Comprehensive screening of anabolic steroids, corticosteroids, and acidic drugs in horse urine by solid-phase extraction and liquid chromatography-mass spectrometry

被引:96
作者
Ho, Emmie N. M. [1 ]
Leung, David K. K. [1 ]
Wan, Terence S. M. [1 ]
Yu, Nola H. [1 ]
机构
[1] Sha Tin Racecourse, Hong Kong Jockey Club, Racing Lab, Shatin, Hong Kong, Peoples R China
关键词
acidic drugs; anabolic steroids; corticosteroids; horse urine; liquid chromatography-mass spectrometry;
D O I
10.1016/j.chroma.2006.03.089
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
This paper reports two highly efficient liquid chromatography-mass spectrometry (LC-MS) methods for the screening of anabolic steroids, corticosteroids, and acidic drugs for the purpose of doping control in equine sports. Sample extraction was performed using a mixed-mode C8-SCX solid-phase extraction (SPE) cartridge. The first eluted fraction (acidic/neutral fraction) was base-washed and the resulting organic extract was used for the screening of anabolic steroids and corticosteroids by LC-MS using multiple reaction monitoring (MRM) in the positive electrospray ionisation (ESI) mode. The remaining aqueous extract was re-adjusted to pH 6 and acidic drugs were recovered by liquid/liquid extraction. Detection was again achieved using LC-MRM but in the negative ESI mode. A total of 40 anabolic steroids and corticosteroids, and over 50 acidic drugs, including some cyclooxygenase-2 (COX-2) inhibitors, oxicams, anti-diabetics, sedatives, diuretics and Delta(9)-tetrahydro-11-norcannabinol-9-carboxylic acid, could be covered by the two LC-MS methods. Both methods utilized a high efficiency reversed-phase column (3.3 cm L x 2.1 mm I.D. with 3 mu m particles) coupled with a fast-scanning triple-quadrupole mass spectrometer to achieve fast turnaround times. The overall turnaround times for both methods were 10 min, inclusive of post-run and equilibration times. (c) 2006 Elsevier B.V. All rights reserved.
引用
收藏
页码:38 / 53
页数:16
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