超高效液相色谱串联质谱法测定酒和功能饮料中3种西地那非衍生物的含量

Determination of 3 kinds of sildenafil derivatives in wine and functional drinks by ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  超高效液相色谱串联质谱法  N-去甲基西地那非  吡唑N-去甲基西地那非  异丁基西地那非  酒  功能饮料

英文关键词:ultra performance liquid chromatography tandem mass spectrometry  N-desmethyl sildenafil  pyrazole N-desmethyl sildenafil  isobutyl sildenafil  wine  functional drinks

中文摘要:

      目的 建立超高效液相色谱串联质谱法(ultra performance liquid chromatography tandem mass spectrometry, UPLC-MS/MS)测定酒和功能饮料中3种西地那非衍生物(N-去甲基西地那非、吡唑N-去甲基西地那非、异丁基西地那非)含量的分析方法。方法 采用Agilent Eclipse Plus C18 (3.0 mm×150 mm, 1.8 μm)反相色谱柱, 0.1%甲酸水和0.1%甲酸乙腈为流动相, 梯度洗脱, 采用多反应监测(multiple reaction monitoring, MRM)检测。结果 在50~500 ng/mL的浓度范围内, N-去甲基西地那非、吡唑N-去甲基西地那非、异丁基西地那非均表现出良好的线性关系, 本方法中3种化合物的检出限(limit of detection, LOD)均为15 ng/mL, 定量限(limit of quantitation, LOQ)均为50 ng/mL。结论 该方法操作简便, 结果可靠, 灵敏度高, 可用于酒和功能饮料中N-去甲基西地那非、吡唑N-去甲基西地那非、异丁基西地那非含量的快速测定。

英文摘要:

      Objective To establish a method for determination of 3 kinds of sildenafil derivatives (N-desmethyl sildenafil, pyrazole N-desmethyl sildenafil, and isobutyl sildenafil) in wine and functional drinks by ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Method The samples were separated on a Agilent Eclipse Plus C18 (3.0 mm×150 mm, 1.8 μm) using 0.1% formic acid solution and 0.1% formic acid acetonitrile as mobile phase with the gradient elution. The samples were determined by multiple reaction monitoring (MRM). Results In the concentration range of 50-500 ng/mL, N-desmethyl sildenafil, pyrazole N-desmethyl sildenafil, and isobutyl sildenafil all showed a good linear relationship. The limits of detection (LODs) of the 3 compounds were 15 ng/mL, and limits of quantitation (LOQs) were 50 ng/mL. Conclusion This method is simple, reproducible and with high sensitivity, which is suitable for the rapid analysis of N-desmethyl sildenafil, pyrazole N-desmethyl sildenafil, and isobutyl sildenafil in wine and functional drinks.