RESUMEN
A total of 480 milk samples were analyzed in four repetitions with four preservative treatments (no preservative, Bronopol, Bronolat and Brononata), three storage times at temperatures up to 4 °C (24, 48 and 72hours after reception), five different water additions (0.0, 2.5, 5.0, 7.5 and 10.0%) and two analytical instruments (electronic cryoscope and FTIR). The objective of this study was to evaluate the effect of these parameters in the determination of the freezing point by the reference method and by Fourier transform infrared spectroscopy, thus determining the best analytical conditions and establishing a mathematical equation for electronic determination by FTIR spectroscopy. Bronolat was the best preservative and Brononata was the worst and is not recommended to analyze freezing point by FTIR. The storage time of the samples did not interfere in the analytical determinations by the precision method and by FTIR.(AU)
Foram analisadas 480 amostras de leite em quatro repetições em relação a quatro tratamentos por conservantes (sem conservante, bronopol, bronolat e brononata), três tempos de armazenamento, em temperatura até 4ºC desde a recepção da amostra (24, 48 e 72 horas), cinco porcentagens de adição de água (0,0; 2,5; 5,0; 7,5 e 10,0%) e dois instrumentos analíticos (crioscópio eletrônico e FTIR). O objetivo foi avaliar o efeito desses parâmetros na determinação do índice crioscópico pelo método de precisão em crioscópio eletrônico e por espectroscopia com transformada de Fourier no infravermelho, determinando-se, assim, as melhores condições analíticas. Entre os conservantes utilizados, bronolat foi o melhor e brononata foi o menos eficiente, não sendo, portanto, recomendado para análise de crioscopia por FTIR. O tempo de armazenamento das amostras não interferiu nas determinações analíticas pelo método de precisão e por FTIR.(AU)
Asunto(s)
Leche/química , Alimentos Crudos/análisis , Conservantes de Alimentos , Congelación , Alimentos Congelados/análisis , Espectroscopía Infrarroja por Transformada de FourierRESUMEN
The objective of this study was to evaluate the CombiScope FTIR equipment based on Fourier Transform Infrared methodology (FTIR), to assess the content of milk urea nitrogen (MUN) in Brazil. Repeatability and reproducibility of CombiScopeTM FTIR (Delta Instruments), and comparison with an enzymatic automated method (Chemspec® 150; Bentley Instruments) were tested to measure raw milk urea nitrogen (MUN). Additionally, MUN levels stability after storage of raw milk samples at 4ºC, and 20ºC for up to 15 days, and capability and precision to detect extraneous urea added as an adulterant to the milk were evaluated by FTIR equipment. There was a high correlation coefficient for the analysis of MUN by FTIR equipment, when compared with the automated enzymatic method, with no significant difference between both. MUN concentration in raw milk remained stable at temperatures of 4ºC for up to 15 days of storage, but after 3 days of storage at 20ºC there was an increase in the MUN levels. The CombiScope FTIR equipment proved to be a reliable method for analysis of MUN content in raw milk. However, results for MUN were not linear with the amount of extraneous urea added to raw milk, having a significant difference for samples when 40mg/dL of urea was added to milk.
O objetivo deste estudo foi realizar a avaliação do CombiScopeTM FTIR (Delta Instruments), um equipamento baseado na espectroscopia de infravermelho por metodologia em Transformada Fourier (FTIR) para a avaliação do teor de nitrogênio uréico no leite (NUL) cru produzido no Brasil. A repetibilidade e reprodutibilidade do CombiScopeTM FTIR (Delta Instruments) e a comparação com um método enzimático automatizado (ChemSpec® 150; Bentley Instruments) foram testados para a medição do nitrogênio uréico no leite (NUL) cru. Adicionalmente, os níveis de NUL após armazenamento das amostras de leite a 4ºC e 20ºC por até 15 dias, e a capacidade e precisão para detectar uréia adicionada de forma fraudulenta ao leite foram avaliados por FTIR. Houve alta correlação entre os métodos FTIR e enzimático automatizado para a análise de uréia, sem diferença significativa entre ambos (p>0,05). A concentração de uréia no leite cru manteve-se estável durante o armazenamento das amostras a 4ºC por até 15 dias. No entanto, após três dias à temperatura de 20ºC houve um aumento nos níveis de uréia. Os resultados obtidos evidenciam que o equipamento CombiScopeTM FTIR é um método confiável para a análise do teor de uréia no leite cru. Entretanto, a detecção de uréia adicionada de forma fraudulenta ao leite cru não foi linearmente proporcional, com diferença significativa para adição de uréia em níveis de 40mg/dL.
Asunto(s)
Espectroscopía Infrarroja por Transformada de Fourier/métodos , Leche/metabolismo , Nitrógeno/análisis , UreaRESUMEN
Four lignin samples were extracted from sugar cane bagasse using four different alcohols (methanol, ethanol, n-propanol, and 1-butanol) via the organosolv-CO2 supercritical pulping process. Langmuir films were characterized by surface pressure vs mean molecular area (Pi-A) isotherms to exploit information at the molecular level carrying out stability tests, cycles of compression/expansion (hysteresis), subphase temperature variations, and metallic ions dissolved into the water subphase at different concentrations. Briefly, it was observed that these lignins are relatively stable on the water surface when compared to those obtained via different extraction processes. Besides, the Pi-A isotherms are shifted to smaller molecular areas at higher subphase temperatures and to larger molecular areas when the metallic ions are dissolved into the subphase. The results are related to the formation of stable aggregates (domains) onto the water subphase by these lignins, as shown in the Pi-A isotherms. It was found as well that the most stable lignin monolayer onto the water subphase is that extracted with 1-butanol. Homogeneous Langmuir-Blodgett (LB) films of this lignin could be produced as confirmed by UV-vis absorption spectroscopy and the cumulative transfer parameter. In addition, FTIR analysis showed that this lignin LB film is structured in a way that the phenyl groups are organized preferentially parallel to the substrate surface. Further, these LB films were deposited onto gold interdigitated electrodes and ITO and applied in studies involving the detection of Cd+2 ions in aqueous solutions at low concentration levels through impedance spectroscopy and electrochemical measurements. FTIR spectroscopy was carried out before and after soaking the thin films into Cd+2 aqueous solutions, revealing a possible physical interaction between the lignin phenyl groups and the heavy metal ions. The importance of using nanostructured systems is demonstrated as well by comparing both LB and cast films.