液相色谱-串联质谱法确证人尿中的利他林及其主要代谢物

建立了固相萃取-液相色谱-串联质谱法同时确证人尿中的利他林及其主要代谢物利他林酸的方法。尿样中的药物经反相C₁₈固相萃取柱净化、氮气吹至干，以甲睾为内标，用流动相溶解后进行液相色谱-串联质谱法测定。该方法的最低检出限为5 μg•L^-1；利他林和利他林酸的回收率分别为80.6%和68.4%；批内和批间的相对标准偏差小于6.0%,能满足国际反兴奋剂机构(WADA)对其最低检测能力500 μg•L^-1的要求。

Confirmation of Methylphenidate and Its Major Metabolite in Human Urine by Liquid Chromatography-Tandem Mass Spectrometry

A solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) for simultaneous determination of methylphenidate and its major metabolite, ritalinic acid in human urine was developed and validated. The analytes were extracted by passing through C₁₈-revised phase extraction cartridge. The elution was evaporated by nitrogen blow， and dissolved by mobile phase, and then assayed by liquid chromatography-electrospray ionization tandem mass spectrometry. The limit of detection (LOD) is 5 μg•L^-1 for two analytes. Recoveries of methylphenidate and ritalinic acid are 80.6% and 68.4%, and inter-relative standard deviation (n=6) are less than 6.0%. The method can answer the requirements of the minimum required performance limit (MRPL) that doping control laboratories need to accomplish for stimulants at the concentration of 500 μg•L^-1 as established by WADA.