UPLC-DAD-Q-TOF-MS/MS测定缓解体力疲劳类保健品中非法添加的化学物质

Detection of Illegally Added Chemicals in Anti-fatigue Health Foods by UPLC-DAD-Q-TOF-MS/MS Method

目的：利用超高效液相-串联四级杆-飞行时间液质联用系统（UPLC-DAD-Q-TOF-MS/MS），建立快速可靠灵敏的测定缓解体力疲劳类保健食品中违法添加西地那非、他达拉非、伐地那非、红地那非、豪莫西地那非、羟基豪莫西地那非、那莫西地那非、氨基他达拉非、伪伐地那非、硫代艾地那非、那红地那非和育亨宾等12种化学药品的液质联用检测方法。方法：采用UPLC-DAD-Q-TOF-MS/MS液质联用仪，以Agilent ZORBAX Eclipse plus C18为色谱柱；以0.1%甲酸-0.01 mol/L乙酸铵水溶液和甲醇梯度洗脱，流速为0.3 mL/min；ESI正离子模式，一级、二级质谱全扫描，进行 UPLC-DAD-Q-TOF-MS/MS的定性及定量分析。结果：经方法学验证，本方法在2～80μg/mL浓度范围内线性良好、精密度（RSD%）小于2%、回收率在80.5%～98.7%之间。结论：本方法快速、准确、灵敏度高、分离度高，为快速筛查缓解体力疲劳类保健食品中非法添加化学物质提供有力工具。

Objective：To establish a fast,accurate and sensitive method by UPLC-DAD-Q-TOF-MS/MS for the de-tection of 12 kinds of illegally added chemicals in anti-fatigue health foods,such as sildenafil,tadalafil,vardenafil, acetildenafil , homosildenafil , hydorxyhomosildenafil , norneosildenafil , aminotadalafil , pseudovardenafil , thioaildenafil . noracetildenafil,and yohimbine.Methods：Agilent ZORBAX Eclipse plus C18 analysis column was used with mobile phase of 0.01 mol/L ammonium acetate aqueous solution（containing 0.1% formic acid）-methanol and gradient elu-tion,the flow rate was 0.3mL/min. ESI＋ scan and MS/MS mode were taken. Qualitative and quantitative analyses were carried out by UPLC-DAD-Q-TOF-MS/MS.Results：The method was validated. A good linear relationship was showed in the concentration of 2 ~80μg/mL,（RSD 〈2%）and the recovery was obtained in range of 80.5% ~98.7%.Conclusion：This method is fast,accurate and sensitive with a high degree of separation,it can be used as a powerful tool for the fast detection of illegally added chemicals in anti-fatigue health foods.