Saudan Christophe, Entenza José M, Baume Norbert, Mangin Patrice, Saugy Martial
Laboratoire Suisse d'Analyse du Dopage, Institut Universitaire de Médecine Légale, Chemin des Croisettes 22, 1066 Epalinges, Switzerland.
J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Nov 21;844(1):168-74. doi: 10.1016/j.jchromb.2006.07.010. Epub 2006 Aug 7.
A simple method using liquid chromatography-linear ion trap mass spectrometry for simultaneous determination of testosterone glucuronide (TG), testosterone sulfate (TS), epitestosterone glucuronide (EG) and epitestosterone sulfate (ES) in urine samples was developed. For validation purposes, a urine containing no detectable amount of TG, TS and EG was selected and fortified with steroid conjugate standards. Quantification was performed using deuterated testosterone conjugates to correct for ion suppression/enhancement during ESI. Assay validation was performed in terms of lower limit of detection (1-3ng/mL), recovery (89-101%), intraday precision (2.0-6.8%), interday precision (3.4-9.6%) and accuracy (101-103%). Application of the method to short-term stability testing of urine samples at temperature ranging from 4 to 37 degrees C during a time-storage of a week lead to the conclusion that addition of sodium azide (10mg/mL) is required for preservation of the analytes.
建立了一种使用液相色谱 - 线性离子阱质谱法同时测定尿液样本中睾酮葡萄糖醛酸苷(TG)、硫酸睾酮(TS)、表睾酮葡萄糖醛酸苷(EG)和表睾酮硫酸盐(ES)的简单方法。为进行验证,选择了一份未检测到TG、TS和EG的尿液,并添加甾体共轭物标准品。使用氘代睾酮共轭物进行定量,以校正电喷雾电离(ESI)过程中的离子抑制/增强。检测验证在检测下限(1 - 3ng/mL)、回收率(89 - 101%)、日内精密度(2.0 - 6.8%)、日间精密度(3.4 - 9.6%)和准确度(101 - 103%)方面进行。将该方法应用于尿液样本在4至37摄氏度温度下为期一周的短期稳定性测试,得出结论:需要添加叠氮化钠(10mg/mL)来保存分析物。