access:https://doi.org/10.1515/acph-2015-0018
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author Szpot Paweł
Buszewicz Grzegorz
author_facet Szpot Paweł
Buszewicz Grzegorz
author_sort Szpot Paweł
collection DOAJ
description This report presents the application of ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry with positive electrospray ionization, to determine ramipril in human plasma. First, the proteins in human plasma were precipitated using acetonitrile, then the supernatant was extracted by ethyl acetate at pH 3 and finally, the extract was analyzed using a UPLC-QTOF- MS system. The method was validated and the coefficient of determination (R2) was > 0.999, the lower limit of quantification (LLOQ) was 0.5 ng mL-1. Precision, recovery and stability were determined for three different concentrations of ramipril. RSD for this method ranged from 3.3 to 8.6 %. The intra-day mean recovery was from 65.3 to 97.3 %. In addition, the fragmentation of ramipril was studied. Due to high resolution of the spectrometer, it was possible to measure fragment masses accurately and determine their molecular and chemical formulas with high accuracy.
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issn 1846-9558
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series Acta Pharmaceutica
spelling doaj-art-4dc554e22abd48b190877dd8d73cf4722025-02-02T09:44:14ZengSciendoActa Pharmaceutica1846-95582015-06-0165215916910.1515/acph-2015-0018acph-2015-0018Determination of ramipril in human plasma and its fragmentation by UPLC-Q-TOF-MS with positive electrospray ionizationSzpot Paweł0Buszewicz Grzegorz1Laboratory of Forensic Toxicology Medical University of Lublin 20-090 Lublin, PolandLaboratory of Forensic Toxicology Medical University of Lublin 20-090 Lublin, PolandThis report presents the application of ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry with positive electrospray ionization, to determine ramipril in human plasma. First, the proteins in human plasma were precipitated using acetonitrile, then the supernatant was extracted by ethyl acetate at pH 3 and finally, the extract was analyzed using a UPLC-QTOF- MS system. The method was validated and the coefficient of determination (R2) was > 0.999, the lower limit of quantification (LLOQ) was 0.5 ng mL-1. Precision, recovery and stability were determined for three different concentrations of ramipril. RSD for this method ranged from 3.3 to 8.6 %. The intra-day mean recovery was from 65.3 to 97.3 %. In addition, the fragmentation of ramipril was studied. Due to high resolution of the spectrometer, it was possible to measure fragment masses accurately and determine their molecular and chemical formulas with high accuracy.https://doi.org/10.1515/acph-2015-0018ramipriluplc-q-tof-msfragmentation pathway
spellingShingle Szpot Paweł
Buszewicz Grzegorz
Determination of ramipril in human plasma and its fragmentation by UPLC-Q-TOF-MS with positive electrospray ionization
Acta Pharmaceutica
ramipril
uplc-q-tof-ms
fragmentation pathway
title Determination of ramipril in human plasma and its fragmentation by UPLC-Q-TOF-MS with positive electrospray ionization
title_full Determination of ramipril in human plasma and its fragmentation by UPLC-Q-TOF-MS with positive electrospray ionization
title_fullStr Determination of ramipril in human plasma and its fragmentation by UPLC-Q-TOF-MS with positive electrospray ionization
title_full_unstemmed Determination of ramipril in human plasma and its fragmentation by UPLC-Q-TOF-MS with positive electrospray ionization
title_short Determination of ramipril in human plasma and its fragmentation by UPLC-Q-TOF-MS with positive electrospray ionization
title_sort determination of ramipril in human plasma and its fragmentation by uplc q tof ms with positive electrospray ionization
topic ramipril
uplc-q-tof-ms
fragmentation pathway
url https://doi.org/10.1515/acph-2015-0018
work_keys_str_mv AT szpotpaweł determinationoframiprilinhumanplasmaanditsfragmentationbyuplcqtofmswithpositiveelectrosprayionization
AT buszewiczgrzegorz determinationoframiprilinhumanplasmaanditsfragmentationbyuplcqtofmswithpositiveelectrosprayionization