DART-MS/MS法直接实时检测保健食品中非法添加的6个PDE5抑制剂的应用研究

Study on rapid and direct analysis of illegally added six PDE5 inhibitors in health food by DART-MS/MS method

目的:建立一种可以快速检测保健食品中非法添加6个磷酸二酯酶5(PDE5)抑制剂西地那非、他达拉非、红地那非、羟基豪莫西地那非、氨基他达拉非、伪伐地那非的方法。方法:采用直接实时分析(DART)离子源结合三重四极杆质谱,DART离子源的样品传输速度为0.2 mm·s-1,载气温度为450℃。Agilent 6410B Triple Quad LC/MS毛细管电压4 kV,干燥气流速为10 L·min-1。扫描模式为子离子全扫描,扫描范围为50～550 amu。待测成分的前体离子为m/z 475.1(西地那非),m/z467.2(红地那非),m/z 505.1(羟基豪莫西地那非),m/z 390.1(他达拉非),m/z 391.2(氨基他达拉非),m/z 460.3(伪伐地那非)。通过对照品与样品的二级质谱图对比进行样品中非法添加成分的定性鉴别。结果:若干批市售保健食品中有4批检出西地那非,1批检出他达拉非。检出限达1μg·g-1,检测时间仅为几分钟。结论:DART-MS可用于固体样品中添加PDE5抑制剂类成分的快速检测,用于药品快速检验中批量样品的初筛更有优势。

Objective：To develop a directed analysis of 6 phosphodiesterase 5（PDE5）inhibitors：sildenafil,tadalafil,acetildenafil,hydroxyhomosildenafil,aminotadalafil,pseudo-vardenfil in health food.Methods：Triple quadrupol MS with DART ion souce was used to perform the direct analysis.The DART sampler delivery rate was 0.2 mm·s-1.The temperature of carry gas of DART was 450 ℃.The capillary voltage was kept at 4 kV.The temperature of the drying gas of triple quadrupol MS was set at 350 ℃.The flow rate of the drying gas of triple quadrupol MS was set at 10 L·min-1,respectively.Product ion scan mode was used with scan range from 50-550 amu.The precursor ions were set as m/z 475.1（sildenafil）,m/z 467.2（acetildenafil）,m/z 505.1（hydroxyhomosildenafil）,m/z 390.1（tadalafil）,m/z 391.2（aminotadalafil）,m/z 460.3（pseudo-vardenfil）.The identification was performed by comparing the mass spectrum of detected peak in samples with the mass spectrum of peak in reference substance.Results：The limit of detection for each of 6 PDE5 inhibitors was under 1 μg·g-1.Sildenafil was detected in 6 samples,and tadalafil was detected in 1 sample.Conclusion：The method is employed to simultaneous detection of 6 PDE5 inhibitors in health food.