The Institute of Environmental and Human Health, Department of Environmental Toxicology, Texas Tech University, Lubbock, TX 79416, United States.
Talanta. 2011 Sep 15;85(3):1317-23. doi: 10.1016/j.talanta.2011.06.011. Epub 2011 Jun 14.
Trenbolone acetate (TbA) is a potent synthetic anabolic steroid that was approved by the FDA as a growth promoter in beef cattle in 1987. Given the endocrine-modulating activity of TbA and its metabolites in all vertebrates, a sensitive and reliable analytical method is needed to detect TbA and related residues in environmental matrices. We have developed a method that incorporates solid phase extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of the three major TbA metabolites (trendione, 17β-trenbolone, 17α-trenbolone) in total suspended particulate matter (TSP) samples. Sample preparation involved pressurized liquid extraction followed by cleanup on solid-phase extraction cartridges. The procedure was optimized to obtain maximum recovery and minimum signal suppression/enhancement from matrix effects. Analytes were separated with a Phenomenex Gemini-NX C18 analytical column (150 mm × 2.0 mm, 3 μm particle size) using an aqueous methanol gradient at a flow rate of 0.2 mL/min. Column effluent underwent positive electrospray ionization (ESI). Two or more diagnostic product ions were acquired from analyte specific precursor ions for unambiguous confirmation and quantification. The method detection limit was 3.27-4.87 ng/g of particulate matter (PM). Method accuracy, determined with analyte recoveries, ranged between 68% and 117%, and method precision, expressed as relative standard deviation, was below 15% at spiked levels of 6.67, 33.3, and 167 ng/g PM. Analysis of TSP samples demonstrated the presence of the target species associated with PM in the vicinity of beef cattle feeding operations.
醋酸群勃龙（TbA）是一种强效的合成同化类固醇，1987 年被 FDA 批准作为牛的生长促进剂。鉴于 TbA 及其代谢物在所有脊椎动物中的内分泌调节活性，需要一种灵敏可靠的分析方法来检测环境基质中的 TbA 和相关残留。我们开发了一种方法，该方法结合固相萃取和液相色谱-串联质谱（LC-MS/MS），用于同时测定总悬浮颗粒物（TSP）样品中的三种主要 TbA 代谢物（群勃龙、17β-群勃龙、17α-群勃龙）。样品制备涉及加压液体萃取，然后用固相萃取小柱进行净化。该程序经过优化，以从基质效应中获得最大的回收率和最小的信号抑制/增强。分析物在 Phenomenex Gemini-NX C18 分析柱（150mm×2.0mm，3μm粒径）上用含甲醇的水溶液梯度洗脱，流速为 0.2mL/min。柱洗脱液进行正电喷雾电离（ESI）。从分析物特定的前体离子中获得两个或更多个诊断产物离子，以进行明确的确认和定量。方法检测限为 3.27-4.87ng/g 颗粒物（PM）。用分析物回收率确定的方法准确性在 68%-117%之间，方法精密度（以相对标准偏差表示）在 6.67、33.3 和 167ng/g PM 加标水平下低于 15%。对 TSP 样品的分析表明，在牛饲养作业附近的 PM 中存在与目标物质相关的物质。
