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Title: Simplified method for the measurement of plasma alkylresorcinols: biomarker of whole grain intake

Author
item ROGRIGUEZ-MORATO, JOSE - Pompeu Fabra University
item JAYAWARDENE, SARAH - Jean Mayer Human Nutrition Research Center On Aging At Tufts University
item DOLNIKOWSKI, GREGORY - Jean Mayer Human Nutrition Research Center On Aging At Tufts University
item GALLUCCIO, JEAN - Jean Mayer Human Nutrition Research Center On Aging At Tufts University
item LICHTENSTEIN, ALICE - Jean Mayer Human Nutrition Research Center On Aging At Tufts University
item MATTHAN, NIRUPA - Jean Mayer Human Nutrition Research Center On Aging At Tufts University

Submitted to: Rapid Communications in Mass Spectrometry
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 4/1/2020
Publication Date: 4/16/2020
Citation: Rogriguez-Morato, J., Jayawardene, S., Dolnikowski, G., Galluccio, J., Lichtenstein, A.H., Matthan, N.R. 2020. Simplified method for the measurement of plasma alkylresorcinols: biomarker of whole grain intake. Rapid Communications in Mass Spectrometry. 34:e8805. https://doi.org/10.1002/rcm.8805.
DOI: https://doi.org/10.1002/rcm.8805

Interpretive Summary: Consuming diets rich in fruits, vegetables and other fiber-containing foods such as whole grains is associated with better health outcomes. However, it is difficult to accurately measure fiber intake. One way to overcome this challenge is by measuring an objective biomarker of compliance. Alkylresorcinols are compounds that are abundant in the outer layer (bran) of wheat, rye and barley grains and are generally not present in products that have been processed or refined. Alkylresorcinols are absorbed and can be measured in blood samples, so they are considered objective biomarkers of whole grain wheat, barley and rye intake. However, current methods to measure alkylresorcinols involve a time consuming multi-step separation process that hampers applicability in large-scale studies. We report a streamlined method to quantify alkylresorcinols in human plasma samples based on protein precipitation and direct injection into an ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometer. Application of this method to a randomized dietary intervention study indicated that plasma alkylresorcinols were higher after participants consumed a diet enriched in whole grains, compared to a diet enriched in simple sugar or refined grains. This simplified method offers a direct and rapid strategy to measure alkylresorcinols as a biomarker of whole grain intake using small amounts of plasma and can be scaled up for large studies.

Technical Abstract: Rationale: Consumption of whole-grains is negatively associated with cardiovascular disease (CVD) risk but quantification of whole-grain intake is challenging. Alkylresorcinols (ARs) are biomarkers of whole-grain intake. Current methods for AR quantification involve a time consuming multi-step separation process that hampers applicability in large-scale studies. Methods: We report a streamlined method to quantify ARs in human plasma based on protein precipitation and direct injection into an ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometer. Results: Separation of 5 major ARs was achieved, with linearity in the 2 to 100 ng/mL range and a LOD of 2 ng/mL. The method was validated by measuring plasma ARs concentrations of subjects who participated in a randomized, cross-over trial evaluating the effect of carbohydrate-type on CVD risk factors. Fiber contents of a simple-, refined- and unrefined-carbohydrate enriched diet were 8.6, 9.6 and 19.5g/1000kcal, respectively. The unrefined-carbohydrate diet with the highest fiber content resulted in the highest plasma AR concentration (125+/-56 nmol/L), and was significantly different (p<0.05) from the other lower fiber diets (29+/-10 nmol/L and 27+/-9 nmol/L, simple and unrefined-carbohydrate, respectively). Conclusions: This method offers a simplified approach to measure plasma ARs concentrations as an objective biomarker of whole-grain intake that can be applied to large-scale cohort studies.