The purpose of this study was to establish a reliable, cost-effective, fast and simple method to quantify simultaneously both bisphenol A (BPA) and bisphenol B (BPB) in liquid food matrixes such as canned beverages (soft drinks and beers) and powdered infant formula using dispersive liquid–liquid micro-extraction (DLLME) with in-situ derivatisation coupled with heart-cutting gas chromatography-mass spectrometry (GC-MS). For the optimisation of the DLLME procedure different amounts of various extractive and dispersive solvents as well as different amounts of the derivative reagent were compared for their effects on extraction efficiency and yields. The optimised procedure consisted of the injection of a mixture containing tetrachloroethylene (extractant), acetonitrile (dispersant) and acetic anhydride (derivatising reagent) directly into an aliquot of beverage samples or into an aqueous extract of powdered milk samples obtained after a pretreatment of the samples. Given the compatibility of the solvents used, and the low volumes involved, the procedure was easily associated with GC-MS end-point determination, which was accomplished by means of an accurate GC dual column (heart-cutting) technique. Careful optimisation of heart-cutting GC-MS conditions, namely pressure of front and auxiliary inlets, have resulted in a good analytical performance. The linearity of the matrix-matched calibration curves was acceptable, with coefficients of determination (r2) always higher than 0.99. Average recoveries of the BPA and BPB spiked at two concentration levels into beverages and powdered infant formula ranged from 68% to 114% and the relative standard deviation (RSD) was <15%. The limits of detection (LOD) in canned beverages were 5.0 and 2.0 ng l^–1 for BPA and BPB, respectively, whereas LOD in powdered infant formula were 60.0 and 30.0 ng l^–1, respectively. The limits of quantification (LOQ) in canned beverages were 10.0 and 7.0 ng l–1 for BPA and BPB, respectively, whereas LOQ in powdered infant formula were 200.0 and 100.0 ng l^–1, respectively. BPA was detected in 21 of 30 canned beverages (ranging from 0.03 to 4.70 µg l^–1) and in two of seven powdered infant formula samples (0.23 and 0.40 µg l^–1) collected in Portugal. BPB was only detected in canned beverages being positive in 15 of 30 samples analysed (ranging from 0.06 to 0.17 µg l^–1). This is the first report about the presence of BPA and BPB in canned beverages and powdered infant formula in the Portuguese market.

The objectives of this study were to monitor the changes in chemical [moisture, acidity, pH, and water activity (a(w))] and physical (color and texture) parameters of "Terrincho" ewe cheese during 60 d of ripening, and to determine the correlations between the changes in instrumental texture and color parameters and the ripening time of the product. Intravarietal comparison of Terrincho ewe cheese from 5 different dairy plants was performed by evaluation of mechanical parameters from texture profile analysis (TPA) and color parameters in terms of CIELAB color space (L*, a*, and b*). In addition to mechanical and color tests, composition analyses and sensory tests were performed. The results were evaluated with statistical methods (single valued and multivariate analysis). During the first 20 d of ripening, an increase in hardness, fracturability, gumminess, chewiness, and yellowness occurred. Simultaneously, adhesiveness, resilience, L* (inside cheese, "i" and external "e"), and cohesiveness decreased. After 20 d of ripening hardness, fracturability, gumminess, and chewiness decreased and cohesiveness increased. The ripening time of Terrincho cheeses can be estimated with 6 variables: L* (external, e), L* (i), b* (inside cheese, i), hardness, a* (i), chewiness, and a constant. The estimation error was 4.2 d. Evaluation of composition, pH, texture profile analyses, color, and related sensory characteristics of Terrincho cheeses from 5 different dairy plants (with 30 d of ripening) revealed correlations between these parameters.