Multicomponent Cleaning Verification of Stainless Steel Surfaces for the Removal of Dairy Residues Using Infrared Microspectroscopy



Abstract:  The application of infrared microspectroscopy (IRMS) technology, combined with multivariate analysis, was evaluated to develop sensitive and robust methods to assess cleanability of stainless steel surfaces for the removal of dairy food residues. UHT milk samples (skim, 1%, 2%, and whole) were analyzed for total nitrogen (Kjeldahl) and fat (Babcock) contents. The coupons were manually soiled with serially diluted milk samples resulting in soils ranging from 0.1 to 428.1 μg/cm2 for protein and 0.1 to 374.17 μg/cm2 for fat, and then autoclaved to simulate a heated equipment surface. Reflectance spectra were collected from stainless steel coupons by using IRMS, and multivariate analysis was used to develop calibration models based on cross-validated partial least squares regression (PLSR). Statistical analysis for the prediction of protein and fat showed a standard error of cross-validation (SECV) of 0.5 and 0.4 μg/cm2 for prediction of protein and fat, respectively, and correlation coefficients (rVal) > 0.99. To improve the sensitivity, swabbing and concentration steps were used prior to IRMS analysis obtaining SECV of 0.04 and 0.01 μg/cm2 for the prediction of protein and fat, respectively, and rVal > 0.99. The PLSR models accurately predicted the levels of protein and fat on autoclaved stainless steel coupons soiled with milk. A simple, reliable, and robust protocol based on IRMS and multivariate analysis was developed for multicomponent characterization of stainless steel surfaces that can contribute to more efficient cleaning verification with regard to contamination on surfaces of processing equipment.

Practical Application:  We report the application of Fourier transform infrared microspectroscopy (FTIR) for the validation of CIP cleaning efficiency that would provide a basis for better understanding of the mechanisms involved in the removal of physical soil and food residues from different types of equipment surfaces commonly utilized in the biotech, pharmaceutical, and food industries. Reliable calibration models were generated that showed the ability to predict the amounts of dairy soils on the surface of stainless steel coupons. Including a swabbing step of the coupons before infrared spectral acquisition provided improved sensitivity and reproducibility for multicomponent cleaning verification. Results from this research project would allow designing experiments to rapidly evaluate different materials and finishes, the effects of process variables, the influence of food components, and the development of reliable and robust cleaning validation protocols to ensure the safety and quality of the product.