Analysis of trenbolone acetate metabolites and melengestrol in environmental matrices using gas chromatography–tandem mass spectrometry

Studies demonstrate that exposure to steroid hormones in receiving waters can adversely impact reproduction of aquatic organisms. In particular, exogenous steroid hormones widely used as growth promoters in animal agriculture are of high concern, yet no gas chromatography–tandem mass spectrometry (G...

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Published in:	Talanta (Oxford) Vol. 99; pp. 238 - 246
Main Authors:	Parker, Jed A., Webster, Jackson P., Kover, Stephanie C., Kolodziej, Edward P.
Format:	Journal Article
Language:	English
Published:	Amsterdam Elsevier B.V 15-09-2012 Elsevier
Subjects:	Analytical chemistry Animals Applied sciences Chemistry Chromatographic methods and physical methods associated with chromatography Endocrine disruption Environment Environmental Pollutants - analysis Environmental Pollutants - isolation & purification Exact sciences and technology Gas chromatographic methods Gas Chromatography-Mass Spectrometry - methods Global environmental pollution Growth promoters Melengestrol Acetate - analysis Melengestrol Acetate - isolation & purification Pollution Spectrometric and optical methods Steroid hormones Tandem Mass Spectrometry - methods Trenbolone Trenbolone Acetate - analysis Trenbolone Acetate - isolation & purification Trenbolone Acetate - metabolism Trendione CAFOs MGA Growth promoters Endocrine disruption MRM SPE MSTFA Trendione Trenbolone GC/MS/MS TBA S/N LC MDLs TMS GC/MS Steroid hormones Steroid Organic matter Chemical analysis Animal feeding Metabolite Surface analysis Derivatization Replica method Sample preparation Standard deviation Quantitative analysis Iodine Implant Steroid hormone Sample Use Isotope dilution Exposure Acetamide Acetate Concentration Gas chromatography Soils Animal Mass spectrometry MS/MS Surface water Analytical method Environment Detection Mass spectrometry
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Summary:	Studies demonstrate that exposure to steroid hormones in receiving waters can adversely impact reproduction of aquatic organisms. In particular, exogenous steroid hormones widely used as growth promoters in animal agriculture are of high concern, yet no gas chromatography–tandem mass spectrometry (GC/MS/MS) analytical methods for the detection of these compounds in complex environmental matrices is described in the literature. This study utilizes analytical methods based upon N-methyl-N-(trimethylsilyl)trifluoro-acetamide-iodine (MSTFA-I2) derivatization for the analysis of metabolites of trenbolone acetate (TBA), including 17α-trenbolone, 17β-trenbolone, and trendione, and melengestrol acetate in receiving waters and surface soils associated with animal agriculture. Results suggest method detection levels of 0.5–1ng/L for the trenbolone metabolites, while detection of melengestrol is qualitative only. Isotope dilution methods employing d3-17β-trenbolone were used to improve steroid quantification. Method recoveries in spiked samples collected from a variety of representative receiving waters generally ranged from 80–120% with consistent and low standard deviation (generally<10%) for replicate analysis. Analysis of a storm water runoff sample from a commercial confined animal feeding operation (CAFO) that used TBA implants detected 17β-trenbolone and trendione at concentrations of 31 and 52ng/L, respectively. Analysis of surface soils at a commercial CAFO using TBA implants detected 17α-trenbolone at concentrations between 4–6ng/g dry weight. Method development efforts suggested that the concentration of I2 in MSTFA, the removal of I2 from sample extracts after derivatization, and the use of Florisil clean-up to reduce organic matter matrix were vital aspects of steroid hormone quantification at low (<30ng/L) concentrations in complex environmental matrices. ► Analysis of trenbolone acetate metabolites and melengestrol by GC–MS/MS is described. ► Limits of detection for steroid analytes are near 1ng/L in environmental samples. ► Trenbolone metabolites can occur near animal agriculture facilities.
Bibliography:	ObjectType-Article-1 SourceType-Scholarly Journals-1 ObjectType-Feature-2 content type line 23
ISSN:	0039-9140 1873-3573
DOI:	10.1016/j.talanta.2012.05.046