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

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• 作者：Alastair B. Ross^a ; ^{alastair.ross@chalmers.se" class="auth_mail" title="E-mail the corresponding author} ; Cecilia Svelander^a ; Otto I. Savolainen^a ; Mads Vendelbo Lind^a ; ^b ; John P. Kirwan^c ; Isabelle Breton^d ; Jean-Philippe Godin^d ; Ann-Sofie Sandberg^a
• 关键词：Alkylresorcinols ; Biomarkers ; Blood plasma ; Whole grain ; Liquid chromatography&ndash ; tandem mass spectrometry
• 刊名：Analytical Biochemistry
• 出版年：2016
• 出版时间：15 April 2016
• 年：2016
• 卷：499
• 期：Complete
• 页码：1-7
• 全文大小：332 K

文摘

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.