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[摘要]
建立固相萃取-超高效液相色谱-串联质谱/质谱法(SPE-UPLC-MS/MS)测定保健品中伐地那非、西地那非、他达那非的分析方法。试样经甲醇或盐酸溶液提取,HLB固相萃取柱净化后,以乙腈和0.1 %甲酸水溶液作为流动相,C18色谱柱分离,采用电喷雾离子源,正离子扫描多反应监测(MRM)模式进行检测。伐地那非、西地那非、他达那非在10~200 μg/L浓度范围内呈良好线性关系,相关系数(r2)均大于0.99。空白样品加标回收率均大于75 %,相对标准偏差小于8 %。胶囊样品中伐地那非、西地那非、他达那非的方法检出限分别为10 μg/kg、10 μg/kg、20 μg/kg;定量限分别为40 μg/kg、40 μg/kg、80 μg/kg。口服液中分别为3 μg/L、3 μg/L、6 μg/L,定量限分别为10 μg/L、10 μg/L、20 μg/L。研究了基质效应的影响,样品基质对伐地那非、西地那非、他达那非的响应表现为抑制作用,伐地那非受到抑制作用最明显。
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[Abstract]
A method was established for the determination of vardenafil, sildenafil, and tadalafil in health foods using solid-phase extraction–ultra-performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The sample was extracted by methanol or hydrochloric acid, and then purified by a hydrophilic/lipophilic balanced (HLB) SPE column. The target compounds were separated on a reversed phase column using a solution of acetonitrile and 0.1 % formic acid in water as the mobile phase, and then detected by positive electrospray ionization under multiple reaction monitoring (MRM) mode. Good linearity of the calibration curves was achieved for three target compounds in the range of 10 ~200 μg/L, with correlation coefficients (r2) greater than 0.99. The average recoveries of the blank matrix sample were all more than 75%, and the relative standard deviations (RSDs) were less than 8%. The limits of detection (LOD) for vardenafil, sildenafil, and tadalafil in the capsule form were 10 μg/kg, 10 μg/kg, and 20 μg/kg, respectively. The limits of quantitation (LOQs) for vardenafil, sildenafil, and tadalafil in the capsule form were 40 μg/kg, 40 μg/kg, and 80 μg/kg, respectively. For oral samples, the LODs were 3 μg/L, 3 μg/L, and 6 μg/L, respectively; the LOQs were 10 μg/L, 10 μg/L, and 20 μg/L, respectively. The sample matrix effects were also studied, which had a suppressive effect on the response of vardenafil, sildenafil, and tadalafil, and the most significant suppressive effect was found on vardenafil.
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