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

Determination of Vardenafil–Sildenafil and Tadalafil in Liqueur by UPLC–MS/MS

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5～1 000 μg/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.

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.