Barrón D, Barbosa J, Pascual J A, Segura J
Department of Analytical Chemistry, University of Barcelona, Spain.
J Mass Spectrom. 1996 Mar;31(3):309-19. doi: 10.1002/(SICI)1096-9888(199603)31:3<309::AID-JMS298>3.0.CO;2-6.
A fully automated method is presented for the determination of anabolic steroids in human urine. On line solid-phase extraction with automatic cartridge exchange is used for sample clean-up followed by an high-performance liquid chromatographic isocratic separation. A narrow-bore 5 microns reversed-phase column (250 x 2.1 mm i.d.) at a flow rate of 0.2 ml min-1 is connected to a particle beam interface linked to a single-quadrupole mass spectrometer. No derivatization is needed and normal electron impact mass spectra are obtained for a series of up to 28 steroids and metabolites. Urine samples collected following the ingestion of therapeutic doses of some of the steroids were analysed and the detection and confirmation of excreted compounds accomplished. A dramatic reduction in human intervention and overall analysis time was achieved compared with other common approaches.
本文介绍了一种用于测定人尿中合成代谢类固醇的全自动方法。采用自动柱切换的在线固相萃取进行样品净化，随后进行高效液相色谱等度分离。一根内径为2.1 mm、长250 mm、粒径5微米的窄孔反相柱，以0.2 ml min-1的流速连接到与单四极杆质谱仪相连的粒子束接口。无需衍生化，即可获得一系列多达28种类固醇和代谢物的正常电子轰击质谱。对摄入某些治疗剂量类固醇后收集的尿液样本进行了分析，并完成了排泄化合物的检测和确认。与其他常用方法相比，大大减少了人工干预并缩短了整体分析时间。
