HPLC-TOF/MS检测补肾强身胶囊中西地那非和他达那非

HPLC-TOF/MS determination of sildenafil and tadalafil in the capsule of aphrodisiacs

目的:建立液相色谱飞行时间质谱联用法(HPLC-TOF/MS)测定补肾强身胶囊中非法添加西地那非和他达那非的定性定量分析方法。方法:以HPLC-TOF/MS通过色谱保留时间,小于3 ppm的质量精度测定,样品与对照品源内碰撞诱导解离(CID)及同位素丰度比来进行定性分析;再以被测物提取离子的峰面积进行定量分析。结果:供试品中西地那非、他达那非与对照品色谱峰的保留时间一致,质量精度小于2.5 ppm;对照品与样品源内CID碎片离子相似;同位素丰度比推测结果相似;提取离子的回归方程分别为Y=9.92×10~5C-4.51×10~5(r=0.9994,n=5),Y=1.96×10~5C-2.70×10~3(r=0.9990,n=5);线性范围分别为0.0715～35.75和0.1006～50.30μg·mL^(-1);最低检测限(以信噪比为3:1计)分别为4和6 ng·mL^(-1);精密度RSD(n=5)分别为2.0%和0.97%;重复性RSD(n=5)分别为2.0%和3.7%;回收率分别为98.9%和90.9%(n=9)。结论:该方法简便、快速、灵敏、准确,适于同时对补肾强身胶囊中西地那非和他达那非定性、定量。

Objective：A qualitative and quantitative HPLC -TOF/MS analytical method for sildenafil and tadalafil illegally added in the capsule of aphrodisiacs has been developed. Method：The two compounds were identified by retention time, the quailty precision measurement with in 3 ppm, the in - source collision induced dissociation （CID） of sample and reference substance, isotopic ratio by MS, and then quantified by the peak area of the extraction ions. Results：For the sample and reference substance of sildenafil and tadalafil , the retention time of chromatographic peaks were uniform, and the quailty precisions were less than 2.5 ppm. The in - source CID of the sample and reference substance were similar. The conjectured results of isotopic ratio were similar too. The regression equation of extraction ions were Y = 9.92 ×10^5 C - 4.51 × 10^5, r = 0. 9994 （ n = 5 ） , Y = 1 . 96 × 10^5 C - 2. 70 × 10^3, r = 0. 9990 （ n =5）. The linear ranges were 0. 0715 -35.75 μg · mL^-1 and 0. 1006 -50. 30 μg · mL^-1. The detection limits （S/ N = 3 ） for sildenafil and tadalafil were 4 and 6 ng· mL^- 1, and the relative standard deviations were 2.0% , 0. 97%. The reapetabilities were 2.0% ,3.7% and the average recoveries were 98.9% ,90.9% （ n =9）. Conclusion：This method is simple, fast , sensitive, accurate. It is applicable in the qualitative and quantitative analytical method to sildenafil and tadalafil added in the capsule of aphrodisiacs.