Kiousi P, Angelis Y S, Lyris E, Koupparis M, Calokerinos A C, Atta-Politou J, Georgakopoulos C G
Doping Control Laboratory of Athens, Olympic Athletic Center of Athens, 15123 Maroussi, Greece.
Bioanalysis. 2009 Oct;1(7):1209-24. doi: 10.4155/bio.09.113.
While a number of different derivatization procedures for screening GC-MS analysis of prohibited substances are followed by doping control laboratories, a unified derivatization procedure for the GC-MS analysis of 190 different doping agents was developed.
Following preliminary experiments, a two-step derivatization procedure was selected. The evaluation of various silylation parameters, such as reagent composition, reaction time, reaction temperature, catalysts and microwave oven reaction time, for this procedure was carried out.
The suitability of the developed procedure was demonstrated through application on urine samples at concentration levels of the minimum required performance limit for all tested substances. This new derivatization procedure, which significantly decreases time and cost, is suitable for a routine basis application.
虽然兴奋剂检测实验室在采用气相色谱-质谱联用仪(GC-MS)分析违禁物质时遵循多种不同的衍生化程序,但已开发出一种用于190种不同兴奋剂的GC-MS分析的统一衍生化程序。
经过初步实验,选择了两步衍生化程序。对该程序的各种硅烷化参数进行了评估,如试剂组成、反应时间、反应温度、催化剂和微波炉反应时间。
通过在所有测试物质的最低所需性能极限浓度水平的尿液样本上应用,证明了所开发程序的适用性。这种显著减少时间和成本的新衍生化程序适用于常规应用。