Rapid screening of doping agents in human urine by vacuum MALDI-linear ion trap mass spectrometry

Hari Kosanam, P. K.Sai Prakash, Charles Yates, Duane Miller, Suma Ramagiri

Research output: Contribution to journalArticle

29 Citations (Scopus)

Abstract

Detection of doping agents in urine frequentiy requires extensive separation prior to chemical analyses. Gas or liquid chromatography coupled to mass spectrometry has produced accurate and sensitive assays, but chromatographic separations require time and, sometimes, chemical derivatization. To avoid such tedious and lengthy procedures, vacuum matrix-assisted laser desorption ionization (vMALDI) coupled with the linear ion trap mass spectrometry (LIT/MS) technique is tested for its applicability as a rapid screening technique. Commonly used doping agents like nandrolone, boldenone, trenbolone, testosterone, and betamethasone were chosen as study compounds. Different MALDI matrixes like α-cyano-4-hydroxycinnamic acid (CHCA), dihyroxy benzoic acid (DHB) with and without cetyl trimethyl ammonium bromide (CTAB), a surfactant, and meso-tetrakis(pentafluorophenyl) porphyrin (F20TPP) were tested. Among them, F20TPP (MW 974.57 Da) was selected as the preferred matrix owing to the lack of interfering matrix peaks at the lower mass range (m/z 100-700). Urine samples spiked with study compounds were processed by solid-phase extraction (SPE) and consistently detected through a linear range of 0.1-100 ng/mL. The limit of detection and lower limit of quantification for all five analytes have been determined to be 0.03 and 0.1 ng/mL, respectively, in urine samples. Testosterone-d3 was used as an internal standard, and the quantitative measurements were achieved by the selective reaction monitoring (SRM) mode. The method was validated and showed consistency in the results. Hence, vMALDI-LIT/MS can be used as a rapid screening method to complement the traditional GC/MS and LC/MS techniques for simultaneous identification, confirmation, and quantification of doping agents in urine.

Original languageEnglish (US)
Pages (from-to)6020-6026
Number of pages7
JournalAnalytical Chemistry
Volume79
Issue number15
DOIs
StatePublished - Aug 1 2007

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Mass spectrometry
Screening
Doping (additives)
Vacuum
Ions
Ionization
Testosterone
Desorption
Trenbolone Acetate
Nandrolone
Betamethasone
Benzoic Acid
Lasers
Liquid chromatography
Porphyrins
Surface-Active Agents
Gas chromatography
Assays
Monitoring
boldenone

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry

Cite this

Rapid screening of doping agents in human urine by vacuum MALDI-linear ion trap mass spectrometry. / Kosanam, Hari; Prakash, P. K.Sai; Yates, Charles; Miller, Duane; Ramagiri, Suma.

In: Analytical Chemistry, Vol. 79, No. 15, 01.08.2007, p. 6020-6026.

Research output: Contribution to journalArticle

Kosanam, Hari ; Prakash, P. K.Sai ; Yates, Charles ; Miller, Duane ; Ramagiri, Suma. / Rapid screening of doping agents in human urine by vacuum MALDI-linear ion trap mass spectrometry. In: Analytical Chemistry. 2007 ; Vol. 79, No. 15. pp. 6020-6026.
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