تسجيل الدخول

تسجيل

Liquid chromatography–mass spectrometry

المؤلف:  Sue Jickells , Adam Negrusz (Editors)

المصدر:  Clarkes Analytical Forensic Toxicology

الجزء والصفحة:  p276-277

2026-10-24

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Liquid chromatography–mass spectrometry

With the development of atmospheric-pressure ionisation techniques, LC-MS has found increasing application in doping control in animal and human sports for both the qualitative and quantitative analysis of drugs. Screening methods have been developed in animal sports testing for corticosteroids (Tang et al. 2001) and diuretics (Eenoo et al. 2001). Methods developed for individual drugs include hydrocortisone (Samuels et al. 1994), triamcinolone acetonide (Koupai-Abyazani et al. 1994b), levodopa and its metabolites (Koupai-Abyazani et al. 1994a), clidinium bromide (Ryan et al. 1996) and glycopyrrolate (Teale and Houghton 1994). The technique has also been applied to the analysis of intact steroid conjugates isolated from horse urine with particular reference to the quantification of testosterone sulfate (Dumasia et al. 1996). Product-ion scan MS/MS has facilitated the development of screening procedures for large numbers of compounds in a single analysis. Leung et al. (2007) reported the high throughput screening of 75 basic drugs in equine plasma by LC-ESI-MS/MS, with sub-parts per billion levels of detection. LC-ESI-MS/MS has also been used for the analysis of eight major anabolic steroids with three ion transitions used for confirmation (Guan et al. 2005). The limit of quantification was 25 pg/mL for boldenone; 50 pg/mL for normethandrolone, nandrolone and methandienone, and 100 pg/mL for testosterone, tetrahydrogestrinone, trenbolone and stanozolol. In human sports drug testing, LC-MS and LC MS/MS are being used increasingly in several areas. Barron et al. (1996) developed a direct method to determine anabolic steroids in human urine by on-line SPE LC-MS. Thevis et al. (2001) used LC-MS/MS for the rapid screening of samples for beta-blockers. Diuretics have been screened by LC-MS techniques (Ventura et al. 1991) and by LC-MS/MS (Thieme et al. 2001). The sulfate conjugate of 19-norandrosterone has been analysed by LC-MS/MS in negative electro spray ionisation mode (Strahm et al., 2007) with a lower limit of quantification of 200 pg/mL, emphasising the applicability of LC-MS for the analysis of drug conjugates. The role of LC MS(/MS) in doping control has been reviewed by Thevis and Schanzer (2007).