Isotope Dilution LC-ESI-MS/MS and low resolution Selected Reaction Monitoring as a tool for the accurate quantification of urinary testosterone
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Other documents of the author: Ereño Artabe, Amaia; Gonzalez-Gago, Adriana; Suarez Fernández, Amanda; Pitarch-Motellón, Jorge; Roig-Navarro, Antoni F.; Pozo, Óscar J.; Rodríguez González, Pablo; García Alonso, J. Ignacio
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comunitat-uji-handle2:10234/33596
comunitat-uji-handle3:10234/33597
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Title
Isotope Dilution LC-ESI-MS/MS and low resolution Selected Reaction Monitoring as a tool for the accurate quantification of urinary testosteroneAuthor (s)
Date
2018-09Publisher
ElsevierBibliographic citation
Ereño 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.2018.09.038Type
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info:eu-repo/semantics/acceptedVersionSubject
Abstract
A 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 ... [+]
A 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. [-]
Investigation project
Spanish 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)Rights
© 2018 Elsevier B.V. All rights reserved.
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