Gerhardt K, Ludwig-Köhn H, Henning H V, Remberg G, Zeeck A
Department of Internal Medicine, University of Göttingen, FRG.
Biomed Environ Mass Spectrom. 1989 Feb;18(2):87-95. doi: 10.1002/bms.1200180202.
Oestrogen metabolites from the urine of males and pregnant and non-pregnant females were enriched by a procedure involving column chromatography on adsorber resins, gels and ion exchangers, enzymatic solvolysis and extraction, thereby separating the oestrogens from most of the interfering material. After derivatization of the oestrogens as their trimethylsilyl ethers profiles were measured with a fused silica column and a flame ionization detector by gas chromatography. Using a combination of capillary gas chromatography and mass spectrometry approximately 50 oestrogen metabolites were detected in the human urine of males and females, of which 19 were unknown urine compounds. Not all could be identified definitely owing to the lack of reference material. Mass spectra of trimethylsilylated oestrogens with functional groups at position 11 (11-dehydroestradiol, 11-dehydroestrone and 11 beta-hydroxyestrone) were discussed in their common and discernible fragmentations.
通过一种涉及在吸附树脂、凝胶和离子交换剂上进行柱色谱、酶促溶剂分解和萃取的方法，富集男性以及怀孕和未怀孕女性尿液中的雌激素代谢物，从而将雌激素与大多数干扰物质分离。雌激素经衍生化为其三甲基硅烷基醚后，用熔融石英柱和火焰离子化检测器通过气相色谱法测定其图谱。结合毛细管气相色谱法和质谱法，在男性和女性的人类尿液中检测到约50种雌激素代谢物，其中19种是未知的尿液化合物。由于缺乏参考物质，并非所有代谢物都能被明确鉴定。讨论了在第11位带有官能团的三甲基硅烷基化雌激素（11-脱氢雌二醇、11-脱氢雌酮和11β-羟基雌酮）的常见且可辨别的碎片质谱。
