Liposomes as potential masking agents in sport doping. Part 1: analysis of phospholipids and sphingomyelins in drugs and biological fluids by aqueous normal-phase liquid chromatography-tandem mass spectrometry.

摘要: In the present work, aqueous normal-phase liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS), in different acquisition modes, was employed for direct analysis and profiling of nine phospholipid classes (phosphatidic acids, phosphatidylserines, phosphatidylethanolamines, lysophosphatidylethanolamines, phosphatidylglycerols, phosphatidylinositols, phosphatidylcholines, lysophosphatidylcholines, sphingomyelins) biological pharmaceutical matrices. After chromatographic separation by a diol column, detection elucidation sphingomyelin molecular species were performed scan modes. For screening analysis, ions [M + H]+ detected positive precursor ion m/z 184 lyso-phosphatidylcholines sphingomyelins; while phosphatidylethanolamines lyso-phosphatidylethanolamines monitoring neutral loss 141 Da; phosphatidylserines using 184 Da. Molecular [M-H]- instead acquired negative 153 phosphatidic acids phosphatidylglycerols; 241 phosphatidylinositols. identification single species, product spectra [M + HCOO]- phosphatidylcholines other phospholipids considered determined each class compared with fragmentation pattern model reference standard. By this approach, nearly 100 sphingomyelins identified. The optimized method then used characterize profiles human plasma urine samples two phospholipid-based formulations, proving that it also allows discriminate compounds endogenous origin from those resulting intake products containing phospholipidic liposomes. Copyright © 2016 John Wiley & Sons, Ltd.