Application of a high resolution benchtop quadrupole-Orbitrap mass spectrometry for the rapid screening, confirmation and quantification of illegal adulterated phosphodiesterase-5 inhibitors in herbal medicines and dietary supplements

作者: Feng Shi , Changchuan Guo , Liping Gong , Jun Li , Peng Dong

DOI: 10.1016/J.CHROMA.2013.12.030

关键词: Mass spectrometryQuantitative analysis (chemistry)Routine screeningOrbitrapChemistryLinear relationshipResolution (mass spectrometry)Dietary supplementChromatographyDetection limit

摘要: In this study, the applicability of high resolution quadrupole-Orbitrap (Q-Orbitrap) mass spectrometry for simultaneous qualitative and quantitative analysis illegal adulterated phosphodiesterase-5 inhibitors (PDE-5 inhibitors) in herbal medicines dietary supplements was investigated. The spectrometer operated full MS scan/dd-MS(2) (data-dependent MS(2)) mode. use 70,000 FWHM narrow windows (5 ppm) could effectively improve selectivity method, increasing signal-to-noise ratio analytes. response showed good linear relationship with analytes' concentrations over wide ranges (e.g., 0.05-10 μg/g sildenafil) all coefficient determinations (r(2)) >0.9996. detection limits (LODs) were range 1.0-5.0 ng/g different recoveries ranged from 85.4% to 96.7%. intra- inter-day accuracies -6.6 10.1%, while precision 0.0039% 13.2%. Among 68 batches 20 (including 83 capsules, 3 pellets 2 liquid) samples, sildenafil detected 8 supplements, noracetildenafil only one supplement. novel Q-Orbitrap has been proved be a very promising powerful tool routine screening adulterate ensuring food safety public health.

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