Wang Yunfei, Yan Kuan, Wang Zhanliang, He Genye, Chang Wei
National Anti-Doping Laboratory, Beijing Sport University, Beijing 100029, China.
J Chromatogr Sci. 2022 Dec 29;61(1):32-37. doi: 10.1093/chromsci/bmac022.
An accurate quantitative method for four prohibited ephedrine substances in human urine has been established, based on ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The quantitative bias caused by pretreatment operations and matrix effects was reduced by the dilute and shoot pretreatment method. The good separation of isomers was achieved with the advantages of the UPLC instrument and Agilent Poroshell 120 EC-C8 UPLC column. Stable quantitative ions were selected during the analysis with MS/MS. The result of the method validation experiment showed an excellent linearity between 50% and 200% threshold concentration with a correlation coefficient (r2) greater than 0.999. The coefficient of variation at the limit of quantification and threshold was <20% and 10%, respectively. The uncertainty was below the maximum uncertainty specified in the technical document of the World Anti-Doping Agency (WADA). The analytical result using this method has passed the WADA-external quality assessment scheme. The anti-doping laboratory has applied the method in routine tests and reported adverse analytical finding.
基于超高效液相色谱串联质谱法（UPLC-MS/MS），建立了一种准确测定人尿中四种违禁麻黄碱类物质的定量方法。采用直接进样前处理方法，减少了前处理操作和基质效应引起的定量偏差。利用UPLC仪器和安捷伦Poroshell 120 EC-C8 UPLC色谱柱的优势，实现了异构体的良好分离。在MS/MS分析过程中选择了稳定的定量离子。方法验证实验结果表明，在50%至200%阈值浓度之间具有良好的线性，相关系数（r2）大于0.999。定量限和阈值处的变异系数分别<20%和10%。不确定度低于世界反兴奋剂机构（WADA）技术文件规定的最大不确定度。使用该方法的分析结果通过了WADA外部质量评估计划。反兴奋剂实验室已将该方法应用于常规检测，并报告了阳性分析结果。
