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1. 发明申请

WO2010018375A1 PREPARATION OF BIOLOGICAL SAMPLES FOR COMPOUND-SPECIFIC CARBON ISOTOPE ANALYSIS 审中-公开
标题翻译：用于化合物碳同位素分析的生物样品的制备
公开(公告)号：WO2010018375A1
公开(公告)日：2010-02-18
申请号：PCT/GB2009/001980
申请日：2009-08-12
申请人： IMPERIAL INNOVATIONS LIMITED , THE UNIVERSITY OF NOTTINGHAM , SEPHTON, Mark, A. , SNAPE, Colin, E. , GOMES, Rachel, L. , MEREDITH, Wil
发明人： SEPHTON, Mark, A. , SNAPE, Colin, E. , GOMES, Rachel, L. , MEREDITH, Wil
IPC分类号： G01N33/74 , G01N33/92 , B01D59/44 , C07C1/00 , G01N1/00
CPC分类号： G01N33/743 , G01N33/92
摘要： The present invention provides a method of measuring the relative ratios of 13 C to 12 C in an organic compound, e.g. a steroid or a conjugated steroid such as the sulphate conjugate of testosterone, using compound-specific carbon isotope analysis. The method comprises: subjecting a sample of the compound to hydropyrolysis in the presence of a transition metal catalyst, preferably platinum but also including palladium, rhodium and iridium, under a hydrogen atmosphere at a temperature below 350 °C, subjecting the hydrocarbon product released via hydropyrolysis to gas chromatography to provide a purified sample of the hydropyrolysed product, combusting the hydropyrolysed product to form carbon dioxide and submitting the resulting carbon dioxide to mass spectrometry to obtain the relative ratios of 13 C to 12 C in the carbon dioxide. The method deconjugates the compound from both sulfate or glucuronide moieties when the compound is derived from urine samples and avoids the need to derivatise the compound prior to the gas chromatography step.
摘要翻译：本发明提供了一种测量有机化合物中13C至12C的相对比例的方法，例如，类固醇或共轭类固醇，如睾丸激素的硫酸盐缀合物，使用化合物特异性碳同位素分析。该方法包括：在氢气氛下，在低于350℃的温度下，在过渡金属催化剂，优选铂，但也包括钯，铑和铱的存在下，使化合物的样品进行加氢热解，使经由加氢热解至气相色谱以提供纯化的水解产物样品，使加氢热解产物燃烧形成二氧化碳，并将所得二氧化碳进行质谱分析，以获得二氧化碳中13C至12C的相对比例。当化合物衍生自尿液样品时，该方法从硫酸盐或葡萄糖醛酸苷部分中分离出化合物，并避免在气相色谱步骤之前衍生化合物。

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