Screening of β-2 agonists and confirmation of fenoterol, orciprenaline, reproterol and terbutaline with gas chromatography-mass spectrometry as tetrahydroisoquinoline derivatives

被引:35
作者
Henze, MK
Opfermann, G
Spahn-Langguth, H
Schänzer, W
机构
[1] Deutsch Sport Hsch, Inst Biochem, D-50933 Cologne, Germany
[2] Univ Halle Wittenberg, Inst Pharmazeut Chem, Halle, Saale, Germany
来源
JOURNAL OF CHROMATOGRAPHY B | 2001年 / 751卷 / 01期
关键词
derivatisation; GC; beta-2; agonists; fenoterol; orciprenaline; reproterol; terbutaline; tetrahydroisoquinoline;
D O I
10.1016/S0378-4347(00)00452-7
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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. (C) 2001 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:93 / 105
页数:13
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