Laboratory of Food Analysis, Ghent University, Harelbekestraat 72, 9000 Ghent, Belgium.
J Mass Spectrom. 2011 Mar;46(3):327-35. doi: 10.1002/jms.1899.
For many years anabolic-androgenic steroids (AAS) are by far the most frequently detected pharmacological substances in doping control. In order to improve their performances, professional sportsmen are often tempted to take dietary supplements. However, due to the frequent and widespread occurrence of contaminated supplements, the use of such products is not without risk for the athletes involved. In order to minimize the chances of an unattended positive doping test or serious health problems, fast and reliable screening methods for the detection of anabolic steroids in dietary supplements are needed. A general screening procedure requires the fast and unambiguous detection of a large range of steroids. Gas chromatography-mass spectrometry (GC-MS) has been used intensively in the detection of doping substances for the past 40 years. Over time, many laboratories have delivered spectra to be included in standard reference databases, one of which is maintained by the National Institute of Standards and Technology (NIST) (Gaithersburg, MD, USA). In recent years, however, liquid chromatography coupled to mass spectrometry (LC-MS) has gained popularity. Unfortunately, existing GC-MS libraries are not applicable to LC-MS analysis. In the present study, a new mass spectral library of 88 steroids was developed, along with a fast UPLC-MS method. For the construction of this mass spectral library, three different mass spectra were measured for each steroid, with a sample cone voltage of 30, 60 and 100 V, respectively. This method was then successfully tested on contaminated dietary supplements which had previously been tested by means of a targeted LC-MS/MS method. Overall, the library search was shown to identify the same compounds as the MRM method.
多年来，合成代谢-雄激素类固醇（AAS）是兴奋剂检测中最常被检测到的药物物质。为了提高成绩，职业运动员经常被诱惑服用膳食补充剂。然而，由于补充剂经常被污染，使用这些产品对相关运动员来说并非没有风险。为了最大限度地降低未经检测的阳性兴奋剂检测或严重健康问题的可能性，需要快速、可靠的筛查方法来检测膳食补充剂中的合成代谢类固醇。一般的筛选程序需要快速、明确地检测广泛的类固醇。气相色谱-质谱联用（GC-MS）在过去 40 年中被广泛用于兴奋剂物质的检测。随着时间的推移，许多实验室都提供了光谱图，以被纳入标准参考数据库，其中一个由美国国家标准与技术研究院（NIST）（马里兰州盖瑟斯堡）维护。然而，近年来，液相色谱-质谱联用（LC-MS）已变得流行。不幸的是，现有的 GC-MS 库不适用于 LC-MS 分析。在本研究中，开发了一个新的 88 种类固醇的质谱数据库，以及一种快速的 UPLC-MS 方法。为了构建这个质谱数据库，对每种类固醇分别测量了三个不同的质谱，样品锥电压分别为 30、60 和 100V。然后，该方法成功地应用于以前通过靶向 LC-MS/MS 方法检测到的受污染的膳食补充剂。总的来说，库搜索被证明可以识别与 MRM 方法相同的化合物。
