Quantification of alkylresorcinols in human plasma by liquid chromatography/tandem mass spectrometry

• Published in: Rapid communications in mass spectrometry Vol. 24; no. 5; pp. 554 - 560
• Main Authors: Ross, Alastair B., Redeuil, Karine, Vigo, Mario, Rezzi, Serge, Nagy, Kornél
• Format: Journal Article
• Language: English
• Published: Chichester, UK John Wiley & Sons, Ltd 15-03-2010
• Subjects: Biomarkers - blood; Chromatography, Liquid - methods; Diet; Epidemiology; Human; Humans; Intakes; Liquid chromatography; Liquid-liquid extraction; Mass spectrometry; Reproducibility of Results; Resorcinols - blood; Rye; Secale; Sensitivity and Specificity; Solid Phase Extraction - methods; Tandem Mass Spectrometry - methods; Triticum; Wheat
• ISSN: 0951-4198; 1097-0231; 1097-0231
• DOI: 10.1002/rcm.4409

Alkylresorcinols (AR) are of interest as biomarkers of wholegrain wheat and rye intake in epidemiological studies and are currently mainly measured by gas chromatography/mass spectrometry (GC/MS) after labour‐intensive sample preparation including liquid‐liquid extraction, solid‐phase extraction (SPE) and chemical derivatization. This manuscript describes and validates an alternative approach based on normal‐phase liquid chromatography/tandem mass spectrometry for the quantification of alkylresorcinols in human plasma. The method requires neither SPE nor chemical derivatization and has a shortened run time compared to GC/MS. Normal‐ and reversed‐phase columns and various mobile phases were evaluated with and without previous SPE of the samples. Normal‐phase chromatography allowed separation of AR from the interfering triacylglycerols, diacylglycerols and sterols and enabled detection of AR even without SPE of the samples. The described method has instrumental lower limits of detection in the 25–75 pg range, and lower limits of quantification in the 75–250 pg range. Pooled human plasma and 2H4‐nonadecylresorcinol (internal standard) was applied to calibrate the method in the 20–12 000 nM range. The overall method showed intra‐batch precision of 8.6% and an averaged accuracy of 100.2%. Applications for diverse human plasma samples are presented and are compared with the results determined by GC/MS. Based on the presented data; this method requiring less sample preparation is suggested for further evaluation as an alternative to GC/MS for analysis of biomarkers of wholegrain wheat and rye intake in epidemiological studies. Copyright © 2010 John Wiley & Sons, Ltd.