Haber E, Muñoz-Guerra J A, Soriano C, Carreras D, Rodriguez C, Rodriguez F A
Doping Control Laboratory, Higher Sports Council, Madrid, Spain.
J Chromatogr B Biomed Sci Appl. 2001 May 5;755(1-2):17-26. doi: 10.1016/s0378-4347(00)00539-9.
This paper presents an automated method for extracting anabolic agents from urine samples for their GC-MS analysis by selected-ion monitoring. The sample preparation was carried out in a Hewlett-Packard 7686 SPE PrepStation system. Each 0.6-ml aliquot was hydrolyzed, extracted, dried and trimethylsilyl (TMS) derivatized in a 2-ml vial without any hands-on labor. When sample preparation was finished 2 microl of the extract was injected into the gas chromatograph by split (1:10) mode. Due to the small amount of free space in the 2-ml vials for handling the sample, parameters like time of hydrolysis, type of shaking, number of extractions and some TMS derivatization parameters had to be adjusted to achieve the best recovery for all of the compounds in the screening. Manual and automated sample preparation schemes were compared in terms of linearity, precision, accuracy, limit of detection and recovery data. When large concentrations were analyzed using the automated method no carry-over effect was observed.
本文介绍了一种从尿液样本中提取合成代谢药物的自动化方法，用于通过选择离子监测进行气相色谱 - 质谱分析。样品制备在惠普7686固相萃取制备工作站系统中进行。每份0.6毫升的等分试样在一个2毫升的小瓶中进行水解、萃取、干燥和三甲基硅烷基（TMS）衍生化，无需任何人工操作。样品制备完成后，将2微升提取物以分流（1:10）模式注入气相色谱仪。由于2毫升小瓶中用于处理样品的自由空间量较小，必须调整水解时间、振荡类型、萃取次数和一些TMS衍生化参数，以实现筛选中所有化合物的最佳回收率。在线性、精密度、准确度、检测限和回收率数据方面对手动和自动样品制备方案进行了比较。使用自动化方法分析高浓度样品时，未观察到残留效应。
