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

AI Article Synopsis

  • Plasma alkylresorcinols are important for studying whole grain intake and disease relationships, but current methods are inefficient with high solvent use and low sample throughput.
  • A new extraction method, HybridSPE, was developed for better recovery (77-82%) from smaller plasma volumes (100 μl) and allows up to 160 samples to be processed daily.
  • The modified liquid chromatography method significantly reduced analysis time to 3 minutes, with high accuracy (93-105%) and low detection limits for different alkylresorcinol homologues.

Article Abstract

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.

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Source
http://dx.doi.org/10.1016/j.ab.2015.12.023DOI Listing

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