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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 monitor the safety of athletes in food and medicine, gas chromatography-mass spectrometry (GC-MS) was used to establish a method for the analysis of a variety of endogenous steroids in the urine of normal athletes. Methods Frozen urine was thawed and centrifuged. The supernatant was extracted by solid-phase extraction, hydrolyzed by β-glucuronidase and extracted again. After derivatization, the SIM pattern of selective ion monitoring was used for detection. Results The detection limit of the method was 0.2-0.5 ng / mL. The average recovery was 93.64% ~ 116.74%. The relative standard deviation (RSD) was less than 6.59%. Conclusion This method can be used for the detection of endogenous steroid agonists.