Rapid high-performance liquid chromatography-electrospray ionization tandem mass spectrometry method for qualitative and quantitative analysis of virgin olive oil phenolic metabolites in human low-density lipoproteins.

A rapid method for detection and quantification of metabolites of specific olive oil phenolic compounds (hydroxytyrosol monoglucuronide, hydroxytyrosol monosulfate, tyrosol glucuronide, tyrosol sulfate and homovanillic acid sulfate) in low-density lipoprotein (LDL) fractions by solidphase extraction (SPE) and high-performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HPLC/ESIMS/MS) is described. A 3m particle size fast C18 Luna column, 5 cm × 2.0 mm I.D., was used at a flow rate of 0.6 mL/min with a mobile phase consisting of 0.1% (v/v) formic acid (A) and acetonitrile (B). A linear gradient profile was used for separation at column temperature 40 ◦ C. The proposed chromatographic procedure is rapid without loosing its separation efficiency and sensitivity. Validation proofs were carried out for the method described, showing a linear system (r > 0.99) and a recovery of 81.9 and 101.3% for hydroxytyrosol and homovanillic acid, respectively. The results show that this method is effective and can be used in routine analysis. © 2006 Elsevier B.V. All rights reserved.