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  

Rapid detection of undeclared phosphodiesterase type 5 inhibitors in dietary supplements by ion mobility spectrometry

作　　者：冯雪[1] 尹利辉[1] 金少鸿[1] 朱俐[1] 

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2016年第2期313-320,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：保健食品中违禁物质检测技术研究(2011BAZ02015-2)

摘　　要：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 k V,迁移管电压为7.5 k V,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0.05~2μg·m L^(-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.

关 键 词：离子迁移谱(IMS) 非法添加 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 快速检测 型磷酸二酯酶抑制剂 电喷雾 保健食品 

分 类 号：R917[医药卫生—药物分析学]