Gonzalo-Lumbreras R, Pimentel-Trapero D, Izqierdo-Hornillos R
Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense, Madrid, Spain.
J Chromatogr B Biomed Sci Appl. 2001 Apr 25;754(2):419-25. doi: 10.1016/s0378-4347(01)00027-5.
Liquid-liquid (using dichloromethane) and liquid-solid extraction processes (using disposable C18 cartridges) were applied to human urine samples spiked with 15 androgenic anabolic steroids (natural and synthetic). The extraction recoveries were assessed from different HPLC separations of anabolic steroids using water-acetonitrile mobile phase, and using calibration graphs obtained by injection into HPLC of standard samples of these compounds before and after extraction. The procedures, including sample preconcentration, showed extraction efficiencies over 90% which were independent on a wide range of concentrations tested. Solid phase extraction yielded poor results for oximetolone, danazol and dehydroepiandrosterone. For real urine samples, hydrolysis using beta-glucuronidase and washing using sodium hydroxide before and after solvent extraction, respectively, is recommended.
液-液萃取(使用二氯甲烷)和液-固萃取过程(使用一次性C18柱)应用于添加了15种雄激素类合成代谢类固醇(天然和合成)的人类尿液样本。通过使用水-乙腈流动相的不同高效液相色谱(HPLC)分离方法对合成代谢类固醇进行评估,并使用这些化合物在萃取前后注入HPLC的标准样品所获得的校准曲线来评估萃取回收率。包括样品预浓缩在内的这些程序显示,萃取效率超过90%,且与所测试的广泛浓度范围无关。固相萃取对氧甲氢龙、达那唑和脱氢表雄酮的萃取效果不佳。对于实际尿液样本,建议分别在溶剂萃取之前使用β-葡萄糖醛酸酶进行水解,在萃取之后使用氢氧化钠进行洗涤。