Comprehensive screening of anabolic steroids, corticosteroids, and acidic drugs in horse urine by solid-phase extraction and liquid chromatography-mass spectrometry.
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 microm 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.
Ho
Emmie N M
EN
Racing Laboratory, The Hong Kong Jockey Club, Sha Tin Racecourse, Sha Tin, N.T., Hong Kong, PR China. emmie.nm.ho@hkjc.org.hk
Leung
David K K
DK
Wan
Terence S M
TS
Yu
Nola H
NH
D000305:Adrenal Cortex Hormones / Q000008:administration & dosage / Q000737:chemistry / Q000652:urine*; D045930:Anabolic Agents / Q000008:administration & dosage / Q000737:chemistry / Q000652:urine*; D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004300:Doping in Sports; D006736:Horses; D015394:Molecular Structure; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013256:Steroids / Q000008:administration & dosage / Q000737:chemistry / Q000652:urine; D015813:Substance Abuse Detection / Q000379:methods*
D000305:Adrenal Cortex Hormones; D045930:Anabolic Agents; D013256:Steroids