Failures in milk coagulation during cheese manufacturing can lead to decreased yield, anomalous behaviour of cheese during storage, significant impact on cheese quality and process wastes. This study proposes a Process Analytical Technology approach based on FT-NIR spectroscopy for milk renneting control during cheese manufacturing. Multivariate Curve Resolution optimized by Alternating Least Squares (MCR-ALS) was used for data analysis and development of Multivariate Statistical Process Control (MSPC) charts. Fifteen renneting batches were set up varying temperature (30, 35, 40 °C), milk pH (6.3, 6.5, 6.7), and fat content (0.1, 2.55, 5 g/100 mL). Three failure batches were also considered. The MCR-ALS models well described the coagulation processes (explained variance ≥99.93%; lack of fit <0.63%; standard deviation of the residuals <0.0067). The three identified MCR-ALS profiles described the main renneting phases. Different shapes and timing of concentration profiles were related to changes in temperature, milk pH, and fat content. The innovative implementation of MSPC charts based on T2
and Q statistics allowed the detection of coagulation failures from the initial phases of the process.
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