Advanced search
1 file | 1.23 MB

Direct quantification of steroid glucuronides in human urine by liquid chromatography-electrospray tandem mass spectrometry

Oscar Juan Pozo Mendoza (UGent) , Peter Van Eenoo (UGent) , Wim Van Thuyne (UGent) , Koen Deventer (UGent) and Frans Delbeke (UGent)
(2008) JOURNAL OF CHROMATOGRAPHY A. 1183(1-2). p.108-118
Author
Organization
Abstract
A method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the direct quantification of glucuronides of testosterone (TG), epitestosterone (EPG), androsterone (AG) and etiocholanolone (ETG) has been developed. The method allowed for the direct determination of these analytes avoiding hydrolysis and derivatization, which are usual steps in commonly used methods based on gas chromatography-mass spectrometry (GC-MS). The electrospray ionization and the product ion spectra of the glucuronides have been studied in order to obtain the most specific transitions. The use of the selected transitions is necessary for the determination of the analytes at low ng/ml concentration levels. Two different approaches have been tested for sample preparation: direct injection after filtration and acidic liquid-liquid extraction (LLE) with ethyl acetate. Both approaches have been validated obtaining satisfactory values for accuracy and precision with limits of detection lower than 1 ng/ml for TG and EPG. Ion suppression was more pronounced after LLE probably due to the concentration of interferences from acidic urine. The applicability of the method has been checked by the analysis of 40 urine samples. The results were compared with those obtained with the common GC-MS method. Results have shown a good correlation between both methods with correlation coefficients higher than 0.97. A slope close to I was obtained for all analytes except for AG possibly due to losses during the extraction process prior to GC-MS.

Downloads

  • (...).pdf
    • full text
    • |
    • UGent only
    • |
    • PDF
    • |
    • 1.23 MB

Citation

Please use this url to cite or link to this publication:

Chicago
Pozo Mendoza, Oscar Juan, Peter Van Eenoo, Wim Van Thuyne, Koen Deventer, and Frans Delbeke. 2008. “Direct Quantification of Steroid Glucuronides in Human Urine by Liquid Chromatography-electrospray Tandem Mass Spectrometry.” Journal of Chromatography A 1183 (1-2): 108–118.
APA
Pozo Mendoza, O. J., Van Eenoo, P., Van Thuyne, W., Deventer, K., & Delbeke, F. (2008). Direct quantification of steroid glucuronides in human urine by liquid chromatography-electrospray tandem mass spectrometry. JOURNAL OF CHROMATOGRAPHY A, 1183(1-2), 108–118.
Vancouver
1.
Pozo Mendoza OJ, Van Eenoo P, Van Thuyne W, Deventer K, Delbeke F. Direct quantification of steroid glucuronides in human urine by liquid chromatography-electrospray tandem mass spectrometry. JOURNAL OF CHROMATOGRAPHY A. 2008;1183(1-2):108–18.
MLA
Pozo Mendoza, Oscar Juan, Peter Van Eenoo, Wim Van Thuyne, et al. “Direct Quantification of Steroid Glucuronides in Human Urine by Liquid Chromatography-electrospray Tandem Mass Spectrometry.” JOURNAL OF CHROMATOGRAPHY A 1183.1-2 (2008): 108–118. Print.
@article{424635,
  abstract     = {A method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the direct quantification of glucuronides of testosterone (TG), epitestosterone (EPG), androsterone (AG) and etiocholanolone (ETG) has been developed. The method allowed for the direct determination of these analytes avoiding hydrolysis and derivatization, which are usual steps in commonly used methods based on gas chromatography-mass spectrometry (GC-MS). The electrospray ionization and the product ion spectra of the glucuronides have been studied in order to obtain the most specific transitions. The use of the selected transitions is necessary for the determination of the analytes at low ng/ml concentration levels. Two different approaches have been tested for sample preparation: direct injection after filtration and acidic liquid-liquid extraction (LLE) with ethyl acetate. Both approaches have been validated obtaining satisfactory values for accuracy and precision with limits of detection lower than 1 ng/ml for TG and EPG. Ion suppression was more pronounced after LLE probably due to the concentration of interferences from acidic urine. The applicability of the method has been checked by the analysis of 40 urine samples. The results were compared with those obtained with the common GC-MS method. Results have shown a good correlation between both methods with correlation coefficients higher than 0.97. A slope close to I was obtained for all analytes except for AG possibly due to losses during the extraction process prior to GC-MS.},
  author       = {Pozo Mendoza, Oscar Juan and Van Eenoo, Peter and Van Thuyne, Wim and Deventer, Koen and Delbeke, Frans},
  issn         = {0021-9673},
  journal      = {JOURNAL OF CHROMATOGRAPHY A},
  language     = {eng},
  number       = {1-2},
  pages        = {108--118},
  title        = {Direct quantification of steroid glucuronides in human urine by liquid chromatography-electrospray tandem mass spectrometry},
  url          = {http://dx.doi.org/10.1016/j.chroma.2008.01.045},
  volume       = {1183},
  year         = {2008},
}

Altmetric
View in Altmetric
Web of Science
Times cited: