Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometric detection for the determination of anabolic steroids and related compounds in nutritional supplements

Abstract

A simple and effective analytical method for the determination of anabolic steroids and related compounds in nutritional supplements is reported. Target compounds are extracted with ethyl acetate, crude extract is purified using dispersive solid-phase extraction (SPE) with primary secondary amine (PSA) as sorbent, and finally they are identified and quantified as underivatized compounds using two-dimensional gas chromatography with time-of-flight mass spectrometric detection (GCxGC-TOF MS). This method was validated for 25 steroids in two types of commercially available solid nutritional supplements: protein concentrate and creatine monohydrate. Repeatability expressed as the relative standard deviation of analyte concentration ranged from 4.1 to 20.5%. Recoveries between 70.0 and 122.6% were obtained for the target compounds except for oxymetholone in protein concentrate where the recovery was low as a result of strong interactions with PSA. Excellent linearity was obtained for six-point calibration with regression coefficients of 0.997-1.000 for all compounds. The limits of quantification ranged from 0.007 to 0.114 mg kg(-1). For a monitoring programme of 48 samples of nutritional supplements, three were positive. Nandrolone, testosterone, dehydroepiandrosterone (DHEA), 5alpha-androstan-3,17-dione, 19-norandrostendione and progesterone were found in positive samples at concentrations between 0.022 and 0.398 mg kg(-1).

A new and improved strategy combining a dispersive-solid phase extraction-based multiclass method with ultra high pressure liquid chromatography for analysis of low molecular weight polyphenols in vegetables

“…This procedure involves initial single phase extraction with acetonitrile followed by salting-out extraction/partitioning by addition of MgSO 4 plus NaCl, and finally using dispersive-solid-phase extraction (dSPE) for clean-up. In addition to pesticide multiresidue analysis in foodstuffs [27][28][29][30][31][32][33][34], QuEChERS concepts have been used for acrylamide [35,36], clinical [37], veterinary drug residue [38,39], food quality [40], supplement testing [41], perfluorinated compounds [42,43], alkaloids [44], environmental and mycotoxins [45][46][47] analytical applications. However, up to date no studies using the QuECh-ERS technique coupled to dSPE for the analysis of free LMW-PPs in vegetables or another kind of matrices have been published.…”

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.…”

Comprehensive two dimensional gas chromatography review

“…Stepan et al [83] analyzed nutritional supplements for prohibited anabolic steroids that are listed by the World Anti-Doping Agency. Existing methods require cleanup and derivatization prior to GC-MS.…”