Chemistry Department, Oregon State University, Corvallis, Oregon 97331-4003, USA.
Anal Chem. 2011 Apr 1;83(7):2622-30. doi: 10.1021/ac103013h. Epub 2011 Mar 10.
A new method was developed for the analysis of natural and synthetic androgenic steroids and their selected metabolites in aquatic environmental matrixes using direct large-volume injection (LVI) high-performance liquid chromatography (HPLC) tandem mass spectrometry (MS/MS). Method accuracy ranged from 87.6 to 108% for analytes with well-matched internal standards. Precision, quantified by relative standard deviation (RSD), was less than 12%. Detection limits for the method ranged from 1.2 to 360 ng/L. The method was demonstrated on a series of 1 h composite wastewater influent samples collected over a day with the purpose of assessing temporal profiles of androgen loads in wastewater. Testosterone, androstenedione, boldenone, and nandrolone were detected in the sample series at concentrations up to 290 ng/L and loads up to 535 mg/h. Boldenone, a synthetic androgen, had a temporal profile that was strongly correlated to testosterone, a natural human androgen, suggesting its source may be endogenous. An analysis of the sample particulate fraction revealed detectable amounts of sorbed testosterone and androstenedione. Androstenedione sorbed to the particulate fraction accounted for an estimated 5 to 7% of the total androstenedione mass.
开发了一种新方法，用于使用直接大体积进样（LVI）高效液相色谱（HPLC）串联质谱（MS/MS）分析水生环境基质中的天然和合成雄激素类固醇及其选定代谢物。对于具有匹配良好的内标物的分析物，方法准确度范围为 87.6%至 108%。通过相对标准偏差（RSD）量化的精密度小于 12%。该方法的检测限范围为 1.2 至 360 ng/L。该方法在一天内采集的一系列 1 小时复合废水进水样本上进行了验证，目的是评估废水中雄激素负荷的时间分布。在样品系列中检测到浓度高达 290 ng/L 且负荷高达 535 mg/h 的睾酮、雄烯二酮、宝丹酮和诺龙。宝丹酮是一种合成雄激素，其时间分布与天然雄激素睾酮强烈相关，表明其来源可能是内源性的。对样品颗粒部分的分析显示可检测到吸附的睾酮和雄烯二酮。吸附到颗粒部分的雄烯二酮估计占总雄烯二酮质量的 5%至 7%。
