固相萃取-气质联用仪检测尿液中多种内源性类固醇

Solid phase extraction and determination of endogenous anabolic steroids in urine by gas chromatography-mass spectrometry

目的为监控运动员食品药品安全问题,利用气质联用仪(gas chromatography-mass spectrometry,GC-MS)建立正常运动员尿液中多种内源性类固醇的分析方法。方法尿液冷冻处理解冻后离心,取上清液经固相萃取,β-葡萄糖醛酸甙酶水解后再次萃取干燥衍生化后,采用选择离子监控SIM模式进行检测。结果方法的最低检出限为0.2~0.5 ng/m L,平均提取回收率为93.64%~116.74%,相对标准偏差(relative standard deviation,RSD)低于6.59%。结论该方法可以用于内源性类固醇兴奋剂的检测。

Objective To develop a method of gas chromatography-mass spectrometry (GC-MS) for the simultaneous identification and quantification of endogenous anabolic steroids in urine of athletes,for assurance of their food and drug safety. Methods The thawed iced urine sample was centrifuged, and the liquid supernatant was extracted using reverse phase C18 column. The methanol eluant was collected, hydrolized by β-glucuronidase, derivatized with a derivatization reagent and detected using GC-MS in SIM mode. Results The limits of detection for endogenous anabolic steroids were in the range of 0.2~0.5 ng/mL, the average recoveries were 93.64%~116.74% with relative standard deviation (RSD) less than 6.59%. Conclusion The method can be used for the determination of endogenous anabolic steroids in urine for doping control.