Comparison of Multiple NIR Spectrometers for Detecting Low-Concentration Nitrogen-Based Adulteration in Protein Powders.

Protein adulteration is a common fraud in the food industry due to the high price of protein sources and their limited availability. Total nitrogen determination is the standard analytical technique for quality control, which is incapable of distinguishing between protein nitrogen and nitrogen from non-protein sources. Three benchtops and one handheld near-infrared spectrometer (NIRS) with different signal processing techniques (grating, Fourier transform, and MEM-micro-electro-mechanical system) were compared with detect adulteration in protein powders at low concentration levels. Whey, beef, and pea protein powders were mixed with a different combination and concentration of high nitrogen content compounds-namely melamine, urea, taurine, and glycine-resulting in a total of 819 samples. NIRS, combined with chemometric tools and various spectral preprocessing techniques, was used to predict adulterant concentrations, while the limit of detection (LOD) and limit of quantification (LOQ) were also assessed to further evaluate instrument performance. Out of all devices and measurement methods compared, the most accurate predictive models were built based on the dataset acquired with a grating benchtop spectrophotometer, reaching R2P values of 0.96 and proximating the 0.1% LOD for melamine and urea. Results imply the possibility of using NIRS combined with chemometrics as a generalized quality control tool for protein powders.

Detecting Low Concentrations of Nitrogen-Based Adulterants in Whey Protein Powder Using Benchtop and Handheld NIR Spectrometers and the Feasibility of Scanning through Plastic Bag.

Nitrogen-rich adulterants in protein powders present sensitivity challenges to conventional combustion methods of protein determination which can be overcome by near Infrared spectroscopy (NIRS). NIRS is a rapid analytical method with high sensitivity and non-invasive advantages. This study developed robust models using benchtop and handheld spectrometers to predict low concentrations of urea, glycine, taurine, and melamine in whey protein powder (WPP). Effectiveness of scanning samples through optical glass and polyethylene bags was also tested for the handheld NIRS. WPP was adulterated up to six concentration levels from 0.5% to 3% w/w. The two spectrometers were used to obtain three datasets of 819 diffuse reflectance spectra each that were pretreated before linear discriminant analysis (LDA) and regression (PLSR). Pretreatment was effective and revealed important absorption bands that could be correlated with the chemical properties of the mixtures. Benchtop NIR spectrometer showed the best results in LDA and PLSR but handheld NIR spectrometers showed comparatively good results. There were high prediction accuracies and low errors attesting to the robustness of the developed PLSR models using independent test set validation. Both the plastic bag and optical glass gave good results with accuracies depending on the adulterant of interest and can be used for field applications.