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尿液样本中睾酮和表睾酮共轭物的短期稳定性:通过液相色谱-线性离子阱质谱法定量分析

Short-term stability of testosterone and epitestosterone conjugates in urine samples: quantification by liquid chromatography-linear ion trap mass spectrometry.

作者信息

Saudan Christophe, Entenza José M, Baume Norbert, Mangin Patrice, Saugy Martial

机构信息

Laboratoire Suisse d'Analyse du Dopage, Institut Universitaire de Médecine Légale, Chemin des Croisettes 22, 1066 Epalinges, Switzerland.

出版信息

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.

Abstract

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.

摘要

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。

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