Rossi S A, Johnson J V, Yost R A
Department of Chemistry, University of Florida, Gainesville 32611.
Biol Mass Spectrom. 1994 Mar;23(3):131-9. doi: 10.1002/bms.1200230303.
Short-column (3.5 m) gas chromatography (GC)/tandem mass spectrometry (MS/MS) has been investigated for the detection of structurally related, underivatized anabolic steroids in urine. The approach described here demonstrates the ability to rapidly and qualitatively detect underivatized anabolic steroids in spiked urine matrices. In this approach, underivatized steroids are determined using a short-column GC separation, ionized by positive ion chemical ionization, and detected by selected reaction monitoring MS/MS. This approach permits positive identification of underivatized anabolic steroids based on retention time and the production of characteristic product ions. Preliminary detection limits studies in spiked urine samples showed quantitative results between 2 and 40 ng steroid per milliliter of uterine. The potential advantages of this approach compared to present screening methods based on conventional (30 m) GC/MS are its rapidity and selectivity. Reliable qualitative identification can be performed with a short-column GC/MS/MS analysis of less than 6 min with a reduction in sample preparation time due to the elimination of the derivatization step.
已对短柱(3.5米)气相色谱(GC)/串联质谱(MS/MS)进行了研究,用于检测尿液中结构相关的未衍生化合成代谢类固醇。此处描述的方法证明了在加标尿液基质中快速、定性检测未衍生化合成代谢类固醇的能力。在该方法中,未衍生化类固醇通过短柱GC分离进行测定,通过正离子化学电离进行离子化,并通过选择反应监测MS/MS进行检测。该方法允许基于保留时间和特征产物离子的产生对未衍生化合成代谢类固醇进行阳性鉴定。加标尿液样品的初步检测限研究表明,每毫升尿液中类固醇的定量结果在2至40纳克之间。与基于传统(30米)GC/MS的现有筛查方法相比,该方法的潜在优势在于其快速性和选择性。通过少于6分钟的短柱GC/MS/MS分析可进行可靠的定性鉴定,由于省去了衍生化步骤,样品制备时间得以缩短。