Massé R, Laliberté C, Tremblay L, Dugal R
Biomed Mass Spectrom. 1985 Mar;12(3):115-21. doi: 10.1002/bms.1200120305.
A sensitive and highly specific method based on capillary column gas chromatography/mass spectrometry has been developed for the detection of 19-nortestosterone (17 beta-hydroxy-4-estren-3-one) metabolites in urine. After intramuscular administration of 19-nortestosterone decanoate to man, urine samples were collected during several days and treated with Helix pomatia digestive juice. The free steroids were extracted and converted into O-methyl-oxime-trimethylsilyl or the trimethylsilyl ether derivatives and analysed by capillary column gas chromatography/mass spectrometry (GC/MS). Three isomeric metabolites were detected and identified as 3 alpha-hydroxy-5 alpha-extran-17-one (19-norandrosterone), 3 alpha-hydroxy-5 beta-estran-17-one (19-noretiocholanolone) and 3 beta-hydroxy-5 alpha-estran-17-one (19-norepiandrosterone). Packed column GC/MS was also employed in the selected ion monitoring mode for the specific detection of 19-norandrosterone, the most abundant urinary metabolite of 19-nortestosterone. These gas chromatographic/mass spectrometric methods are highly specific tests which can be used on a routine basis for the confirmation of 19-nortestosterone administration to athletes as well as for therapeutic monitoring following administration of the drug.
已开发出一种基于毛细管柱气相色谱/质谱联用的灵敏且高度特异的方法，用于检测尿液中的19-去甲睾酮（17β-羟基-4-雌烯-3-酮）代谢物。给男性肌肉注射癸酸诺龙后，连续数天收集尿液样本，并用罗马蜗牛消化液处理。游离类固醇经提取后转化为O-甲基肟-三甲基硅烷基或三甲基硅烷基醚衍生物，然后通过毛细管柱气相色谱/质谱联用（GC/MS）进行分析。检测并鉴定出三种异构体代谢物，分别为3α-羟基-5α-雌烷-17-酮（19-去甲雄酮）、3α-羟基-5β-雌烷-17-酮（19-去甲本胆烷醇酮）和3β-羟基-5α-雌烷-17-酮（19-去甲表雄酮）。填充柱GC/MS也用于选择离子监测模式，以特异性检测19-去甲雄酮，它是19-去甲睾酮在尿液中含量最高的代谢物。这些气相色谱/质谱联用方法是高度特异的检测方法，可常规用于确认运动员是否使用了19-去甲睾酮，以及在用药后进行治疗监测。
