Feasibility of capillary liquid chromatography/microchip atmospheric pressure photoionization mass spectrometry in analyzing anabolic steroids in urine samples

• Published in: Rapid communications in mass spectrometry 2010-04, Vol.24 (7), p.958-964
• Main Authors: Ahonen, Linda L., Haapala, Markus, Saarela, Ville, Franssila, Sami, Kotiaho, Tapio, Kostiainen, Risto
• Format: Article
• Language: English
• Subjects: Anabolic Agents - urine; Atmospheric pressure; Barometric pressure; beta-Glucosidase - chemistry; beta-Glucosidase - metabolism; Capillary Electrochromatography - methods; Capillary pressure; Feasibility; Humans; Linear Models; Liquid chromatography; Mass spectrometry; Mass Spectrometry - methods; Methandrostenolone - urine; Methyltestosterone - urine; Microchip Analytical Procedures - methods; Nandrolone - urine; Nebulizers and Vaporizers; Photoionization; Reproducibility of Results; Sensitivity and Specificity; Steroids - urine; Urine
• ISSN: 0951-4198; 1097-0231; 1097-0231
• DOI: 10.1002/rcm.4468

We examined the feasibility of capillary liquid chromatography/microchip atmospheric pressure photoionization tandem mass spectrometry (capLC/µAPPI‐MS/MS) for the analysis of anabolic steroids in human urine. The urine samples were pretreated by enzymatic hydrolysis (with β‐glucuronidase from Helix pomatia), and the compounds were liquid‐liquid extracted with diethyl ether. After separation the compounds were vaporized by microchip APPI, photoionized by a 10 eV krypton discharge lamp, and detected by selected reaction monitoring. The capLC/µAPPI‐MS/MS method showed good sensitivity with detection limits at the level of 1.0 ng mL−1, good linearity with correlation coefficients between 0.9954 and 0.9990, and good repeatability with relative standard deviations below 10%. These results demonstrate that microchip APPI combined with capLC/MS/MS provides a new potential method for analyzing non‐polar and neutral compounds in biological samples. Copyright © 2010 John Wiley & Sons, Ltd.