High sensitive analysis of steroids in doping control using gas chromatography/time‐of‐flight mass‐spectrometry

Abstract

The method of high sensitive gas chromatographic/time-of-flight mass-spectrometric (GC/TOF-MS) analysis of steroids was developed. Low-resolution TOF-MS instrument (with fast spectral acquisition rate) was used. This method is based on the formation of the silyl derivatives of steroids; exchange of the reagent mixture (pyridine and N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA)) for tert-butylmethylether; offline large sample volume injection of this solution based on sorption concentration of the respective derivatives from the vapour-gas mixture flow formed from the solution and inert gas flows; and entire analytes solvent-free concentrate transfer into the injector of the gas chromatograph. Detection limits for 100 µl sample solution volume were 0.5-2 pg/µl (depending on the component). Application of TOF-MS model 'TruTOF' (Leco, St Joseph, MO, USA) coupled with gas chromatograph and ChromaTOF software (Leco, St Joseph, MO, USA) allowed extraction of the full mass spectra and resolving coeluted peaks. Due to use of the proposed method (10 µl sample aliquot) and GC/TOF-MS, two times more steroid-like compounds were registered in the urine extract in comparison with the injection of 1 µl of the same sample solution.

Sensitivity of GC‐EI/MS, GC‐EI/MS/MS, LC‐ESI/MS/MS, LC‐Ag+CIS/MS/MS, and GC‐ESI/MS/MS for analysis of anabolic steroids in doping control

“…Numerous analytical methods have been developed and applied to steroids analysis using various instrumental set‐ups including chromatography and mass spectrometry. Gas chromatography‐electron ionization/mass spectrometry (GC‐EI/MS) with trimethylsilylation (TMS) derivatives is the traditional technique used to detect anabolic steroids . Recently, gas chromatography‐electron ionization/tandem mass spectrometry (GC‐EI/MS/MS) has been shown to be a powerful analytical method for steroid analysis .…”

Current Status and Bioanalytical Challenges in The Detection of Unknown Anabolic Androgenic Steroids in Doping Control Analysis

“…Hence, the development of full acquisition methods based on HR instru ments is a promising alternative, not only for the open detection of AAS but also for the compre hensive target screening in doping control ana lysis (Table 2) [50][51][52][53][54][55][56][57][58][59][60][61][62][63][64][65][66]. Their modus operandi is the acquisition of the fullscan raw data and, therefore, the detection of all compounds ion ized by the source.…”

“…Bioanalytical challenges in the detection of unknown anabolic androgenic steroids | Review www.future-science.com Theoretically application [50] Dilute and shoot Positive samples [59] Dilute and shoot …”

Doping control analysis of anabolic steroids in equine urine by gas chromatography‐tandem mass spectrometry

“…The effective screening of anabolic steroids in doping control is critical, as according to the recently published Anti‐Doping Testing Figures Report by WADA, anabolic agents are still the most reported misused prohibited substances amongst all substance groups. The conventional method for the detection of anabolic steroids in biological samples is by the use of gas chromatography‐mass spectrometry (GC‐MS) . Liquid chromatography‐mass spectrometry (LC‐MS) has become a compatible technique for doping control testing in sports in recent years as LC‐MS has the ability to handle heat labile and large biomolecules, with faster instrument turnaround time and better sensitivity .…”