title: A new and improved strategy combining a dispersive-solid phase extraction-based multiclass method with ultra high pressure liquid chromatography for analysis of low molecular weight polyphenols in vegetables.
abstract: This paper reports on the development and optimization of a modified Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) based extraction technique coupled with a clean-up dispersive-solid phase extraction (dSPE) as a new, reliable and powerful strategy to enhance the extraction efficiency of free low molecular-weight polyphenols in selected species of dietary vegetables. The process involves two simple steps. First, the homogenized samples are extracted and partitioned using an organic solvent and salt solution. Then, the supernatant is further extracted and cleaned using a dSPE technique. Final clear extracts of vegetables were concentrated under vacuum to near dryness and taken up into initial mobile phase (0.1% formic acid and 20% methanol). The separation and quantification of free low molecular weight polyphenols from the vegetable extracts was achieved by ultrahigh pressure liquid chromatography (UHPLC) equipped with a phodiode array (PDA) detection system and a Trifunctional High Strength Silica capillary analytical column (HSS T3), specially designed for polar compounds. The performance of the method was assessed by studying the selectivity, linear dynamic range, the limit of detection (LOD) and limit of quantification (LOQ), precision, trueness, and matrix effects. The validation parameters of the method showed satisfactory figures of merit. Good linearity (Rvalues2>0.954; (+)-catechin in carrot samples) was achieved at the studied concentration range. Reproducibility was better than 3%. Consistent recoveries of polyphenols ranging from 78.4 to 99.9% were observed when all target vegetable samples were spiked at two concentration levels, with relative standard deviations (RSDs, n=5) lower than 2.9%. The LODs and the LOQs ranged from 0.005 μg mL(-1) (trans-resveratrol, carrot) to 0.62 μg mL(-1) (syringic acid, garlic) and from 0.016 μg mL(-1) (trans-resveratrol, carrot) to 0.87 μg mL(-1) ((+)-catechin, carrot) depending on the compound. The method was applied for studying the occurrence of free low molecular weight polyphenols in eight selected dietary vegetables (broccoli, tomato, carrot, garlic, onion, red pepper, green pepper and beetroot), providing a valuable and promising tool for food quality evaluation.
authors.affiliation: Centro de Química da Madeira, Centro de Ciências Exactas e da Engenharia da Universidade da Madeira, 9000-390 Funchal, Portugal.
authors.forename: Catarina L
authors.initials: CL
authors.lastname: Silva
authors.forename: Nathaly
authors.initials: N
authors.lastname: Haesen
authors.forename: José S
authors.initials: JS
authors.lastname: Câmara
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D000704:Analysis of Variance; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D016018:Least-Squares Analysis; D057230:Limit of Detection; D008278:Magnesium Sulfate / Q000737:chemistry; D008970:Molecular Weight; D059808:Polyphenols / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D012965:Sodium Chloride / Q000737:chemistry; D052616:Solid Phase Extraction / Q000379:methods*; D014675:Vegetables / Q000737:chemistry*
chemical_list: D000097:Acetonitriles; D059808:Polyphenols; D012965:Sodium Chloride; D008278:Magnesium Sulfate; C032159:acetonitrile