超高效液相色谱–串联质谱法同时测定露酒中伐地那非、西地那非和他达拉非含量

以甲醇提取样品,采用超高效液相色谱–串联质谱(UPLC–MS/MS)法同时测定露酒中西地那非、伐地那非和他达拉非。以甲醇–0.1%甲酸水溶液为流动相,质谱采用电喷雾ESI+扫描模式,通过多反应监测模式进行定性及定量分析。伐地那非、西地那非和他达拉非的线性范围均为5~1 000μg/L,检出限均为0.001 mg/kg,线性相关系数均大于0.999。实际样品中伐地那非、西地那非、他达拉非的加标回收率分别为91.0%~96.0%,92.0%~96.0%,89.5%~92.4%。测定结果的相对标准偏差均小于2%(n=6)。该方法操作简单、快捷,精密度、回收率高,适用于露酒中伐地那非、西地那非和他达拉非的含量分析。

Determination of Vardenaifl-Sildenaifl and Tadalaifl in Liqueur by UPLC-MS/MS

Samples were extracted by methanol, vardenafil, sildenafiland tadalafil in liqueur were determined by ultra performance liquid chromatography-tandem mass spectrometry at the same time. With mobile phase of methanol-0.1% for-mic acid solution, the mass spectrometry was operated in the positive ion mode of multiple reaction monitoring.The linear range of vardenafil, sildenafil and tadalafil was 5-1 000μg/L, the detection limit was 0.001 mg/kg, and correlation co-efficient was more than 0.999. The average recoveries of vardenafil, sildenafil and tadalafil were 91.0%-96.0%, 92.0%-96.0% and 89.5%-92.4%, respectively, and the relative standard deviation(RSD) was less than 2%(n=6). The method is simple, rapid, high efficiency and yield, which is suitable for determination of vardenafil, sildenafil and tadalafil in liqueur.