The accuracy, repeatability, and reproducibility characteristics of a liquid chromatographic method for the determination of ochratoxin A (OTA) in white wine, red wine, and beer were established in a collaborative study involving 18 laboratories in 10 countries. Blind duplicates of blank, spiked, and naturally contaminated materials at levels ranging from ≤0.01 to 3.00 ng/mL were analyzed. Wine and beer samples were diluted with a solution containing polyethylene glycol and sodium hydrogen carbonate, and the diluted samples were filtered and cleaned up on an immunoaffinity column. OTA was eluted with methanol and quantified by reversed-phase liquid chromatography with fluorometric detection. Average recoveries from white wine, red wine, and beer ranged from 88.2 to 105.4% (at spiking levels ranging from 0.1 to 2.0 ng/mL), from 84.3 to 93.1% (at spiking levels ranging from 0.2 to 3.0 ng/mL), and from 87.0 to 95.0% (at spiking levels ranging from 0.2 to 1.5 ng/mL), respectively. Relative standard deviations for within-laboratory repeatability (RSDr) ranged from 6.6 to 10.8% for white wine, from 6.5 to 10.8% for red wine, and from 4.7 to 16.5% for beer. Relative standard deviations for between-laboratories reproducibility (RSDR) ranged from 13.1 to 15.9% for white wine, from 11.9 to 13.6% for red wine, and from 15.2 to 26.1% for beer. HORRAT values were ≤0.4 for the 3 matrixes.

An analytical method applying ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was validated for the determination of aflatoxins M2, M1, G2, G1, B2, B1, deoxynivalenol, ochratoxin A, fumonisins B1 and B2, hydrolyzed fumonisins B1 and B2, zearalenone and sterigmatocystin in crackers. The obtained recoveries (70 to 110%) and relative standard deviations (< 13%) were considered satisfactory. Method limits of quantification ranged from 0.20 µg kg-1 (sterigmatocystin) to 12.27 µg kg-1 (deoxynivalenol). The validated method was then applied for mycotoxin determination in 60 cracker samples (cream crackers and water and salt crackers) obtained from the metropolitan area of the state of Rio de Janeiro, RJ. Deoxynivalenol, zearalenone and fumonisin B1 were found, respectively, in 100, 50 and 28% of the analyzed samples. The maximum permissible limits established by Brazilian legislation for deoxynivalenol and zearalenone were not exceeded in the analyzed samples.

Aceitação sensorial e perfil de textura instrumental da carne cozida do pacu (Piaractus mesopotamicus), do tambaqui (Colossoma macropomum) e do seu hibrido tambacu eviscerados e estocados em gelo* Sensory acceptance of cooked, gutted ice-stored pacu (Piaractus mesopotamicus), tambaqui (Colossoma macropomum), and their hybrid tambacu Alexandre Borges,** Bianca Gonçalves Medina,*** Carlos Adam Conte-Junior,**** Mônica Queiroz de Freitas**** ResumoEste estudo teve como objetivo realizar e avaliar o teste de aceitação sensorial e a análise de textura instrumental da carne do pacu, tambaqui e o seu híbrido tambacu eviscerados e estocados em gelo. Os testes de aceitação e análise do perfil de textura instrumental foram realizados na carne cozida dos peixes previamente estocadas em gelo nos dias 1, 5 e 10 dias para pacu e tambacu e estocado nos dias 1, 10 e 18 dias para tambaqui. Para todas as espécies, as análises foram realizadas com 120 consumidores. Nenhuma diferença significativa (p>0,05) na aceitação dos consumidores entre os três períodos de estocagem para todos os peixes nem dos atributos elasticidade, coesividade, mastigabilidade e resiliência na textura instrumental foi observada. Contudo, ocorreu variação dos atributos dureza e adesividade para todas as amostras estudadas nos diferentes períodos de estocagem. Os consumidores de peixe deste experimento apresentaram neofobia alimentar. Conclui-se que os três peixes eviscerados e estocados em gelo mantiveram as características sensoriais aceitáveis durante o tempo de estocagem.Palavras-chave: peixes, aceitação sensorial, textura instrumental, estocagem. AbstractThe objective of this study was to assess the acceptance and instrumental texture of the flesh of gutted ice-stored pacu, tambaqui, and the hybrid tambacu stored in ice. The acceptance and instrumental texture tests were performed on the cooked flesh of the fish (pacu and tambacu) stored in ice for 1, 5, and 10 days, and 1, 10, and 18 days for tambaqui. A total of 120 regular fish consumers performed the sensory analyses of all three fish species. Storage period did not affect the degree of acceptance of any of the three fish (p>0.05). Springiness, cohesiveness, chewiness, and resilience did not vary significantly (p<0.05) but hardness and adhesiveness were statistically affected by storage periods for all three fish. Fish consumers seemed to present food neophobia.In conclusion, gutted ice-stored tambacu, pacu, and tambaqui remained sensorially acceptable over ice storage.