离子迁移谱法快速检测保健食品中添加的5型磷酸二酯酶抑制剂

目的:建立快速检测保健食品中非法添加的西地那非、那红地那非、他达拉非、氨基他达拉非、伪伐地那非、那莫西地那非、二乙胺他达拉非7种5型磷酸二酯酶抑制剂的离子迁移谱方法。方法:采用离子迁移谱正离子模式检测西地那非、那红地那非、他达拉非、氨基他达拉非、伪伐地那非、那莫西地那非、二乙胺他达拉非7种5型磷酸二酯酶抑制剂,离子源电压为2.5 kV,迁移管电压为7.5 kV,进气口温度和迁移管温度均为180℃。利用所建立方法对20批市售缓解体力疲劳类保健食品进行非法添加筛查,并通过LC-MS进行确认。结果:7种5型磷酸二酯酶抑制剂迁移时间在13.8~16.2 ms之间,检出限为0.05~2 μg·mL^-1。20批市售样品中13批检出西地那非,2批检出他达拉非,2批同时检出西地那非与他达拉非,与LC-MS检测结果一致。结论:离子迁移谱检测方法快速、灵敏,可以作为缓解体力疲劳类保健食品中非法添加的西地那非、那红地那非、他达拉非、氨基他达拉非、伪伐地那非、那莫西地那非、二乙胺他达拉非7种5型磷酸二酯酶抑制剂的快速初筛方法。

Objective: To establish a rapid ion mobility spectrometry(IMS) method for detecting seven kinds of phosphodiesterase type 5 inhibitors(sildenafil,nor-acetildenafil,tadalafil,aminotadalafil,pseudovardenafil, norneosildenafil,diethylaminetadalafil) in dietary supplements.Methods: A positive mode ion mobility spectrometry(IMS) method was employed to detect seven kinds of phosphodiesterase type 5 inhibitors(sildenafil, nor-acetildenafil,tadalafil,aminotadalafil,pseudovardenafil,norneosildenafil,diethylaminetadalafil).The electrospray ionization(ESI) source voltage was 2.5 kV,and the drift tube voltage was 7.5 kV.The gas inlet and drift tube were both controlled at the temperature of 180℃.Results: The drift time of all seven kinds of phosphodiesterase type 5 inhibitors were between 13.8 and 16.2 ms,and their detection limits were 0.05-2 μg·mL^-1.20 batches of dietary supplements samples were detected by the established method and results showed that sildenafil was detected in 13 batches,tadalafil was detected in 2 batches,both sildenafil and tadalafil were detected in 2 batches.In addition,these results were consistent with that of LC-MS.Conclusion: The established method is rapid and sensitive,which could be used for the rapid detection of undeclared phosphodiesterase type 5 inhibitors(sildenafil,nor-acetildenafil,tadalafil,aminotadalafil,pseudovardenafil, norneosildenafil,diethylaminetadalafil) in dietary supplements.

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