Rapid Screening and Confirmation of Illegally Added Phosphodiestrase-5 Inhibitors and Analogues in Health Foods by Liquid Chromatography-Ion Trap-Time of Flight Tandem Mass Spectrometry
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Rapid Screening and Confirmation of Illegally Added Phosphodiestrase-5 Inhibitors and Analogues in Health Foods by Liquid Chromatography-Ion Trap-Time of Flight Tandem Mass Spectrometry
Vol. 33, Issue 3, Pages: 239-247(2014)
作者机构:
1. 湖南出入境检验检疫局技术中心
2. 湖南师范大学化学化工学院
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Rapid Screening and Confirmation of Illegally Added Phosphodiestrase-5 Inhibitors and Analogues in Health Foods by Liquid Chromatography-Ion Trap-Time of Flight Tandem Mass Spectrometry. [J]. 33(3):239-247(2014)
DOI:
Rapid Screening and Confirmation of Illegally Added Phosphodiestrase-5 Inhibitors and Analogues in Health Foods by Liquid Chromatography-Ion Trap-Time of Flight Tandem Mass Spectrometry. [J]. 33(3):239-247(2014)DOI:
Rapid Screening and Confirmation of Illegally Added Phosphodiestrase-5 Inhibitors and Analogues in Health Foods by Liquid Chromatography-Ion Trap-Time of Flight Tandem Mass Spectrometry
A method was developed for the screening and confirmation of 28 illegally added phosphodiestrase-5 inhibitors(PDE-5) including sildenafil,tadalafil,vardenafil and analogues in health foods by liquid chromatography-ion trap-time of flight tandem mass spectrometry(LC-MS-IT-TOF).The accurate mass and multiple-stage mass spectrometry databases of 28 compounds were established.The analytes in samples were extracted with methanol and separated on a C18 column(150 mm×4.6 mm,3.5 μm) by gradient elution using acetonitrile-0.1% acetic acid as mobile phase.The results showed that the limits of detection(LOD,S/N≥3) were in the range of 0.2-7.0 μg/L.The limits of quantitation(LOQ,S/N≥10) were in the ranges of 0.04-1.18 mg/kg for capsule and 0.007-0.235 mg/L for oral solution,respectively.The method validation was carried out by LOQ levels,and the recoveries were in the range of 31.0%-114.0% with relative standard deviations(RSDs) of 25%-149%.The screening of analytes was performed by precision mass matching and library searching.The retention time,isotopic abundance and multiple-stage ion mass spectra were employed for the confirmation.This method is simple,rapid,credible and sensitive,and could be applied in the simultaneous screening and identification for illegally added PDE-5 and analogues in health foods.Moreover,the ion fragmentation patterns of these drugs could be exploited to predict the chemical formulas and structures of the unknown derivatives and structural analogs of phosphodiestrase-5 inhibitors.
关键词
保健食品磷酸二酯酶-5抑制剂类似物筛查离子阱飞行时间串联质谱
Keywords
health foodphosphodiestrase-5 inhibitoranaloguescreeningliquid chromatography-ion trap-time of flight tandem mass spectrometry(LC-MS-IT-TOF)
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