Doping Control Center, Korea Institute of Science and Technology, Hwarang-ro 14-gil 5, Seongbuk-gu, Seoul, 136-791, Korea; Department of Chemistry, Research Institute for Natural Sciences, Korea University, 145, Anam-ro, Seongbuk-gu, Seoul, 136-701, Korea.
Drug Test Anal. 2014 Nov-Dec;6(11-12):1174-85. doi: 10.1002/dta.1747. Epub 2014 Nov 9.
Metal ion coordination ionspray (M(+) CIS) ionization is a powerful technique to enhance ionization efficiency and sensitivity. In this study, we developed and validated an analytical method for simultaneous ionization and analysis of 84 anabolic androgenic steroids (65 exogenous and 19 endogenous) using liquid chromatography-silver ion coordination ionspray/triple-quadrupole mass spectrometry (LC-Ag(+) CIS/MS/MS). The concentrations of silver ions and organic solvents have been optimized to increase the amount of silver ion coordinated complexes. A combination of 25 μM of silver ions and methanol showed the best sensitivity. The validation results showed the intra- (0.8-9.2%) and inter-day (2.5-14.9%) precisions, limits of detection (0.0005-5.0 ng/mL), and matrix effect (71.8-100.3%) for the screening analysis. No significant ion suppression was observed. In addition, this method was successfully applied to analysis of positive samples from suspected abusers and useful for the detection of the trace levels of anabolic steroids in human urine samples.
金属离子配合离子喷雾（M(+) CIS）电离是一种增强电离效率和灵敏度的强大技术。在这项研究中，我们开发并验证了一种使用液相色谱-银离子配合离子喷雾/三重四极杆质谱（LC-Ag(+) CIS/MS/MS）同时对 84 种合成代谢雄激素类固醇（65 种外源性和 19 种内源性）进行同时电离和分析的分析方法。优化了银离子和有机溶剂的浓度以增加银离子配位复合物的数量。25 μM 的银离子和甲醇的组合表现出最佳的灵敏度。验证结果表明，筛选分析的日内（0.8-9.2%）和日间（2.5-14.9%）精密度、检测限（0.0005-5.0ng/mL）和基质效应（71.8-100.3%）。未观察到明显的离子抑制。此外，该方法成功应用于疑似滥用者阳性样本的分析，可用于检测人尿液样本中痕量水平的合成代谢类固醇。
