Chang Hong, Wu Shimin, Hu Jianying, Asami Mari, Kunikane Shoichi
College of Urban and Environmental Sciences, Peking University, Beijing 100871, China.
J Chromatogr A. 2008 Jun 27;1195(1-2):44-51. doi: 10.1016/j.chroma.2008.04.055. Epub 2008 Apr 25.
A sensitive ultra-performance liquid chromatography-electrospray tandem mass spectrometry method, combined with solid-phase extraction and silica cartridge cleanup, was established for nine androgens (androstenedione, 19-nor-4-androstene-3,17-diol, androsterone, epiandrosterone, testosterone, methyltestosterone, trenbolone, nandrolone, stanozolol) and nine progestogens (progesterone, 17alpha-hydroxyprogesterone, 21alpha-hydroxyprogesterone, 6alpha-methyl-hydroxyprogesterone, 17alpha,20beta-dihydroxy-4-pregnene-3-one, megestrol acetate, norethindrone, norgestrel, medroxyprogesterone acetate) in environmental waters. For the various water matrices considered, the overall method recoveries were from 78 to 100%, and no apparent signal suppression was found. The method detection limits for the eighteen analytes in the influent, effluent and surface water samples were 0.20-50, 0.04-20 and 0.01-12 ng/L, respectively. This method was used to analyze the residual androgens and progestogens in the wastewater and surface water samples from Japan, and ten analytes (0.03 (medroxyprogesterone acetate)-1441 ng/L (androsterone)) were detected in the wastewater samples, and four analytes (0.06 (progesterone)-0.46 ng/L (androstenedione)) were detected in the surface water samples.
建立了一种灵敏的超高效液相色谱-电喷雾串联质谱法，结合固相萃取和硅胶柱净化，用于测定环境水体中的9种雄激素（雄烯二酮、19-去甲-4-雄烯-3,17-二醇、雄酮、表雄酮、睾酮、甲基睾酮、群勃龙、诺龙、司坦唑醇）和9种孕激素（孕酮、17α-羟基孕酮、21α-羟基孕酮、6α-甲基-羟基孕酮、17α,20β-二羟基-4-孕烯-3-酮、醋酸甲地孕酮、炔诺酮、左炔诺孕酮、醋酸甲羟孕酮）。对于所考虑的各种水体基质，该方法的总体回收率为78%至100%，未发现明显的信号抑制。进水、出水和地表水样品中18种分析物的方法检出限分别为0.20 - 50、0.04 - 20和0.01 - 12 ng/L。该方法用于分析日本废水和地表水样品中的残留雄激素和孕激素，在废水样品中检测到10种分析物（0.03（醋酸甲羟孕酮）- 1441 ng/L（雄酮）），在地表水样品中检测到4种分析物（0.06（孕酮）- 0.46 ng/L（雄烯二酮））。
