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

详细信息	查看全文 | 推荐本文 |

• 作者：Maria N. Irakli^a ; Victoria F. Samanidou^b ; Costas G. Biliaderis^c ; Ioannis N. Papadoyannis^b ; ^{papadoya@chem.auth.gr}
• 关键词：IS ; internal standard ; LOD ; limits of detection ; LOQ ; limits of quantification ; SPE ; solid-phase extraction ; GA ; gallic acid ; PRCA ; protocatechuic acid ; 4-OHBA ; 4-hydroxybenzoic acid ; VA ; vanillic acid ; CA ; caffeic acid ; SRA ; syringic acid ; p-CA ; p-coumar
• 刊名：Food Chemistry
• 出版年：2012
• 期刊代码：48_03088146
• 类别：abs
• 出版时间：1 October, 2012
• 卷：134
• 期：3
• 页码：1624-1632
• 文件大小：503 K

摘要

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 C₁₈ column, 5 渭m (250 mm 脳 4.6 mm) thermostated at 30 掳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 渭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.