期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1275, 期 -, 页码 1-8出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2012.12.022
关键词
HPLC-APCI-MS; Dispersive liquid-liquid microextraction; beta-Carotene; Retinol; Retinol esters; Fruit juices
资金
- Comunidad Autonoma de la Region de Murcia (CARM, Fundacion Seneca) [15217/PI/10]
- Spanish MICINN [CTQ2009-08267/BQU]
- Hero Espana, S.A.
- Fundacion Seneca, CARM
A detailed optimization of dispersive liquid-liquid microextraction (DLLME) was carried out for developing liquid chromatographic (HPLC) techniques, using both fluorescence and atmospheric pressure chemical ionization mass spectrometric (APCI-MS) detection, for the simultaneous analysis of preforms of vitamin A: retinol (R), retinyl acetate (RA), retinyl palmitate (RP) and beta-carotene (beta-C). The HPLC analyses were carried out using a mobile phase composed of methanol and water, with gradient elution. The APCI-MS and fluorescence spectra permitted the correct identification of compounds in the analyzed samples. Parameters affecting DLLME were optimized using 2 mL of methanol (disperser solvent) containing 150 mu L carbon tetrachloride (extraction solvent). The precision ranged from 6% to 8% (RSD) and the limits of detection were between 0.03 and 1.4 ng mL(-1), depending on the compound. The enrichment factor values were in the 21-44 range. juice samples were analyzed without saponification and no matrix effect was found when using fluorescence detection, so calibration was possible with aqueous standards. However, a matrix effect appeared with APCI-MS, in which case it was necessary to apply matrix-matched calibration. There was great variability in the forms of vitamin A present in the juices, the most abundant ester being retinyl acetate (0.04 to 3.4 mu g mL(-1)), followed by the amount of retinol (0.01 to 0.16 mu g mL(-1)), while retinyl palmitate was not detected, except in the milk-containing juice, in which RP was the main form. The representative carotenoid beta-carotene was present in the orange, peach, mango and multifruit juices in high amounts. The method was validated using two certified reference materials. (C) 2012 Elsevier B.V. All rights reserved.
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