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采用气相色谱-串联质谱法分析毛发中的合成代谢类固醇。

Analysis of anabolic steroids in hair by GC/MS/MS.

作者信息

Gambelunghe C, Sommavilla M, Ferranti C, Rossi R, Aroni K, Manes N, Bacci M

机构信息

Department of Clinical and Experimental Medicine, Division of Legal and Sports Medicine, University of Perugia, Italy.

出版信息

Biomed Chromatogr. 2007 Apr;21(4):369-75. doi: 10.1002/bmc.763.

Abstract

A simple and sensitive gas chromatography/tandem mass spectrometry (GC/MS/MS) method is described for the detection of anabolic steroids, usually found in keratin matrix at very low concentrations. Hair samples from seven athletes who spontaneously reported their abuse of anabolic steroids, and in a single case cocaine, were analyzed for methyltestosterone, nandrolone, boldenone, fluoxymesterolone, cocaine and its metabolite benzoylecgonine. Anabolic steroids were determinate by digestion of hair samples in 1 m NaOH for 15 min at 95 degrees C. After cooling, samples were purificated by solid-phase and liquid-liquid extraction, then anabolic steroids were converted to their trimethylsilyl derivative and finally analyzed by GC/MS/MS. For detection of cocaine and benzoylecgonine, hair samples were extracted with methanol in an ultrasonic bath for 2 h at 56 degrees C then overnight in a thermostatic bath at the same temperature. After the incubation, methanol was evaporated to dryness, and benzoylecgonine was converted to its trimethylsilyl derivative prior of GC/MS/MS analysis. Results obtained are in agreement with the athletes' reports, confirming that hair is a valid biological matrix to establish long-term intake of drugs.

摘要

本文描述了一种简单且灵敏的气相色谱/串联质谱(GC/MS/MS)方法,用于检测通常在角蛋白基质中以极低浓度存在的合成代谢类固醇。对七名自发报告滥用合成代谢类固醇的运动员以及一例滥用可卡因的运动员的毛发样本进行分析,检测其中的甲基睾酮、诺龙、勃地酮、氟羟甲睾酮、可卡因及其代谢物苯甲酰爱康宁。合成代谢类固醇的检测方法为:将毛发样本在1 m氢氧化钠中于95℃消化15分钟。冷却后,通过固相萃取和液液萃取对样本进行净化,然后将合成代谢类固醇转化为其三甲硅烷基衍生物,最后通过GC/MS/MS进行分析。对于可卡因和苯甲酰爱康宁的检测,毛发样本在56℃的超声浴中用甲醇萃取2小时,然后在相同温度的恒温浴中萃取过夜。孵育后,将甲醇蒸发至干,并在进行GC/MS/MS分析之前将苯甲酰爱康宁转化为其三甲硅烷基衍生物。所得结果与运动员的报告一致,证实毛发是确定长期药物摄入情况的有效生物基质。

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