Development and validation of an HPLC-method for determination of free and bound phenolic acids in cereals after solid-phase extraction

作者：Irakli Maria N; Samanidou Victoria F; Biliaderis Costas G; Papadoyannis Ioannis N^*

来源：Food Chemistry, 2012, 134(3): 1624-1632.

DOI：10.1016/j.foodchem.2012.03.046

• Phenolic acids
• Cereals
• SPE
• HPLC

Whole cereal grains are a good source of phenolic acids associated with reduced risk of chronic diseases. This paper reports the development and validation of a high-performance liquid chromatography-diode array detection (HPLC-DAD) method for the determination of phenolic acids in cereals in either free or bound form. Extraction of free phenolic acids and clean-up was performed by an optimised solid-phase extraction (SPE) protocol on Oasis HLB cartridges using aqueous methanol as eluant. The mean recovery of analytes ranged between 84% and 106%. Bound phenolic acids were extracted using alkaline hydrolysis with mean recoveries of 80-95%, except for gallic acid, caffeic acid and protocatechuic acid. Both free and bound phenolic extracts were separated on a Nucleosil 100 C-18 column, 5 mu m (250 mm x 4.6 mm) thermostated at 30 degrees C, using a linear gradient elution system consisting of 1% (v/v) acetic acid in methanol. Method validation was performed by means of linearity, accuracy, intra-day and inter-day precision and sensitivity. Detection limits ranged between 0.13 and 0.18 mu g/g. The method was applied to the analysis of free and bound phenolic acids contents in durum wheat, bread wheat, barley, oat, rice, rye, corn and triticale.

• 出版日期2012-10-1