A high-throughput method for liquid chromatography-tandem mass spectrometry determination of plasma alkylresorcinols, biomarkers of whole grain wheat and rye intake.
Journal article, 2016

Plasma alkylresorcinols are increasingly analyzed in cohort studies to improve estimates of whole grain intake and their relationship with disease incidence. Current methods require large volumes of solvent (>10 ml/sample) and have relatively low daily sample throughput. We tested five different supported extraction methods for extracting alkylresorcinols from plasma and improved a normal-phase liquid chromatography coupled to a tandem mass spectrometer method to reduce sample analysis time. The method was validated and compared with gas chromatography-mass spectrometry analysis. Sample preparation with HybridSPE supported extraction was most effective for alkylresorcinol extraction, with recoveries of 77-82% from 100 μl of plasma. The use of 96-well plates allowed extraction of 160 samples per day. Using a 5-cm NH2 column and heptane reduced run times to 3 min. The new method had a limit of detection and limit of quantification equivalent to 1.1-1.8 nmol/L and 3.5-6.1 nmol/L plasma, respectively, for the different alkylresorcinol homologues. Accuracy was 93-105%, and intra- and inter-batch precision values were 4-18% across different plasma concentrations. This method makes it possible to quantify plasma alkylresorcinols in 100 μl of plasma at a rate of at least 160 samples per day without the need for large volumes of organic solvents.

whole grain

Alkylresorcinols

intake

Plasma biomarkers

Author

Alastair Ross

Chalmers, Biology and Biological Engineering, Food and Nutrition Science

Cecilia Svelander

Chalmers, Biology and Biological Engineering, Food and Nutrition Science

Otto Savolainen

Chalmers, Biology and Biological Engineering, Food and Nutrition Science

Mads Vendelbo Lind

Chalmers, Biology and Biological Engineering, Food and Nutrition Science

J.P. Kirwan

Cleveland Clinic Foundation

I. Breton

Nestle S.A.

J. P. Godin

Nestle S.A.

Ann-Sofie Sandberg

Chalmers, Biology and Biological Engineering, Food and Nutrition Science

Analytical Biochemistry

0003-2697 (ISSN) 1096-0309 (eISSN)

Vol. 499 1-7

Subject Categories

Analytical Chemistry

Nutrition and Dietetics

Infrastructure

Chalmers Infrastructure for Mass spectrometry

Areas of Advance

Life Science Engineering (2010-2018)

DOI

10.1016/j.ab.2015.12.023

PubMed

26827992

More information

Created

10/7/2017