Show simple item record

dc.contributor.authorEreño Artabe, Amaia
dc.contributor.authorGonzalez-Gago, Adriana
dc.contributor.authorSuarez Fernández, Amanda
dc.contributor.authorPitarch-Motellón, Jorge
dc.contributor.authorRoig-Navarro, Antoni F.
dc.contributor.authorPozo, Óscar J.
dc.contributor.authorRodríguez González, Pablo
dc.contributor.authorGarcía Alonso, J. Ignacio
dc.date.accessioned2018-09-24T10:45:35Z
dc.date.available2018-09-24T10:45:35Z
dc.date.issued2018-09
dc.identifier.citationEreño Artabe A, González-Gago A, Suarez Fernández A, Pitarch Motellón J, Roig-Navarro AF, Pozo OJ, Rodríguez- González P, García Alonso JI, Isotope Dilution LC-ESI-MS/MS and low resolution Selected Reaction Monitoring as a tool for the accurate quantification of urinary testosterone, Journal of Pharmaceutical and Biomedical Analysis (2018), https://doi.org/10.1016/j.jpba.2018.09.038ca_CA
dc.identifier.urihttp://hdl.handle.net/10234/176215
dc.description.abstractA new analytical method for the quantification of testosterone in human urine samples by isotope dilution mass spectrometry is proposed. A standard solution of 13C2-testosterone is added to the samples at the beginning of the sample preparation procedure and then the measurements are carried out by UHPLC-ESI-MS/MS. In the proposed method, the resolution of the first quadrupole of the tandem MS instrument is reduced to transmit the whole precursor ion cluster to the collision cell and measure the isotopic distribution of the in-cell product ions with a small number of SRM transitions. The construction of a methodological calibration graph is avoided using a labelled analogue previously characterised in terms of concentration and isotopic enrichment in combination with multiple linear regression. In this way, the molar fractions of natural and labelled testosterone are calculated in each sample injection and the amount of endogenous testosterone computed from the known amount of labelled analogue. Recovery values between 97 and 107% and precisions between 0.4 and 3.7% (as %RSD) were obtained for testosterone concentrations in urine in the range of 1 to 8 ng g-1. The proposed low resolution SRM methodology was compared for the analysis of human urine samples with the traditional IDMS method based on a calibration graph and the IDMS method based on multiple linear regression combined with standard resolution SRM. A similar accuracy and precision was obtained by the three tested approaches. However, using the low resolution SRM method there was no need to resort to calibration graphs or to specific dedicated software to calculate isotopic distributions by tandem MS and a higher sensitivity was obtained. The proposed low resolution SRM method was successfully applied to the analysis of the certified freeze-dried human urine NMIA MX005.ca_CA
dc.format.extent23 p.ca_CA
dc.format.mimetypeapplication/pdfca_CA
dc.language.isoengca_CA
dc.publisherElsevierca_CA
dc.rights© 2018 Elsevier B.V. All rights reserved.ca_CA
dc.subjecttestosteroneca_CA
dc.subjecturineca_CA
dc.subjectisotopeca_CA
dc.subjectdilutionca_CA
dc.subjectmass spectrometryca_CA
dc.titleIsotope Dilution LC-ESI-MS/MS and low resolution Selected Reaction Monitoring as a tool for the accurate quantification of urinary testosteroneca_CA
dc.typeinfo:eu-repo/semantics/articleca_CA
dc.identifier.doihttps://doi.org/10.1016/j.jpba.2018.09.038
dc.relation.projectIDSpanish Ministry of Economy and Competitiveness (Project Ref. CTQ2015-70366-P, co-funded by FEDER) ; Clarín-Marie Curie Cofound program (ACB 14-09) ; Spanish Health National System (CPII16/00027)ca_CA
dc.rights.accessRightsinfo:eu-repo/semantics/embargoedAccessca_CA
dc.relation.publisherVersionhttps://www.sciencedirect.com/science/article/pii/S0731708518313451?via%3Dihubca_CA
dc.date.embargoEndDate2020-09-19
dc.type.versioninfo:eu-repo/semantics/acceptedVersionca_CA


Files in this item

Thumbnail

This item appears in the following Collection(s)

Show simple item record