Comparison of purification procedures for the isolation and detection of anabolic residues in faeces using gas chromatography-mass spectrometry†
(Note: The full text of this document is currently only available in the PDF Version )
Thierry Hamoir, Gaspard Pottie, Dirk Courtheyn, Hubert De Brabander, Philippe Delahaut and Luc Leyssens
Abstract
Within several regional field laboratories and the national reference laboratory a harmonised methodology for the analysis of anabolic residues in faecal samples was developed. The method consists of a liquid–liquid and a solid-phase extraction step, followed by a high-performance liquid chromatography purification step. Using gas chromatography-mass spectrometry, currently illegally used anabolic steroids can be detected in faeces at the ppb level. Within this context acidification, followed by centrifugation under cooling, allows efficient, practical and rapid defatting of faecal samples. Furthermore, a combination of a silica and an aminopropyl solid-phase extraction column was found to give the best results as regards the sample purification process.
References
- F. Smets and G. Vandewalle, Z. Lebensm.-Unters. Forsch., 1984, 178, 38 Search PubMed.
- D. Courtheyn, J. Vercammen, H. De Brabander, I. Vandenreyt, P. Batjoens, K. Vanoosthuyze and C. Van Peteghem, Analyst, 1994, 119, 2557 RSC.
- H. De Brabander, J. Van Hende, P. Batjoens, L. Hendriks, J. Raus, F. Smets, G. Pottie, L. Van Ginkel and R. W. Stephany, Analyst, 1994, 119, 2581 RSC.
- P. Batjoens, H. De Brabander, F. Smets and G. Pottie, Analyst, 1994, 119, 2607 RSC.
- L. Leyssens, E. Royakers, B. Gielen, M. Misotten, J. Schoofs, J. Czech, J. P. Noben, L. Hendriks and J. Raus, J. Chromatogr., 1994, 654, 43 CrossRef CAS.
- H. De Brabander, P. Batjoens, K. De Wasch, D. Courtheyn, G. Pottie and F. Smets, Trends Anal. Chem., 1997, 16, 485 CrossRef CAS.
- Off. J. Eur. Comm., 1993, L 118, 64 Search PubMed.
- T. M. C. M. De Kok, P. J. Levels, A. Van Faasen, M. Hazen, F. Ten Hoor and J. C. S. Kleinjans, J. Chromatogr., 1992, 580, 135 CrossRef CAS.
- T. Hamoir, F. Smets and G. Pottie, unpublished works.
- L. R. Snyder and J. J. Kirkland, Introduction to Modern Liquid Chromatography, Wiley, New York, 1974 Search PubMed.
- J. Rosén, K.-E. Hellenäs, P. Törnqvist and P. Shearan, Analyst, 1994, 119, 2635 RSC.