Vulliet Emmanuelle, Baugros Jean-Baptiste, Flament-Waton Marie-Magdeleine, Grenier-Loustalot Marie-Florence
Service Central d'Analyse du CNRS-USR59, Chemin du Canal, BP 22, 69390, Vernaison, France.
Anal Bioanal Chem. 2007 Mar;387(6):2143-51. doi: 10.1007/s00216-006-1084-z. Epub 2007 Jan 16.
An analytical method for the determination of 12 selected estrogens, progestagens and corticosteroids is presented. The optimization of the method, including liquid chromatography separation, extraction on a solid phase, purification on a silica gel cartridge and detection by mass spectrometry, is described. Both the repeatability, with relative standard deviation ranging from 1.4 to 2.7%, and the accuracy, with recoveries ranging from 92.7 to 102.4%, were very satisfactory for ten of the target analytes. The limits of detection were lower than 1 ng/L for progestagens, androgens and corticosteroids, and ranged between 0.9 and 4.3 ng/L for estrogens. The results of the analysis of two sewage treatment plants in the area of Lyon (France) by this method reveal that all the compounds investigated are present in the effluents. The estrogen most frequently detected was estrone, with a median of 26.1 ng/L. The target progestagens were detected with concentrations ranging between 5 and 41 ng/L. Androgens were also present in most of the samples in the range 1-30 ng/L, while the corticosteroids were present only in one plant, with a median of 31.9 ng/L.
本文介绍了一种用于测定12种选定雌激素、孕激素和皮质类固醇的分析方法。描述了该方法的优化过程,包括液相色谱分离、固相萃取、硅胶柱净化以及质谱检测。对于十种目标分析物,该方法的重复性(相对标准偏差范围为1.4%至2.7%)和准确度(回收率范围为92.7%至102.4%)均非常令人满意。孕激素、雄激素和皮质类固醇的检测限低于1 ng/L,雌激素的检测限在0.9至4.3 ng/L之间。采用该方法对法国里昂地区的两家污水处理厂进行分析的结果表明,所有研究的化合物均存在于污水排放物中。最常检测到的雌激素是雌酮,中位数为26.1 ng/L。目标孕激素的检测浓度范围为5至41 ng/L。大多数样品中也存在雄激素,浓度范围为1至30 ng/L,而皮质类固醇仅在一家工厂的样品中出现,中位数为31.9 ng/L。