作者: João Gonçalves , Catarina L. Silva , Paula C. Castilho , José S. Câmara
DOI: 10.1016/J.MICROC.2012.05.037
关键词: Vanillic acid 、 Syringic acid 、 Gentisic acid 、 Chemistry 、 Chromatography 、 Sample preparation 、 Elution 、 Hydroxybenzoic acid 、 Coumaric acid 、 Formic acid
摘要: Abstract An attractive, fast, low-consumption and very promising high-throughput strategy based on microextraction by packed sorbent (MEPS), reversed phase ultra-high pressure liquid chromatography (UHPLC), was developed validated for the determination quantification of hydroxybenzoic (gallic acid, protocatechuic gentisic vanillic syringic acid), hydroxycinnamic acids ( p -coumaric m o ferrulic acid cinnamic acid) in wines. Important factors affecting performance MEPS such as type material (C2, C8, C18, SIL C8/SCX), number extraction cycles (extract–discard), sample volume elution were tested optimized. The optimal conditions obtained using C8 50 μL five cycles. analytes separated a new Trifunctional High Strength Silica analytical column (HSS T3; 100% silica particle), specially designed polar compounds, binary mobile composed aqueous 0.1% formic (eluent A) methanol B) gradient mode (10 min total analysis). This stationary phase, proved to be an excellent alternative conventional C18 columns benzoic derivatives method fully terms linearity, limits detection (LOD), (LOQ), yield, accuracy inter/intra-day precision, synthetic wine spiked with acids, demonstrated good linearity r 2 ‐values > 0.998 within established concentration range (0.2–40 μg mL − 1 ). Under optimized conditions, LOD 0.01–0.2 μg mL , LOQ 0.03–0.7 μg mL expressed relative standard deviation (RSD %), 0.3–6% observed. proposed also applied analysis red white wines recoveries 80–100% 77–99%, respectively, obtained. approach offers attractive phenolic from samples, providing advantages including decreased preparation, faster throughput easy perform compared traditional methodologies. Moreover it could potentially extended other media.