Central Agricultural Office Food and Feed Safety Directorate, Mester utca 81, Budapest 1092, Hungary.
Chemosphere. 2010 Feb;78(8):972-9. doi: 10.1016/j.chemosphere.2009.12.025. Epub 2010 Jan 13.
The assessment of steroidal hormones in the environment requires sensitive and selective analytical techniques suitable for sample matrices. This paper reports a simple method to analyze simultaneously six corticosteroids (triamcinolone, cortisol, dexamethasone, flumethasone, prednisolone, triamcinolone acetonide), four androgens (boldenone, epitestosterone, methyltestosterone, nortestosterone), and progesterone in river and drinking water sources. The developed method is based on a single solid-phase extraction (SPE) followed by liquid chromatography/tandem mass spectrometry (LC-MS/MS) with atmospheric pressure chemical ionization (APCI). The main advantage of this method over other methods includes the use of a single SPE with a low volume cartridge for sample preparation, separation of steroids on alkyl-amide stationary phase with no matrix interferences by LC-MS/MS analysis, and simultaneous analysis of more than two groups of steroids. The method was characterized by generally good performance, analyzing three groups of steroids using 100 and 1000mL samples with average recovery ranges of 80-109% and 68-126%, respectively at a level of 1ngL(-1). The limit of detection (LOD) ranged from 0.06 to 0.2 and 0.01-0.21ngL(-1) for 100mL and 1000mL samples volumes, respectively. Sixty samples of Danube River and drinking water sources from different regions of Hungary were collected to analyze target steroids in two sampling periods in 2008 and 2009. Steroids, except cortisol, dexamethasone, flumethasone, prednisolone, epitestosterone and progesterone were below detection limits. Endogenous steroids (cortisol, epitestosterone, progesterone) were present in the concentration range of 0.08-2.67ngL(-1) while synthetic corticosteroids (dexamethasone, flumethasone, and prednisolone) varied from 0.064 to 1.43ngL(-1). Steroids were present in river water, except progesterone, which was present only in ground water. Levels of steroids are compared with other rivers in the world and were briefly discussed.
环境中甾体激素的评估需要适合样品基质的灵敏和选择性分析技术。本文报道了一种简单的方法，可同时分析 6 种皮质甾酮（曲安西龙、皮质醇、地塞米松、氟美松、泼尼松龙、曲安西龙醋酸酯）、4 种雄激素（宝丹酮、表睾酮、甲基睾酮、去甲睾酮）和孕激素在河流和饮用水源中的含量。所开发的方法基于单次固相萃取（SPE），随后进行液相色谱/串联质谱（LC-MS/MS）分析，采用大气压化学电离（APCI）。与其他方法相比，该方法的主要优点包括：使用小体积 SPE 进行样品制备，采用烷基酰胺固定相进行类固醇分离，LC-MS/MS 分析无基质干扰，可同时分析两组以上的类固醇。该方法的性能通常较好，使用 100 和 1000mL 样品分析三组类固醇，平均回收率范围分别为 80-109%和 68-126%，检测水平为 1ngL(-1)。检出限（LOD）范围为 0.06-0.2 和 0.01-0.21ngL(-1)，100 和 1000mL 样品体积的检出限分别为 0.06-0.2 和 0.01-0.21ngL(-1)。采集了来自匈牙利不同地区的多瑙河和饮用水源的 60 个样本，以在 2008 年和 2009 年的两个采样期分析目标类固醇。除皮质醇、地塞米松、氟美松、泼尼松龙、表睾酮和孕激素外，其他类固醇均低于检测限。内源性类固醇（皮质醇、表睾酮、孕激素）浓度范围为 0.08-2.67ngL(-1)，而合成皮质甾酮（地塞米松、氟美松和泼尼松龙）浓度范围为 0.064-1.43ngL(-1)。除孕激素外，类固醇均存在于河水中，而孕激素仅存在于地下水中。与世界上其他河流的类固醇水平进行了比较，并进行了简要讨论。
