气相色谱-药学学报.DOC

· PAGE 1668· 药学学报 Acta Pharmaceutica Sinica 2012, 47 (12): 1667?1670 邢延一等: 气相色谱-高分辨质谱联用法检测人尿中21种兴奋剂 · PAGE 1669· 药学学报 Acta Pharmaceutica Sinica 2012, 47 (12): 1667?1670 · PAGE 1667· 气相色谱-高分辨质谱联用法检测人尿中21种兴奋剂 邢延一*, 刘 欣, 张玉梅, 王小兵, 徐友宣 (国家体育总局反兴奋剂中心, 北京 100029) 摘要: 采用气相色谱-高分辨质谱联用技术建立人尿中包括诺龙、宝丹酮、美雄酮在内的21种兴奋剂的检测方法。样品经液液萃取, 浓缩, 三甲基硅烷化衍生, 利用气相色谱/高分辨质谱及多离子检测技术 (MID) 同时检测21种兴奋剂。按照世界反兴奋剂组织 (WADA) 认可实验室方法验证程序进行验证, 该方法的检出限为ng·mL?1水平; 回收率为66%～103%之间 (n = 6), 回收率的相对标准偏差小于10.0%; 对3个不同浓度下样品定量检测的精密度测试。结果表明, 精密度RSD分别低于9.5%, 10.0%, 9.7%。 关键词: 兴奋剂检测; 气相色谱; 高分辨质谱 中图分类号: R917 文献标识码: A 文章编号: 0513-4870 (2012) 12-1667-04 Determination of doping in human urine by gas chromatography-high resolution mass spectrometry XING Yan-yi*, LIU Xin, ZHANG Yu-mei, WANG Xiao-bing, XU You-xuan (China Anti-Doping Agency, Beijing 100029, China) Abstract: A method was evaluated for determination of twenty-one doping (including nandrolone, boldenone and methandienone) in human urine by gas chromatography-high resolution mass spectrometry. Samples were prepared by liquid-liquid extraction, concentrated, TMS derivatization and limit of detection at ng·mL?1 by MID/GC/HRMS. According to the code of the World Anti-Doping Agency (WADA), precision and recoveries of the procedure were evaluated by replicate analysis (n = 6), the recoveries in the range of 66%?103%, with the RSD below 10.0%. The precision within the day of the method with three different concentrations was also determined, RSD were less than 9.5%, 10.0% and 9.7%. Key words: doping analysis; GC; HRMS 收稿日期: 2012-07-24; 修回日期: 2012-09-27.*通讯作者 E-mail: xingyanyi@兴奋剂, 作为竞技体育的毒瘤, 不但影响体育竞赛的公平性, 也严重危害运动员的身体健康[1 收稿日期: 2012-07-24 *通讯作者 E-mail: xingyanyi@ 经典的兴奋剂检测方法主要包括气相色谱-质谱联用 (GC-MS) 和液相色谱-质谱联用 (LC-MS)。由于检测要求的不断提高, 各种兴奋剂的检出限也在不断降低, 气相色谱-高分辨质谱、液相色谱?串联质谱等技术开始应用于兴奋剂等禁用物质的检测[6, 7]。最初气相色谱-高分辨质谱主要应用于检测5种低浓度的甾体类兴奋剂[8]。由于气相色谱-高分辨质谱具