超高效液相色谱-串联质谱法同时测定保健品中三种违禁成分.pdf

现代食品科技 Modern Food Science and Technology 2014, Vol.30, No.11 超高效液相色谱-串联质谱法同时测定保健品中 三种违禁成分 李锦清，綦艳，郦明浩，龙顺荣，邱启东 （广东产品质量监督检验研究院，广东顺德528300） 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。 关键词：UPLC-MS/MS 法；保健品；伐地那非；西地那非；他达那非；基质效应 文章篇号：1673-9078(2014)11-246-250 DOI: 10.13982/j.mfst.1673-9078.2014.11.043 Simultaneous Determination of Sildenafil, Vardenafil, and Tadalafil in Health Foods by Ultra-performance Liquid Chromatography Tandem Mass Spectrometry LI Jin-qing, QI Yan, LI Ming-hao, LONG Shun-rong, QIU Qi-dong (Guangdong Testing Institute for Product Quality Supervision, Shunde 528300, China) 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) m