Wiley, Rapid Communications in Mass Spectrometry, 20(22), p. 3089-3099, 2008
DOI: 10.1002/rcm.3705
Full text: Unavailable
A rapid-resolution liquid chromatography/mass spectrometric (RRLC/MS) method for detection and quantitation of polyphenols in grape berry skins and seeds has been developed. Pulp-free berry skins were treated with liquid nitrogen and ground; seeds were also ground. Then, 3 g of samples were extracted with 30 mL of a mixture of methanol/water/formic acid 70:30:1 (v/v/v) under sonication and 1 μL of the final extract was injected into two 100 x 2.1 mm i.d., 1.8 μm Zorbax Eclipse plus C18 columns connected in series. Compounds were fractionated using a gradient elution of acidified acetonitrile/methanol 50:50 (v/v)/water. Columns were thermostatted at 70°C. MS was carried out on an Agilent 6410 QqQ instrument equipped with an electrospray ionization source. Positive and negative MS/MS product ion scans were used for compound identification, whereas positive full scan MS in the m/z range 200-1400 was used for quantitation. By means of mass spectra comparison, various flavonols, flavan-3-ols, anthocyanins and stilbenes were identified. Quantitation was performed by external calibration, and concentration values were corrected for matrix effect that was evaluated in separate experiments. Semi-quantitative estimation was performed for compounds for which standards were not commercially available. Recoveries ranged from 90-102% with relative standard deviation (RSD)