尿中睾酮与表睾酮的三甲基硅烷化及其比值的GC—MS测定

TRIMETHYLSILYLATION OF TESTOSTERONE, EPI-TESTOSTERONE AND DETERMINATION OF THEIR RATIO IN URINE BY GC-MS

对睾酮及表睾酮的三甲基硅烷化进行了详细考察,找到了较好的抗氧剂巯基乙醇,确定了较好的衍生化条件,衍生化产物单一。并采用GC—MS法测定了尿中睾酮与表睾酮的比值。实验条件为:以氦为载气,SE—54熔融石英柔性毛细管柱、程序升温进行样品分离,多离子检测(MID),监测m/z432的离子。该法专属、灵敏、快速。睾酮与表睾酮比值在1:1～10:1(睾酮为20ng/μl)与相应峰面积比呈线性关系(r=0.998),最低检测限为1ng,最低检测尿药浓度为8ng/ml。

The trimethylsilylation of testosterone and epitestosterone was discussed in detail inthis reprot. Both derivative conditions under which testosterone and epi-testosrone were prepared intoTMS-derivatives in the presence of mercaptoethanol as an antioxidizing agent and method for the analy-sis of the ratio of testosterone to epi-testosterone in urine, based on GC--MS, had been established.The conditions of detection were: carrier gas was helium, derivatives were separated with SE-54 fusedsilica capillary column, using temperature program and detected by using mutiple ion detection mode inwhich the ion of m/z 432 was the monitoring ion. The method is rapid, sensitive and specific. For theratio of testosterone to epi-testosterone(testosterone:20 ng/μl), there is a linearity between ratio 1:1and 10:1(r=0.998), the limit of detection for testosterone and epi-testosterone is 1 ng, and the mi-nimum concentration of detection in urine is 8 ng/ml.