Combination of liquid chromatography/tandem mass spectrometry and gas chromatography/mass spectrometry for the detection of 21 anabolic steroid residues in bovine urine

✍ Scribed by Christof Van Poucke; Mario Van De Velde; Carlos Van Peteghem

• Publisher: John Wiley and Sons
• Year: 2005
• Tongue: English
• Weight: 152 KB
• Volume: 40
• Category: Article
• ISSN: 1076-5174
• DOI: 10.1002/jms.845

✦ Synopsis

Abstract

For the detection of anabolic steroid residues in bovine urine, a highly sensitive liquid chromatographic/electrospray ionization tandem mass spectrometric (LC/ESI‐MS/MS) method was developed using both positive and negative ionization. For four compounds the ESI mode was not sensitive enough and gas chromatographic/mass spectrometric GC/MS detection was therefore still necessary as a complementary method. The sample clean‐up consisted of solid‐phase extraction (SPE) on a C~18~ column followed by enzymatic hydrolysis and a second solid‐phase extraction on a combination of a C~18~ and a NH~2~ column. After this last SPE clean‐up, the eluate was split into two equal aliquots. One aliquot was further purified and after derivatization used for GC/MS analysis. The other aliquot was analyzed with LC/MS/MS in both ESI+ and ESI− modes. The method was validated according to the European Commission Decision 2002/657/EC. Decision limits (CCα) were between 0.16 and 1 ng ml^−1^ for the compounds detected with the LC/MS/MS method. The developed method is used in routine analysis in our laboratory. Copyright © 2005 John Wiley & Sons, Ltd.