Screening of beta-2 agonists and confirmation of fenoterol, orciprenaline, reproterol and terbutaline with gas chromatography-mass spectrometry as tetrahydroisoquinoline derivatives.
A new method for a comprehensive screening and confirmation of beta-2 agonists in human urine is presented based on gas chromatography-low-resolution mass spectrometry (GC-MS) using electron impact ionisation (EI). After hydrolysis of the conjugates with beta-glucuronidase/arylsulfatase a derivatisation step with formaldehyde converts fenoterol, orciprenaline, reproterol and terbutaline to one derivative, a tetrahydroisoquinoline, while the other beta-2 agonists remain unchanged. Liquid-liquid extraction and trimethylsilylation follow. The tetrahydroisoquinoline derivatives show good gas chromatographic and mass spectrometric behaviour. The detection limit of these four beta-2 agonists in the screening using low-resolution mass spectrometry is 10 ng/ml of urine. The other beta-2 agonists are detected as parent compounds with the same recovery after sample preparation with and without formaldehyde. The EI mass spectra of the tetrahydroisoquinoline derivatives are presented.
Henze
M K
MK
Institut für Biochemie, Deutsche Sporthochschule Koln, Cologne, Germany.
Opfermann
G
G
Spahn-Langguth
H
H
Schänzer
W
W
D058672:Adrenergic beta-2 Receptor Antagonists; D000318:Adrenergic beta-Agonists / Q000032:analysis / Q000652:urine*; D002138:Calibration; D004338:Drug Combinations; D005280:Fenoterol / Q000032:analysis / Q000652:urine; D005557:Formaldehyde / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D006863:Hydrogen-Ion Concentration; D007546:Isoquinolines / Q000737:chemistry; D009921:Metaproterenol / Q000031:analogs & derivatives* / Q000032:analysis / Q000652:urine; D012680:Sensitivity and Specificity; D015813:Substance Abuse Detection; D013726:Terbutaline / Q000032:analysis / Q000652:urine; D013806:Theophylline / Q000031:analogs & derivatives* / Q000032:analysis / Q000652:urine
D058672:Adrenergic beta-2 Receptor Antagonists; D000318:Adrenergic beta-Agonists; D004338:Drug Combinations; D007546:Isoquinolines; C014792:reproterol; D005557:Formaldehyde; D005280:Fenoterol; D009921:Metaproterenol; D013806:Theophylline; D013726:Terbutaline