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液相色谱-串联质谱法进行兴奋剂检测分析的实例:麻黄碱、β受体阻滞剂、利尿剂、拟交感神经药和交联血红蛋白。

Examples of doping control analysis by liquid chromatography-tandem mass spectrometry: ephedrines, beta-receptor blocking agents, diuretics, sympathomimetics, and cross-linked hemoglobins.

作者信息

Thevis Mario, Schänzer Wilhelm

机构信息

Institute of Biochemistry, German Sport University, Cologne, Carl-Diem Weg 6, 50933 Cologne, Germany.

出版信息

J Chromatogr Sci. 2005 Jan;43(1):22-31. doi: 10.1093/chromsci/43.1.22.

Abstract

The application of modern and powerful analytical instruments consisting of liquid chromatographs (LCs), sophisticated atmospheric pressure ion sources, and sensitive mass analyzers has improved quality as well as speed of doping control analyses markedly during the last 5 years. Numerous compounds such as beta-receptor blocking agents or diuretics require derivatization prior to gas chromatographic (GC) and mass spectrometric (MS) measurement, which is the reason for extended sample preparation periods. In addition, several substances demonstrate poor GC-MS properties even after chemical modification, and peptide hormones such as cross-linked hemoglobins cannot be analyzed at all by means of GC-MS. With the availability of electrospray ionization and robust tandem MSs (e.g., triple-stage quadrupole or ion trap instruments) many new or complementary screening and confirmation assays have been developed, providing detailed qualitative and quantitative information on prohibited drugs. With selected categories of compounds (ephedrines, beta-blockers, b2-agonists, diuretics, and bovine hemoglobin-based oxygen therapeutics) that are banned according to the rules of the World Anti-Doping Agency and International Olympic Committee, the advantages of LC-MS-MS procedures over conventional GC-MS assays are demonstrated, such as enhanced separation of analytes, shorter sample pretreatment, and identification of substances that are not identified by GC-MS.

摘要

在过去5年中,由液相色谱仪(LC)、精密大气压离子源和灵敏质量分析仪组成的现代高性能分析仪器的应用显著提高了兴奋剂检测分析的质量和速度。许多化合物,如β受体阻滞剂或利尿剂,在进行气相色谱(GC)和质谱(MS)测量之前需要进行衍生化处理,这就是样品制备时间延长的原因。此外,一些物质即使经过化学修饰后,其GC-MS性能仍然较差,而肽类激素如交联血红蛋白根本无法通过GC-MS进行分析。随着电喷雾电离和强大的串联质谱仪(如三级四极杆或离子阱仪器)的出现,已经开发出许多新的或补充性的筛查和确证分析方法,能够提供有关违禁药物的详细定性和定量信息。通过世界反兴奋剂机构和国际奥委会规则所禁止的特定类别化合物(麻黄碱、β受体阻滞剂、β2激动剂、利尿剂和基于牛血红蛋白的氧治疗剂),证明了液相色谱-串联质谱(LC-MS-MS)方法相对于传统GC-MS分析方法的优势,如分析物分离效果增强、样品预处理时间缩短以及鉴定出GC-MS无法鉴定的物质。

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