Whey protein supplement adulteration with rice flour quantification: A simple method using ATR-FT-MIR and iPLS




Palabras clave:

Fourier-transform mid infrared spectroscopy, interval partial least squared regression, whey protein supplement, adulteration, rice flour


In this work, a method using ATR-FT-MIR and iPLS was developed to quantify whey protein supplement adulteration with rice flour. The original vanilla flavor commercial whey protein samples were adulterated with commercial rice flour with concentrations between 11.49% to 29.14% (w/w). After the adulteration, the ATR-FT-MIR spectra were obtained with no additional preparation procedure. The iPLS model analysis was performed using RStudio software with the mdatools package. The RMSEC was 1.26, the R2= 0.954 and the cross-validation error (RMSECV) was 3.31. The prediction error (RMSEP) for the validation set was equal 3.48 and the validation R2 was 0.610. These parameters, associated with the fact that the method does not require sample preparation, demonstrate the procedure viability as a tool to quantify adulterations of whey protein with rice flour.


Andrade, J., Pereira, C. G., Almeida, J. C., Viana, C. C. R., Neves, L. N. de O., et al. (2019). FTIR-ATR determination of protein content to evaluate whey protein concentrate adulteration. LWT, 99(September 2018), 166–172.

Czepielewska, E., Makarewicz-Wujec, M., Różewski, F., Wojtasik, E., & Kozłowska-Wojciechowska, M. (2018). Drug adulteration of food supplements: A threat to public health in the European Union? Regulatory Toxicology and Pharmacology, 97(October 2017), 98–102.

Garrido, B. C., Souza, G. H. M. F., Lourenço, D. C., & Fasciotti, M. (2016). Proteomics in quality control: Whey protein-based supplements. Journal of Proteomics, 147, 48–55.

Gorla, G., Mestres, M., Boqué, R., Riu, J., Spanu, D., & Giussani, B. (2020). ATR-MIR spectroscopy to predict commercial milk major components: A comparison between a handheld and a benchtop instrument. Chemometrics and Intelligent Laboratory Systems, 200(October 2019).

Jamwal, R., Amit, Kumari, S., Sharma, S., Kelly, S., Cannavan, A., & Singh, D. K. (2021). Recent trends in the use of FTIR spectroscopy integrated with chemometrics for the detection of edible oil adulteration. Vibrational Spectroscopy, 113(January), 103222.

Kucheryavskiy, S. (2020). mdatools – R package for chemometrics. Chemometrics and Intelligent Laboratory Systems, 198(January), 103937.

Lohumi, S., Lee, S., Lee, H., & Cho, B. K. (2015). A review of vibrational spectroscopic techniques for the detection of food authenticity and adulteration. Trends in Food Science and Technology, 46(1), 85–98.

Lukacs, M., Bazar, G., Pollner, B., Henn, R., Kirchler, C. G., Huck, C. W., & Kovacs, Z. (2018). Near infrared spectroscopy as an alternative quick method for simultaneous detection of multiple adulterants in whey protein-based sports supplement. Food Control, 94(April), 331–340.

Nespeca, M. G., Pavini, W. D., & de Oliveira, J. E. (2019). Multivariate filters combined with interval partial least square method: A strategy for optimizing PLS models developed with near infrared data of multicomponent solutions. Vibrational Spectroscopy, 102(January), 97–102.

Pavia, D.L., Lampman, G. M., Kriz, G. S., & Vyvyan, J. R. (2010). Introdução à Espectroscopia (4a). CENGAGE.

Pereira, C. G., Andrade, J., Ranquine, T., de Moura, I. N., da Rocha, R. A., Furtado, M. A. M., … Anjos, V. (2018). Characterization and detection of adulterated whey protein supplements using stationary and time-resolved fluorescence spectroscopy. LWT, 97(May), 180–186.

Rohman, A., & Che Man, Y. B. (2011). The use of Fourier transform mid infrared (FT-MIR) spectroscopy for detection and quantification of adulteration in virgin coconut oil. Food Chemistry, 129(2), 583–588.

Stöbener, A., Naefken, U., Kleber, J., & Liese, A. (2019). Determination of trace amounts with ATR FTIR spectroscopy and chemometrics: 5-(hydroxymethyl)furfural in honey. Talanta, 204(May), 1–5.

Tondi, G., & Petutschnigg, A. (2015). Middle infrared (ATR FT-MIR) characterization of industrial tannin extracts. Industrial Crops and Products, 65, 422–428.

Wang, H., Gu, J., Wang, S., & Saporta, G. (2019). Spacial Partial least Squares autoregression: Algorithm and Aplications. Chemometrics and Intelligent Laboratory Systems, 184, 123–131.

Yang, J., Yin, C., Miao, X., Meng, X., Liu, Z., & Hu, L. (2021). Rapid discrimination of adulteration in Radix Astragali combining diffuse reflectance mid-infrared Fourier transform spectroscopy with chemometrics. Spectrochimica Acta - Part A: Molecular and Biomolecular Spectroscopy, 248, 119251.

Zhang, X., Yang, J., Lin, T., & Ying, Y. (2021). Food and agro-product quality evaluation based on spectroscopy and deep learning: A review. Trends in Food Science and Technology, 112(April), 431–441.



Cómo citar

Braga, S. C. G. N. ., Braga, F. L. ., Boschetti, A. de F. ., Gerardth, L. F. F. ., da Rocha, M. A. C. ., & Cecatto, L. . (2021). Whey protein supplement adulteration with rice flour quantification: A simple method using ATR-FT-MIR and iPLS. Scientia Agropecuaria, 12(3), 379-383. https://doi.org/10.17268/sci.agropecu.2021.041



Artículos originales