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Ochratoxin A is the main contaminant mycotoxin of grapes produced mainly by Aspergillus niger and Aspergillus carbonarius. Besides, it is possible that the formation of modified mycotoxin occurs through the plant defense mechanism or also by fungus actions itself. The objective of this study was to evaluate the influence of grape variety and maturation stage on the formation of OTA and modified mycotoxin. The determination of OTA was performed by high-performance liquid chromatography, and a high-resolution mass spectrometry was used for the detection of modified ochratoxin. A positive correlation was observed between the following grapes physicochemical parameters: pH, total soluble solids, total glycosides in glucose, total anthocyanin, and OTA levels produced by A. niger and A. carbonarius. Therefore, the higher the concentrations of these parameters, the greater the production of mycotoxin in grapes. Among the elected targets, we identified the 14-decarboxy-ochratoxin A in Muscat Italia variety at veraison and 15 days after the beginning of veraison stages; and ethylamide-ochratoxin A as a biomarker in the Syrah variety at the ripeness stage.

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Recebido em 8/11/12; aceito em 30/4/13; publicado na web em 10/6/13 QUANTIFICATION OF BETA-LACTAM ANTIBIOTICS IN VETERINARY DRUGS: AMOXICILLIN AND AMPICILLIN DETERMINATION BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY. This work focused on the development and validation of an RP-HPLC-UV method for quantification of beta-lactam antibiotics in three pharmaceutical samples. Active principles analyzed were amoxicillin and ampicillin, in 3 veterinary drugs. Mobile phase comprised 5 mmol L-1 phosphoric acid solution at pH 2.00, acetonitrile with gradient elution mode and detection wavelength at 220 nm. The method was validated according to the Brazilian National Health Surveillance regulation, where linear range and linearity, selectivity, precision, accuracy and ruggedness were evaluated. Inter day precision and accuracy for pharmaceutical samples 1, 2 and 3 were: 1.43 and 1.43%; 4.71 and 3.74%; 2.72 and 1.72%, respectively, while regression coefficients for analytical curves exceeded 0.99. The method had acceptable merit figure values, indicating reliable quantification. Analyzed samples had active principle concentrations varying from-12 to +21% compared to manufacturer label claims, rendering the medicine unsafe for administration to animals.