RESUMOEste trabalho se propôs a desenvolver um modelo preditivo para identificação de perda de estabilidade e de sedimentação em leite UAT por determinação da atividade enzimática de aminopeptidase no leite por espectrofotometria. Foram analisadas amostras de leite cru, pasteurizado e UAT após envase durante seis meses, na região Sul do Brasil. Acidez, crioscopia, gordura, extrato seco total, extrato seco desengordurado e densidade foram analisados nos leites cru e pasteurizado. Amostras de leite cru foram ainda submetidas à análise de contagem de psicrotróficos e à atividade de aminopeptidase, e amostras de leite UAT estocadas foram analisadas quanto ao grau de proteólise mediante análises sensoriais e atividade de aminopeptidase. Alterações sensoriais foram observadas em tempos de estocagem menores para amostras originadas de leite cru com contagem de psicrotróficos acima de 10 7 UFC mL -1. Não houve correlação entre a atividade de aminopeptidase e proteólise e também não foi observada correlação significativa entre os parâmetros físico-químicos e a ocorrência de proteólise no leite estocado. O modelo estudado não foi apto para predizer perda de estabilidade e ocorrência de proteólise no leite UAT.

A multi-residue method for the determination of the β-lactam antibiotics ampicillin, cefazolin, cloxacillin, dicloxacillin, nafcillin, oxacillin, penicillin G, penicillin V and the tetracyclines chlotetracycline, tetracycline and oxytetracycline was optimised and validated in bovine muscle. The method is based on the extraction of the residues from muscle using water/acetonitrile (2/8, v/v) with subsequent use of dispersive solid-phase C18 and hexane for purification. Extracts were analysed using ultra-performance liquid chromatography (UPLC-MS/MS) coupled with the mass spectrometer in positive electrospray ionisation mode (ESI+) for all analytes. The method was validated according to the requirements of European Commission Decision 2002/657/EC. The validation results were obtained within the MRL range of 0-1.5 of the MRL, with recoveries varying from 90% to 110% and CV < 20% (n = 54), except for cloxacillin, dicloxacillin and nafcillin. However, matrix interference was observed. The decision limit (CCα) ranged from 10% to 15% of the MRL. The uncertainty measurement was estimated based on both bottom-up and top-down strategies and the uncertainty values were found to be lower than 20% of the MRL. The method has a simple extraction procedure whereby analytes are separated with reasonable resolutions in a single 11-min chromatographic run. According to the validation results, this method is suitable for monitoring β-lactams and tetracyclines according to National Program for Residue and Contaminant Control - Brazil (NPRC-Brazil) in bovine muscle.

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.

The present study attempted to identify climate conditions that are associated with the occurrence of pyrethroid residues using a multivariate principal component analysis (PCA). A total of 132 raw milk samples were collected from dairy farms in Minas Gerais State -Brazil and analyzed for seven analytes using gas chromatography with electron capture detection. Of the 132 milk samples, pyrethroid residues were identified in 14 (10.6%) milk samples, of which 12 (9.1%) and two (1.5%) milk samples had the identification of cypermethrin and deltamethrin, respectively. From those samples, nine (6.8%) milk samples were regarded as non-compliant for cypermethrin with this analyte concentration above the maximum residue limits set by Brazilian legislation. A PCA assessing pyrethroid residues in bulk tank milk demonstrated that the average temperature and the Temperature-Humidity Index were associated with pyrethroids residues in bulk milk tank, although the relative humidity was inversely correlated. Thus, the data analysis indicated that the pyrethrid residues associated with some climate conditions can predict the moments with higher risk of occurrence of pyrethroid residues in bulk tank milk.Keywords: veterinary drug, pesticide, raw milk, seasonality, dairy cow Palavras-chaves: medicamento veterinário, pesticida, leite cru, sazonalidade, bovino leiteiro RESUMO O presente trabalho objetivou identificar fatores climáticos associados à ocorrência de resíduos de piretroides em amostras de leite de tanque por análise multivariada de componentes principais (ACP). Para o presente trabalho, 132 amostras de leite cru foram coletadas em fazendas leiteiras localizadas no estado de Minas Gerais (Brasil

Influência de diferentes tipos de micro-organismos na contagem bacteriana total por citometria de fluxo do leite cru refrigeradoHouve uma forte correlação positiva e significativa entre os valores de contagem de psicrotróficos (r = 0,67) e mesófilos (r = 0,70), determinados pelo método de referência, e os valores da contagem bacteriana total, determinados pela citometria de fluxo. Foi possível estabelecer uma curva de calibração para o citômetro de fluxo utilizando equações de regressão linear. As equações para a contagem bacteriana obtida por citometria de fluxo em função da contagem de mesófilos e psicrotróficos foram: log (CBI) = 0,701 log mesófilos + 1,9091 e log (CBI) = 0,4703 log psicrotróficos + 3,2784, respectivamente. Não foi possível estabelecer curvas de calibrações para termófilos e termodúricos, pois as correlações obtidas entre as contagens desses microorganismos e a contagem bacteriana total, determinada por citometria de fluxo, foram fracas (r = 0,30 e 0,27, respectivamente).Palavras-chave: leite de tanque, qualidade de leite, leite ABSTRACT Total Bacterial count was performed in 179 raw milk samples from different dairy farms in Minas Gerais

The influence of seasonality and the training and implementation of good dairy farming practices on raw milk production and quality was evaluated on dairy farms in Minas Gerais State, Brazil. The physico-chemical composition, somatic cell count (SCC) and total bacterial count (TBC) were determined in 3,096 milk samples collected from bulk tanks originated from 43 dairy farms over a three-year period and correlated with key climatic factors. The recommended milking management practices were applied through a training program and correlated with the seasonal data in three stages: I) prior to training (dry period); II) 48 days after the training (transition period); III) 96 days after the training (rainy period). In the first stage, a diagnosis of the situation was performed with raw milk samplings for laboratory analysis, and training for implementation of good milking practices. In stages II and II, the checklist and laboratory analysis were also performed. The rainfall and high temperatures were found to represent the main factors affecting the milk composition and production, and TBC. The composition and physical properties of raw milk, and the TBC and SCC parameters can be controlled or minimized by applying proper milking management practices and constant monitoring.

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 CombiScope™ 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 4°C, and 20°C 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 4°C for up to 15 days of storage, but after 3 days of storage at 20°C 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.Keywords: milk, validation, milk urea nitrogen, infrared spectroscopy, FTIR Palavras-chave: leite, validação, nitrogênio uréico no leite, espectroscopia no infravermelho, FTIR RESUMO O objetivo deste estudo foi realizar a avaliação do CombiScope™ 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

High performance liquid chromatography was used in order to detect cheese whey in samples of raw milk preserved with Bronopol ® . Six samples were collected and divided in 45 aliquots of 40mL. From these, 15 were used as control and stored frozen, 15 were added with Bronopol ® and stored at 7ºC, and the other 15 were added with Bronopol ® and stored at 30ºC. In all groups, five levels of cheese whey addition (0, 2, 5, 10, and 20%) were tested. The samples were submitted to high performance liquid chromatography on the 2 nd , 4 th , and 8 th days of storage. A completely random design was used, following the factorial scheme (5x3x3) and the results were compared through the non-parametric Kruskal-Wallis test. There was no difference among the treatments (P>0.05), which allows the conclusion that raw milk preserved with Bronopol ® may be used for the determination of cheese whey addition in milk through high performance liquid chromatography.