固相萃取-超高效液相色谱-电喷雾串联质谱法同时检测尿样中的麻黄碱和N-甲基麻黄碱

建立了固相萃取-超高效液相色谱-电喷雾串联质谱(SPE-UPLC-ESI MS/MS)联用方法,定量测定尿样中的麻黄碱和N-甲基麻黄碱。样品经Oasis MCX柱提取、纯化和富集后,采用电喷雾(ESI)离子源电离,正离子多反应监测(MRM)模式质谱进行定性和定量分析。麻黄碱和N-甲基麻黄碱在0.0250~2.50 μg/L质量浓度范围内线性关系良好,线性相关系数分别为0.9998和0.9992,提取回收率高于80%,提取效率的RSD小于5.0%,检出限均达到0.01 μg/L,可大大延长尿样检材中麻黄碱和N-甲基麻黄碱的检测周期。结果表明,该方法快速、准确,为尿液中痕量麻黄碱和N-甲基麻黄碱的分析提供了灵敏的分析方法。

Simultaneous determination of ephedrine and N-methylephedrine in urine by solid phase extraction-ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry

A rapid and sensitive method has been developed for the simultaneous determination of ephedrine and N-methylephedrine in urine samples by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (SPE-UPLC-ESI MS/MS). The samples were extracted with Oasis MCX solid phase extraction cartridges and measured in the modes of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM). Good linearities were observed in the range of 0.0250-2.50 μg/L with correlation coefficient over 0.9990 for both analytes. The recoveries were above 80% with RSDs less than 5.0%. The limits of detection were 0.01 μg/L. The method proves to be rapid and sensitive for the trace determination of ephedrine and N-methylephedrine in urine samples.