摘要
目的:建立基于液相色谱-高分辨质谱联用技术快速检测药片、胶囊和注射液中的32种蛋白同化制剂的方法,为反兴奋剂以及司法鉴定领域蛋白同化制剂的检测提供技术支持。方法:药片研磨成粉末,胶囊内粉末采用甲醇∶水(7∶3)溶液提取,注射液直接经离心过滤后进样。采用Waters Acquity UPLC HSS T3 column(100 mm×2.1 mm,1.8μm)柱分离,以含0.1%甲酸和5%乙腈的乙酸铵(20 mmol/L)溶液-乙腈体系作为流动相进行梯度洗脱,加热电喷雾离子源正离子模式,一级全扫描/数据依赖二级扫描模式检测。对建立的分析方法进行方法学验证,对选择性、灵敏度、基质效应、延迟效应等参数进行考察,并应用于20份办案机关查获的药片、胶囊和注射液样品中蛋白同化制剂的检测。结果:粉末基质中32种蛋白同化制剂检出限在1~200μg/g范围内,注射液基质中检出限在1~200 ng/mL范围内。20份查获样品中检测到美雄酮、司坦唑醇等5种蛋白同化制剂,均与外包装标签标识不符。结论:液相色谱-高分辨质谱联用技术前处理简便,灵敏度高,适用于反兴奋剂和司法鉴定领域药片、胶囊和注射液样品中蛋白同化制剂的检测。
Objective To determine 32 anabolic agents in tablets,capsules and injections using liquid chromatography-high resolution mass spectrometry(LC-HRMS),so as to provide technical support in the fields of anti-doping and judicial identification.Methods The tablet grinded into powder,capsule samples extracted using a methanol:water(7:3)solution and injection underwent centrifugation and filtration.The separation was performed on a Waters Acquity UPLC HSS T3 column(100 mm×2.1 mm,1.8μm),followed by gradient elution using ammonium acetate(20 mmol/L)solution containing 0.1%formic acid,5%acetonitrile and acetonitrile system as mobile phases,and detection by heated electrospray ionization in positive mode with a primary full-scan/data-dependent secondary scan mode.The established analytical method was subjected to methodological validation and parameters such as selectivity,sensitivity,matrix effect and delay effect were investigated.Meanwhile,the method was applied to the detection of anabolic agents in 20 samples of tablets,capsules and injections provided by the authorities.Results The detection limits for 32 anabolic agents ranged from 1~200μg/mg in the powder and 1~200 ng/mL in the injection.When this method was applied to the analysis of actual samples,five anabolic agents,including methandrostenolone and stanozolol,were identified among the 20 samples,disconsistent with labels on the package.Conclusion The LC-HRMS method is simple in pretreatment,sensitive and suitable for the detection of anabolic agents in tablet,capsule and injection samples in the fields of anti-doping and judicial identification.
作者
刘玙
范先煜
郭振硕
钱小雨
向平
严慧
Liu Yu;Fan Xianyu;Guo Zhenshuo;Qian Xiaoyu;Xiang Ping;Yan Hui(Academy of Forensic Science,Shanghai Key Laboratory of Forensic Medicine,Shanghai Forensic Service Platform,Key Laboratory of Forensic Science,Ministry of Justice,Shanghai 200063,China;Kunming Medical University,Kunming 650500,China)
出处
《中国运动医学杂志》
北大核心
2025年第6期451-465,共15页
Chinese Journal of Sports Medicine
基金
中央公益课题资助项目(GY2022G-2)
上海市法医学重点实验室资助项目(21DZ2270800)
司法部司法鉴定重点实验室资助项目
上海市司法鉴定专业技术服务平台资助项目。
关键词
蛋白同化制剂
司坦唑醇
药片
液相色谱-高分辨质谱
anabolic androgenic steroids
Stanozolol
in vitro samples
liquid chromatography-high resolution mass spectrometry
