GC-MS determination of steroids related to androgen biosynthesis in human hair with pentafluorophenyldimethylsilyl-trimethylsilyl derivatisation
GC-MS determination of steroids related to androgen biosynthesis in human hair with pentafluorophenyldimethylsilyl-trimethylsilyl derivatisation
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DOI：
10.1039/a903912k
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发表时间：
1999-09-01
期刊：
影响因子：
4.2
通讯作者：
Chung, BC
中科院分区：
文献类型：
--
作者：
Choi, MH;Chung, BC
建立了以d(3)-睾酮为内标的气相色谱-质谱法同时测定人发中雄烯二酮、二氢睾酮、脱氢表雄酮、睾酮、雄酮、黄胆酮、孕酮和孕烯醇酮的方法。该方法包括碱解、液-液萃取，然后转化为混合的五氟苯基二甲基硅基-三甲基硅基(氟苯甲基-TMS)衍生物，在选择离子监测(SIM)模式下进行灵敏分析。该方法具有良好的总重复性和重现性，分别为4.88~11.24和3.19~9.58%。首次实现了人发中DHT、DHEA和孕烯醇酮的GC-MS定量，并对睾酮进行了定量。在0.12-8.45ngg(-1)的浓度范围内可以检测到头发样品中的四种类固醇。未检出雄烯二酮、雄酮、黄胆醇酮和孕酮等4种类固醇。该方法的检出限为0.02ngg(-1)~0.5ngg(-1)，线性关系良好，相关系数为0.991~0.996。检测到的四种类固醇在男性和女性头发样本中的浓度不同。
An efficient method for the simultaneous determination of eight steroids, androstenedione, dihydrotestosterone (DHT), dehydroepiandrosterone (DHEA), testosterone, androsterone, etiocholanolone, progesterone and pregnenolone, in human hair by gas chromatography-mass spectrometry (GC-MS) using d(3)-testosterone as internal standard is described. The method involves alkaline digestion, liquid-liquid extraction and subsequent conversion to mixed pentafluorophenyldimethylsilyl-trimethylsilyl (flophemesyl-TMS) derivatives for sensitive analysis in the selected ion monitoring (SIM) mode. This method showed good overall repeatability and reproducibility of 4.88-11.24 and 3.19-9.58%, respectively. For the first time, the quantification of DHT, DHEA and pregnenolone in human hair has been achieved by GC-MS, testosterone was also quantified. The detection of four steroids in hair samples was possible in the concentration range 0.12-8.45 ng g(-1). The other four steroids, androstenedione, androsterone, etiocholanolone and progesterone, were not detected. The detection limits for SIM of the steroids varied in the range 0.02-0.5 ng g(-1), and the SIM responses were linear with correlation coefficients varying from 0.991 to 0.996 for most of the steroids studied. The concentrations of the four steroids detected were different in male and female hair samples.