The extraction procedures (solid/liquid SPE and liquid/liquid LLE) and HPLC separation and quantification methods of polyphenolic compounds have been checked in virgin olive oils in order to explain the differences in content reported in the literature. The work has been carried out on oils prepared from one cultivar and produced under the same protocol. The extraction methods are practically equivalent, but the SPE technique is more favorable because it is faster and simpler. It has been proved that the chromatographic features and the method of chemical expression of the concentrations may greatly affect the final values. Thus, under the same analytical method, the total concentration values of polyphenols of the same oil show variations from 18% to 80%, according to the formality of expression as gallic acid, caffeic acid, or tyrosol equivalents. The role of the nature and spectrophotometric features of the phenols and of the internal standard is also discussed, and it was found to be an important source of reported variation. A gradient separation with an eluent mixture acetonitrile-sulfuric acid (0.1 mol/L), detection at 225 nm, and quantitative calculation of polyphenolic compounds in oils (expressed as tyrosol equivalents, THY(eq)) is proposed.
The fate of four new fungicides (cyprodinil, fludioxonil, pyrimethanil,
and tebuconazole) from the
treatment on vine to the production of wine was studied. The
influence of clarifying agents
(bentonite, charcoal, potassium caseinate, gelatin, and
polyvinylpolypyrrolidone) on residue
concentrations in wine was also studied. The fungicide residues on
grapes showed different decay
rates after treatment, with first-order kinetics and half-lives ranging
from 8 to 57 days. Grape
processing into wine caused considerable residue reduction with
cyprodinil (ca. 80%), fludioxonil
(ca. 70%), and tebuconazole (ca. 50%) and no
reduction with pyrimethanil. The two wine-making
techniques employed (with and without maceration) had the same
influence on the residue
concentrations in wine, except for fludioxonil which showed maximum
residue reduction with
vinification with maceration. Among the clarifying agents tested,
only charcoal showed effective
action on the elimination of residue content in wine, proving complete
elimination, or almost, of
fungicide residues.
Keywords: Fungicides; residues; wine-making
The stability of extra virgin olive oils is mainly due to their relatively low fatty acids unsaturation and to the antioxidant activity of some of the unsaponifiable components. We studied the activity of alpha-tocopherol in extra virgin olive oil in its natural state, using new and simple oxidizing conditions in "thin layer" and "bulk phase". Oxidation time course was monitored at 37 degrees C or 75 degrees C. A storage test was also performed. Two parameters were evaluated: depletion of alpha-tocopherol and formation of PUFA hydroperoxides, measured as conjugated dienes (CD) and peroxide value. The value of complex polyphenols was also measured. alpha-Tocopherol concentration decreased in function of time and temperature and showed a strong inverse correlation with the increase of CD. When alpha-tocopherol reached a "threshold value" of 60-70 mg/kg, a significant increase of CD formation was observed, together with a good correlation between CD and peroxide value. The initial amount of alpha-tocopherol is one of the components that influences oil oxidative susceptibility.
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