质谱学报2016，Vol.37Issue(6)：554-561,8.DOI:10.7538/zpxb.youxian.2016.0034
超高效液相色谱-串联质谱法测定保健食品中10种磷酸二酯酶-5抑制剂
Simultaneous Determination of Ten Phosphodiesterase-5 Inhibitors in Health Foods by Ultra Performance Liquid Chromatography with Tandem Mass Spectrometry
摘要
Abstract
A method was developed for simultaneous determination of ten phosphodies-terase-5 (PDE-5)inhibitors in health foods by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),such as vardenafil,acetildenafil,sildena-fil,homosildenafil,udenafil,tadalafil,thioaildenafil,gendenafil,pseudovarnafil,nor-neosildenafil.The separation was performed using water containing 0.1% formic acid and methanol as mobile phases with gradient elution at a flow rate of 0.2 mL/min. Qualitative and quantitative analysis were achieved after the chromatographic separation on a Waters Acquity UPLC BEH C18 column (100 mm×2.1 mm×1.7 μm).The elec-trospray ionization (ESI)source in positive ion mode was used for analysis of ten phos-phodiesterase-5 inhibitors in the multiple reaction monitoring (MRM)mode.The nucle-ar ratio of parent ion and daughter ion,cone voltage,collision voltage were investiga-ted.The sample was ultrasonic-assisted treatment using the methanol as extraction sol-vent,and then purified by Waters Oasis HLB solid-phase extraction (SPE)column. The results indicate that the linear range of the method is from 1.0 μg/L to 100.0 μg/L with R 2 >0.993,which means the method has a good linearity.The limits of detection (LOD)and limits of quantification (LOQ)of ten phosphodiesterase-5 inhibitors are 0.3-1.0 μg/kg and 1.0-2.5 μg/kg,respectively.The average recoveries of ten phosphodies-terase-5 inhibitors at three spiked levels of 100.0,200.0 and 1 000.0 μg/kg are 85.6%-94.3%.The method was applied to analysis of the investigated compounds in twenty health foods.The results indicate that sildenafil are found in eighteen samples with the range of 1.3-210.8 mg/g,vardenafil and tadalafil are found in a tablet and a capsule, respectively.This method is accurate,simple,rapid and feasible for simultaneous deter-mination of phosphodiesterase-5 inhibitors in health foods.关键词
超高效液相色谱-串联质谱 (UPLC-MS/MS)/磷酸二酯酶-5抑制剂(PDE-5 )/固相萃取/保健食品Key words
ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)/phosphodiesterase-5 inhibitors (PDE-5)/solid phase extraction/health foods分类
化学化工引用本文复制引用
勾新磊,赵新颖,高峡,周明强,刘伟丽..超高效液相色谱-串联质谱法测定保健食品中10种磷酸二酯酶-5抑制剂[J].质谱学报,2016,37(6):554-561,8.基金项目
北京市科学技术研究院创新工程Ⅲ-1项目(2015-178305) （2015-178305）
北京市科学技术研究院萌芽计划项目(2015-02)资助 （2015-02）
