超高效液相色谱-串联质谱测定减肥保健食品中辛弗林及其电喷雾质谱裂解途径研究

ESI Fragmentation Studies and Determination of Synephrine in the Weight-loss Functional Foods by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了测定减肥保健食品中辛氟林的超高效液相色谱-串联质谱分析方法。不同类型减肥保健食品经超声提取,固相萃取净化后,以ACQUITY UPLC BEH HILIC色谱柱分离,采用多反应监测正离子模式检测,监测离子对为m/z168/150和m/z168/135,定量离子对为m/z168/150。结果表明,辛氟林在0.03～50μg/L的范围内与其峰面积呈良好的线性关系,相关系数为0.9990。在低、中、高3个添加水平范围内的平均回收率为80.3%～98.4%。同时研究了辛弗林的电喷雾电离串联质谱特征,推测其裂解途径。该方法准确、灵敏度高、操作简便,可用于不同减肥保健食品中辛弗林的检测。

A comprehensive analytical method based on ultra performance liquid chromatography-tandem mass spectrometry has been developed for the determination of synephrine.Various weight-loss functional foods were extracted under ultrasoniccation and were cleaned up by solid phase extraction. The solution was separated on ACQUITY UPLC BEH HILIC column（100×2.1mm,1.7μm）,and synephrine was detected by MS/MS technique using positive electrospray ionization and multiple reaction monitoring（MRM ）mode,employing two precursor-product ion pairs：m/z168/150and m/z168/135, as qualitative ion pairs,and m/z168/150as quantification ion pairs.The calibration curve showed good linearity for synephrine in the range of 0.03～50μg/L,and the correlative coefficient was 0.9990.The mean recoveries at three spiked levels（low,middle,high）were 80.3%～98.4%.The work also studied the mass spectrum characterization of synephrine and speculated on fragmentation pathways.The method is accurate,sensitive,simple,and suitable for the determination of synephrine in the different weight-loss functional foods.