阿卡地新(AICAR)的LC-MS/MS检测方法的建立及应用

Detection of AICAR in Urine by Liquid Chromatography Tandem Mass Spectrometry

目的：建立阿卡地新（AICAR）的LC-MS/MS检测方法,在日常检测中使用。方法：取2 ml尿样,加入50μlβ-葡萄糖醛酸苷酶进行酶解,C18-SPE固相萃取,洗脱液氮气下吹干,后溶解上样。用此方法检测290名运动员内源性AICAR浓度,建立中国运动员AICAR内源性水平数据库。结果：方法验证中得出线性相关系数、最低检测限和定量限,满足日常定性定量要求;药物日间精密度〈20%,日内精密度〈15%,回收率在85%以上;基质效应在80%～110%之间,符合一般验证要求;得到290名运动员内源性AICAR浓度平均值为1.5μg/ml,标准偏差为1.1μg/ml。结论：本方法灵敏度高、选择性强、重现性好,可以在日常检测中使用。

Objective The purpose of this study was to explore the method for detection of AICAR. Method Blank urine samples were collected from 290 Chinese athletes and positive urine sample was from a volunteer.50 μl beta-glucuranidase was added to 2 ml of urine sample. Then the urine was extracted by liquid-solid C18 SPE and evaporated to dryness by liquid nitrogen,and finally the dry residue was dissolved and injected into the LC-MS/MS system to detect the AICAR. Results Correlation coefficient,LOD and LOQ of this method are appropriate for routine quantitative and qualitative requirement in doping control. The intra-day and interday RSD,recovery rate,and matrix effect are respectively less than 20%,above 85% and between 80%～110%.The average concentration of endogenous AICAR in urine sample from 290 Chinese athletes is 1.5 ± 1.1 μg/ml. Conclusion The reproducibility,sensitivity,and selectivity of this method are high enough to meet the requirements of daily doping control.