摘要
目的建立一种超高效液相色谱-三重四极杆/复合线性离子阱质谱(ultra performance liquid chromatography-triple quadrupole linear/ion trap of mass spectrometry,UPLC-Qtrap-MS/MS)检测方法,用于保健食品中西地那非类衍生物的快速筛查和鉴定。方法样品经甲醇提取,经甲醇-水(50:50,V:V)适当稀释,采用0.1%甲酸水(A)和0.1%甲酸乙腈(B)作为流动相进行洗脱,质谱(ESI+)采用母离子扫描模式(precursor ion)对西地那非类似物进行检测,利用一级、二级、三级质谱碎片进行结构解析。结果通过该方法成功发现了一种新型的西地那非类衍生物。结论该方法快速、准确、灵敏,可用于保健食品中西地那非类衍生物的筛查。
Objective To establish an method for rapid screening and determination of sildenafil analogues illegally added in healthy foods by ultra performance liquid chromatography-triple quadrupole linear/ion trap of mass spectrometry（UPLC-Qtrap-MS/MS）. Methods After samples were extracted with methanol solution and diluted with 50% MeOH to an appropriate concentration, H2O（0.1% formic acid） and acetonitrile（0.1% formic acid） were employed to elute samples. The mass spectrometer operated in positive ion and in precursor ion mode to determine the sildenafil analogues. The structural properties of this analogue were elucidated by MS, MS～2, MS～3 spectroscopy. Results A new type of sildenafil analogues illegally was successfully discovered by this method. Conclusion The method is rapid, accurate and sensitive, which can be used to detect sildenafil analogues illegally added in health foods.
出处
《食品安全质量检测学报》
CAS
2017年第10期3991-3996,共6页
Journal of Food Safety and Quality
基金
陕西省科技统筹创新工程项目(2014FWPT-01)~~
关键词
西地那非类衍生物
超高效液相色谱-三重四极杆-线性离子阱质谱
母离子扫描模式
保健食品
sildenafil analogues
ultra performance liquid chromatography-triple quadrupole linear/ion trap of mass spectrometry
precursor ion scan mode
healthy foods
