Chinese Journal of Chromatography 2006-01-01

[Determination of anabolic steroid hormones in animal muscle tissues by gas chromatography/mass spectrometry].

Jie Chen, Yan Qin, Meijin Zhang

文献索引：Se Pu 24(1) , 19-22, (2006)

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摘要

A gas chromatography/mass spectrometry (GC/MS) method was developed for the determination of multi-residues of steroid anabolic hormones epitestosterone (ETS), testosterone 17-propionate (PTS), nandrolone (17beta-NT), 17alpha-methyltestosterone (MTS), 17beta-estradiol (17beta-ES), estriol ( EST), 17alpha-ethinylestradiol (EES), estrone (ESN) and 17beta-estradiol 3-benzoate (BES) in the muscle tissues of various animal species. Homogenized tissue samples were enzymatically digested in acetate buffer (pH 5.0). Consequently, methanol was added and the mixtures were extracted under ultrasonication incubation. Clean-up was carried out for at least two times with methyl tert-butyl ether (MTBE) liquid-liquid partitioning followed by a reversed-phase solid phase extraction (SPE) cartridge purification. The eluate with methanol was evaporated to dryness by N2 at 40 degrees C and derivatization was achieved with N-methyl-N-( trimethylsilyl) trifluoroacetamide/iodotrimethylsilane/dithioerythritol (MSTFA-TMIS-DTE) at 60 degrees C for 45 min. The reaction mixture was injected into a gas chromatograph with a DB-1 capillary column coupled with a mass spectrometer. The samples were tested by different selected ion monitoring modes with electron impact (EI) source for the androgens and estrogens. The limits of quantitation (LOQ) for the above 9 hormones were in the range of 1.0 - 2.0 microg/kg. At the 2.0 microg/kg LOQ spiked level, the mean recoveries were within 62.5% - 80.5%, and the relative standard deviations were within 12.5% - 26.8%. The real sample tests showed this method can be used for the sensitive and accurate determination of multi-steroid anabolic hormones residues in biological muscle samples.