Determination of testosterone in human hair by gas chromatography-selected ion monitoring mass spectrometry†

Abstract

A method for the determination of testosterone in human hair by gas chromatography-mass spectrometry using d₃-testosterone as internal standard is described. Our method consisted of alkaline digestion, fast liquid–liquid extraction, LH-20 chromatography and derivatization with heptafluorobutyric anhydride. Quantification was achieved by selected ion monitoring of m/z 680 (testosterone) and m/z 683 (d₃-testosterone). Our method needed no complex corrections for isotope contributions. The procedure provided a sensitive and specific technique with good accuracy and precision. For the first time, testosterone has been quantified by gas chromatography-mass spectrometry in human hair. The concentrations (median, range, ng g^–1 hair) reflected a significant (p = 0.05; t-test) sex difference with 2.7 ng g^–1 (2.5–4.2) in male and 1.7 ng g^–1 (1.0–3.4) in female hair.

References

1. G. Casademont, B. Pérez and J. A. García Regueiro, J. Chromatogr. B, 1996, 686, 189.
2. J. P. Perry, J. H. MacIndoe, W. R. Yates, S. D. Scott and T. L. Holman, Clin. Chem., 1997, 43(5), 731.
3. C. Ayotte, D. Goudreault and A. Charlebois, J. Chromatogr. B, 1996, 687, 3.
4. D. Barrón, J. Barbosa, J. A. Pascual and J. Segura, J. Mass. Spectrom., 1996, 31, 309.
5. T. Furuta, K. Kusano and Y. Kasuya, J. Chromatogr., Biomed. Appl., 1990, 525, 15.
6. M. R. Moeller, J. Chromatogr., Biomed. Appl., 1992, 580, 125 and references cited therein.
7. A. Gleixner and H. H. D. Meyer, Fresenius' J. Anal. Chem., 1997, 357, 1198.
8. S. A. Wudy, U. A. Wachter, J. Homoki, W. M. Teller and C. H. L. Shackleton, Steroids, 1992, 57, 319.
9. K. M. Höld, D. G. Wilkins, D. J. Crouch, D. E. Rollins and R. A. Maes, J. Anal. Toxicol., 1996, 20, 345.
10. C. H. L. Shackleton and J. W. Honour, Clin. Chim. Acta, 1976, 69, 267.
11. C. H. L. Shackleton, J. Chromatogr., 1986, 379, 91 and references cited therein.
12. D. de Boer, M. E. Gainza Bernal, R. D. van Oyen and R. A. Maes, Biol. Mass Spectrom., 1991, 20, 459.
13. C. K. Hatton and D. H. Catlin, Clin. Lab. Med., 1987, 7(3), 655.
14. S. J. Gaskell and E. M. H. Finlay, J. Labelled Compd. Radiopharm., 1980, 17, 861.