Gas chromatographic-tandem mass spectrometric determination of anabolic steroids and their esters in hair - Application in doping control and meat quality control

100-mg amount of powdered hair was treated with methanol in an ultrasonic b ath for extraction of esters, then alkaline digested with 1 M NaOH for an o ptimum recovery of other drugs. The two liquid preparations were subsequent ly extracted with ethyl acetate, pooled, then Finally highly purified using a twin solid-phase extraction on amino and silica cartridges. The residue was derivatized with N-methyl-N(trimethylsilyl)-trifluoracetamide (MSTFA) p rior to injection. Analysis was conducted by gas chromatography coupled to a triple quadrupole mass spectrometer. The generally chosen parent ion was the molecular ion while two daughter ions were selected for each compound w ith collision energies ranging from -16 to -21 eV. Internal standards were nandrolone d(3) for non-esterified drugs and testosterone phenyl propionate for esters. The limits of detection calculated from an analysis of the bla nks (n = 30) were 0.08 pg/mg for nandrolone, 6.20 pg/mg for boldenone, 0.07 pg/mg for methyl testosterone, 0.15 pg/mg for ethinyl estradiol, 2.10 pg/m g for metandienone, 0.86 pg/mg for testosterone propionate, 0.95 pg/mg for testosterone cypionate, 1.90 pg/mg for nandrolone decanoate, 3.10 pg/mg for testosterone decanoate and 4.80 pg/mg for testosterone undecanoate. Applic ation to doping control has been demonstrated. In a series of 18 sportsmen, two tested positive for anabolic steroids in hair whereas urinalysis was n egative for both of them. The first positive case was nandrolone and the se cond case concerned the identification of testosterone undecanoate. Measure d in 10 white males aged between 22 and 31 years, the testosterone concentr ation was in the range 1.7-9.2 pg/mg (mean=5.0 pg/mg). The method was also applied in meat quality control. Of the 187 analyses realized based upon ha ir and urine sampling in slaughter houses, 23 were positive for anabolic st eroids in hair: one case for boldenone, one case for metandienone, two case s for testosterone propionate, three cases for nandrolone, five cases for t estosterone decanoate and 11 cases for methyl testosterone. in the meantime , urinalysis was always negative for these drugs or their metabolites. (C) 1999 Elsevier Science B.V. All rights reserved.