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Rapid analysis of anabolic steroid metabolites in urine by combining field asymmetric waveform ion mobility spectrometry with liquid chromatography and mass spectrometry

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journal contribution
posted on 24.08.2017, 11:08 by Kayleigh L. Arthur, Matthew Turner, Alan D. Brailsford, Andrew T. Kicman, David A. Cowan, Jim Reynolds, Colin Creaser
© 2017 American Chemical Society. The combination of field asymmetric waveform ion mobility spectrometry with liquid chromatography-mass spectrometry (LC-FAIMS-MS) has been developed for the analysis of glucuronide and sulfate metabolites of seven anabolic-androgenic steroids in urine. Separation by FAIMS-MS was investigated in positive ion mode for selected cationic adducts (H + , NH 4 + , Na + , K + , and Cs + ). LC-FAIMS-MS analysis of the doubly sodiated adducts ([M + 2Na - H] + ) of isobaric and coeluting steroid metabolites allowed their rapid (8 min) qualitative and quantitative determination in spiked urine using hydrophilic interaction liquid chromatography prior to FAIMS-MS separation, with discrimination > 95% achieved between the steroids investigated. A quantitative evaluation of the LC-FAIMS-MS method was performed giving limits of detection in the range 1-6 ng mL -1 , limits of quantification in the range 3-20 ng mL -1 , with reproducibility (%RSD < 10%; n = 6) and linearity (R 2 > 0.99). The LC-FAIMS-MS method demonstrates increases in signal-to-noise ratios for the doubly sodiated steroid metabolites in unspiked urine ( > 250%) by the reduction of isobaric interferences from the matrix. An alternative or additional tool for identification of the steroid metabolites is based on the observations of different patterns of sodium acetate clusters that are characteristic for each metabolite.

History

School

  • Science

Department

  • Chemistry

Published in

Analytical Chemistry

Volume

89

Issue

14

Pages

7431 - 7437

Citation

ARTHUR, K.L. ...et al., 2017. Rapid analysis of anabolic steroid metabolites in urine by combining field asymmetric waveform ion mobility spectrometry with liquid chromatography and mass spectrometry. Analytical Chemistry, 89(14), pp. 7431-7437.

Publisher

© American Chemical Society (ACS)

Version

AM (Accepted Manuscript)

Publisher statement

This work is made available according to the conditions of the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0) licence. Full details of this licence are available at: https://creativecommons.org/licenses/by-nc-nd/4.0/

Acceptance date

14/06/2017

Publication date

2017-06-14

Notes

This document is the unedited Author’s version of a Submitted Work that was subsequently accepted for publication in Analytical Chemistry, copyright © American Chemical Society after peer review. To access the final edited and published work see http://dx.doi.org/10.1021/acs.analchem.7b00940

ISSN

0003-2700

eISSN

1520-6882

Language

en

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