Fourier-transformed infrared (FTIR) spectroscopy for detecting milk powder addition in Cyprus goat milk: a preliminary study for future adulteration detection in halloumi cheese
Main Article Content
Keywords
adulteration, chemometrics, FTIR spectroscopy, milk powder
Abstract
This study was about the adulteration of milk with milk powder and serves as a precursor for future studies on halloumi cheese adulteration with milk powder. Three different commercial milk powders of different geographic origins were tested to check the impact of milk powder origin versus the amount of milk powder added in milk as an adulterant. Three different concentrations of skim milk powder (SMP) were added (0.5%, 1%, and 3%) to Cyprus goat milk, and the mixtures were then heated to 90°C (a crucial step in halloumi cheese preparation). Fourier-transformed infrared (FTIR) spectra were collected after freeze-drying, and Partial Least Squares Discriminant Analysis, a supervised classification method, was applied in terms of chemometrics to test the classification of samples. The adulterated milk samples of this study are used in halloumi cheese making to check after cooking the discrimination of adulterated halloumi cheese at low percentage of adulteration with SMP by applying FTIR and chemometrics in future. Based on the present study, the origin of milk powder is not significant, and it is assumed that generally, for future studies the origin of milk powder will not affect sample classification.
References
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Arsenos, G., Vouraki, S., Ragkos, A., Theodoridis, A. 2021. Trends and Challenges for Sustainable Development of Sheep and Goat Systems. In Pastoralism and Sustainable Development, Book of Abstracts; Capone, R., Bottalico, F., El Bilali, H., Ottomano Palsimano, G., Cardone, G., Acquafredda, A., eds.; CIHEAM: Bari, Italy, 2021; p. 10.
Capici, C., Mimmo, T., Kerschbaumer, L., Cesco, S., and Scampicchio, M. 2015. Determination of cheese-authenticity by carbon and nitrogen isotope analysis: stelvio cheese as a case study. Food Analytical Methods 8: 2157–2162. 10.1007/s12161-015-0113-y
Cruz, J., Gergov, G., Tarapoulouzi, M., Kirilova, E., Kostadinova, O., and Nikolova, K. 2024. Classification of apple varieties by VIS-NIR diffuse reflectance spectroscopy and chemometrics. Bulgarian Chemical Communications 56, 106.
De Girolamo, A., Arroyo, M.C., Cervellieri, S., Cortese, M., Pascale, M., Logrieco, A.F., and Lippolis, V. 2020. Detection of durum wheat pasta adulteration with common wheat by infrared spectroscopy and chemometrics: a case study. Food Science and Technology (LWT) 127: 109368. 10.1016/j.lwt.2020.109368
de Oliveira, L.V.A., Kleemann, C.R., Molognoni, L., Daguer, H., Hoff, R.B., and Prudencio, E.S. 2022. Reference LC-MS/MS method to detect fresh cheeses adulteration with whey. Food Research International 156: 111140. 10.1016/j.foodres.2022.111140
Du, L. 2024. New insights into raw milk adulterated with milk-powder identification: ATR-FTIR spectroscopic fingerprints combined with machine learning and feature selection approaches. Journal of Food Composition and Analysis 133: 106443. 10.1016/j.jfca.2024.106443
European Commission. 2021. European Commission registers Χαλλούμι/halloumi/hellim as a protected designation of -origin (PDO). Available at: https://ec.europa.eu/-commission/-presscorner/detail/en/ip_21_1623 (Accessed: 20 January 2026).
Genis, D.O., Sezer, B., Durna, S., and Boyaci, I.H. 2021. Determination of milk fat authenticity in ultra-filtered white cheese by using Raman spectroscopy with multivariate data analysis. Food Chemistry 336: 127699. 10.1016/j.foodchem.2020.127699
Ionescu, A.D., Cîrîc, A.I., and Begea, M. 2023. A review of milk frauds and adulterations from a technological perspective. Applied Sciences 13(17): 9821. 10.3390/app13179821
Karaziack, C.B., Vidal, C., Pasquini, C., Barbin, D.F., and Viotto, W.H. 2024. Application of near-infrared hyperspectral imaging for determination of cheese chemical composition. Journal of Food Composition and Analysis 127: 105994. 10.1016/j.jfca.2024.105994
Kharbach, M., Alaoui Mansouri, M., Taabouz, M., and Yu, H. 2023. Current application of advancing spectroscopy techniques in food analysis: data handling with chemometric approaches. Foods 12(14): 2753. 10.3390/foods12142753
Kováčová, M., Výrostková, J., Dudriková, E., Zigo, F., Semjon, B., and Regecová, I. 2021. Assessment of quality and safety of farm level produced cheeses from sheep and goat milk. Applied Sciences 11(7): 3196. 10.3390/app11073196
Kritikou, A.S., Aalizadeh, R., Damalas, D.E., Barla, I.V., Baessmann, C., and Thomaidis, N.S. 2022. MALDI-TOF-MS integrated workflow for food authenticity investigations: an untargeted protein-based approach for rapid detection of PDO feta cheese adulteration. Food Chemistry 370: 131057. 10.1016/j.foodchem.2021.131057
Li, S., Delger, M., Dave, A., Singh, H., and Ye, A. 2022. Seasonal variations in the composition and physicochemical characteristics of sheep and goat milks. Foods 11(12): 1737. 10.3390/foods11121737
Maritano, V., Barge, P., Biglia, A., Comba, L., Aimonino, D.R., Tortia, C., and Gay, P. 2024. Anti-counterfeiting and fraud mitigation solutions for high-value food products. Journal of Food Protection 87(4): 100251. 10.1016/j.jfp.2024.100251
Nayik, G.A., Jagdale, Y.D., Gaikwad, S.A., Devkatte, A.N., Dar, A.H., and Ansari, M.J. 2022. Nutritional profile, processing and potential products: a comparative review of goat milk. Dairy 3(3): 622–647. 10.3390/dairy3030044
Oliveri, P., Malegori, C., and Casale, M. 2020. Chemometrics: multivariate analysis of chemical data. In: Chemical Analysis of Food, 2nd ed; Pico Y. Academic Press, New York, NY, pp. 33–76. 10.1016/B978-0-12-813266-1.00002-4
Papademas, P., and Robinson, R.K. 1998. Halloumi cheese: the product and its characteristics. International Journal of Dairy Technology 51(3): 98–103. 10.1111/j.1471-0307.1998.tb02646.x
Pinto, S., Rathour, A.K., Prajapati, J.P., Jana, A.H., and Solanky, M.J. 2007. Utilization of whey protein concentrate in processed cheese spread. Natural Product Radiance, 6(5): 398–401.
Ray C.L., Gawenis, J.A., Bylo, M.P., Pescaglia, J., and Greenlief, C.M. 2023. Detection of vegetable oil adulteration in pre-grated bovine hard cheeses via 1H NMR Spectroscopy. Molecules 28(3): 920. 10.3390/molecules28030920
Saad, A.H., Salama, E., Sweedy, M.Y., and Abd Algwad, A. 2023. Fatty acid analysis of soft cheese using gas chromatography as a prospective method for the detection of cheese adulterations with vegetable oil. Journal of Advanced Veterinary Research 13(6): 1011–1016.
Siddiqui, S.A., Salman, S.H.M., Redha, A.A., Zannou, O., Chabi, I.B., Oussou, K.F., Bhowmik, S., Nirmal, N.P., and Maqsood, S. 2024. Physicochemical and nutritional properties of different non--bovine milk and dairy products: a review. International Dairy Journal 148: 105790. 10.1016/j.idairyj.2023.105790
Smaoui, S., Tarapoulouzi, M., Agriopoulou, S., D’Amore, T., and Varzakas, T. 2023. Current state of milk, dairy products, meat and meat products, eggs, fish and fishery products authentication and chemometrics. Foods 12(23): 4254. 10.3390/foods12234254
Tarapoulouzi, M., Agriopoulou, S., Artemi, A. (2024). Quality Schemes and Geographical Indicators in the Cheese Agribusiness and the Case of the Cypriot Traditional Cheese Halloumi. In: Galati, A., Fiore, M., Thrassou, A., Vrontis, D. (eds) Agribusiness Innovation and Contextual Evolution, Volume I. Palgrave Intersections of Business and the Sciences, in association with Gnosis Mediterranean Institute for Management Science. Palgrave Macmillan, Cham, Switzerland, pp. 155–182. 10.1007/978-3-031-45738-8_7
Tarapoulouzi, M., Entrenas, J.A., Pérez-Marín, D., Pashalidis, I., and Theocharis, C.R. 2024b. A preliminary study on determining seasonal variations in halloumi cheese using near-infrared spectroscopy and chemometrics. Processes 12(7): 1517. 10.3390/pr12071517
Tarapoulouzi, M., Kokkinofta, R., and Theocharis, C.R. 2020. Chemometric analysis combined with FTIR spectroscopy of milk and halloumi cheese samples according to species’ origin. Food Science & Nutrition 8(7): 3262–3273. 10.1002/fsn3.1603
Tarapoulouzi, M., Logan, N., Hardy, M., Montgomery, H., Haughey, S.A., Elliott, C.T., and Theocharis, C.R. 2024c. A pre-trial study to identify species of origin in halloumi cheese utilising chemometrics with near-infrared and hyperspectral imaging technologies. Analytica 5(1): 17–27. 10.3390/analytica5010002
Tarapoulouzi, M., and Theocharis, C.R. 2022. Discrimination of Cheddar, Kefalotyri, and Halloumi cheese samples by the chemometric analysis of Fourier transform infrared spectroscopy and proton nuclear magnetic resonance spectra. Journal of Food Process Engineering 45(7): e13933. 10.1111/jfpe.13933
Tarapoulouzi, M., and Theocharis, C.R. 2023. Discrimination of Anari cheese samples in comparison with halloumi cheese samples regarding the origin of the species by FTIR measurements and chemometrics. Analytica 4(3): 374–384. 10.3390/analytica4030027
Tsagkaris, A.S., Kalogiouri, N., Hrbek, V., and Hajslova, J. 2023. Spelt authenticity assessment using a rapid and simple Fourier transform infrared spectroscopy (FTIR) method combined to advanced chemometrics. European Food Research and Technology 249(2): 441–450. 10.1007/s00217-022-04128-2
Visconti, L.G., Diniz, P.H.G.D., de Sousa Fernandes, D.D., Rodriguez, M.S., and Di Anibal, C.V. 2024. Authentication of grated hard cheeses and quantification of adulteration by FT-NIR spectroscopy and multivariate analysis. International Dairy Journal 158: 106035. 10.1016/j.idairyj.2024.106035
Wang, L., Han, M., Li, X., Zhang, N., and Cheng, H. 2021. Review of classification methods on unbalanced data sets. IEEE Access 9: 64606–64628. 10.1109/ACCESS.2021.3074243
Alsaleem, K.A., Hamouda, M.E., Alayouni, R.R., Elfaruk, M.S., and Hammam, A.R. 2023. Effect of skim milk powder and whey protein concentrate addition on the manufacture of probiotic Mozzarella cheese. Fermentation 9(11): 948. 10.3390/fermentation9110948
Arsenos, G., Vouraki, S., Ragkos, A., Theodoridis, A. 2021. Trends and Challenges for Sustainable Development of Sheep and Goat Systems. In Pastoralism and Sustainable Development, Book of Abstracts; Capone, R., Bottalico, F., El Bilali, H., Ottomano Palsimano, G., Cardone, G., Acquafredda, A., eds.; CIHEAM: Bari, Italy, 2021; p. 10.
Capici, C., Mimmo, T., Kerschbaumer, L., Cesco, S., and Scampicchio, M. 2015. Determination of cheese-authenticity by carbon and nitrogen isotope analysis: stelvio cheese as a case study. Food Analytical Methods 8: 2157–2162. 10.1007/s12161-015-0113-y
Cruz, J., Gergov, G., Tarapoulouzi, M., Kirilova, E., Kostadinova, O., and Nikolova, K. 2024. Classification of apple varieties by VIS-NIR diffuse reflectance spectroscopy and chemometrics. Bulgarian Chemical Communications 56, 106.
De Girolamo, A., Arroyo, M.C., Cervellieri, S., Cortese, M., Pascale, M., Logrieco, A.F., and Lippolis, V. 2020. Detection of durum wheat pasta adulteration with common wheat by infrared spectroscopy and chemometrics: a case study. Food Science and Technology (LWT) 127: 109368. 10.1016/j.lwt.2020.109368
de Oliveira, L.V.A., Kleemann, C.R., Molognoni, L., Daguer, H., Hoff, R.B., and Prudencio, E.S. 2022. Reference LC-MS/MS method to detect fresh cheeses adulteration with whey. Food Research International 156: 111140. 10.1016/j.foodres.2022.111140
Du, L. 2024. New insights into raw milk adulterated with milk-powder identification: ATR-FTIR spectroscopic fingerprints combined with machine learning and feature selection approaches. Journal of Food Composition and Analysis 133: 106443. 10.1016/j.jfca.2024.106443
European Commission. 2021. European Commission registers Χαλλούμι/halloumi/hellim as a protected designation of -origin (PDO). Available at: https://ec.europa.eu/-commission/-presscorner/detail/en/ip_21_1623 (Accessed: 20 January 2026).
Genis, D.O., Sezer, B., Durna, S., and Boyaci, I.H. 2021. Determination of milk fat authenticity in ultra-filtered white cheese by using Raman spectroscopy with multivariate data analysis. Food Chemistry 336: 127699. 10.1016/j.foodchem.2020.127699
Ionescu, A.D., Cîrîc, A.I., and Begea, M. 2023. A review of milk frauds and adulterations from a technological perspective. Applied Sciences 13(17): 9821. 10.3390/app13179821
Karaziack, C.B., Vidal, C., Pasquini, C., Barbin, D.F., and Viotto, W.H. 2024. Application of near-infrared hyperspectral imaging for determination of cheese chemical composition. Journal of Food Composition and Analysis 127: 105994. 10.1016/j.jfca.2024.105994
Kharbach, M., Alaoui Mansouri, M., Taabouz, M., and Yu, H. 2023. Current application of advancing spectroscopy techniques in food analysis: data handling with chemometric approaches. Foods 12(14): 2753. 10.3390/foods12142753
Kováčová, M., Výrostková, J., Dudriková, E., Zigo, F., Semjon, B., and Regecová, I. 2021. Assessment of quality and safety of farm level produced cheeses from sheep and goat milk. Applied Sciences 11(7): 3196. 10.3390/app11073196
Kritikou, A.S., Aalizadeh, R., Damalas, D.E., Barla, I.V., Baessmann, C., and Thomaidis, N.S. 2022. MALDI-TOF-MS integrated workflow for food authenticity investigations: an untargeted protein-based approach for rapid detection of PDO feta cheese adulteration. Food Chemistry 370: 131057. 10.1016/j.foodchem.2021.131057
Li, S., Delger, M., Dave, A., Singh, H., and Ye, A. 2022. Seasonal variations in the composition and physicochemical characteristics of sheep and goat milks. Foods 11(12): 1737. 10.3390/foods11121737
Maritano, V., Barge, P., Biglia, A., Comba, L., Aimonino, D.R., Tortia, C., and Gay, P. 2024. Anti-counterfeiting and fraud mitigation solutions for high-value food products. Journal of Food Protection 87(4): 100251. 10.1016/j.jfp.2024.100251
Nayik, G.A., Jagdale, Y.D., Gaikwad, S.A., Devkatte, A.N., Dar, A.H., and Ansari, M.J. 2022. Nutritional profile, processing and potential products: a comparative review of goat milk. Dairy 3(3): 622–647. 10.3390/dairy3030044
Oliveri, P., Malegori, C., and Casale, M. 2020. Chemometrics: multivariate analysis of chemical data. In: Chemical Analysis of Food, 2nd ed; Pico Y. Academic Press, New York, NY, pp. 33–76. 10.1016/B978-0-12-813266-1.00002-4
Papademas, P., and Robinson, R.K. 1998. Halloumi cheese: the product and its characteristics. International Journal of Dairy Technology 51(3): 98–103. 10.1111/j.1471-0307.1998.tb02646.x
Pinto, S., Rathour, A.K., Prajapati, J.P., Jana, A.H., and Solanky, M.J. 2007. Utilization of whey protein concentrate in processed cheese spread. Natural Product Radiance, 6(5): 398–401.
Ray C.L., Gawenis, J.A., Bylo, M.P., Pescaglia, J., and Greenlief, C.M. 2023. Detection of vegetable oil adulteration in pre-grated bovine hard cheeses via 1H NMR Spectroscopy. Molecules 28(3): 920. 10.3390/molecules28030920
Saad, A.H., Salama, E., Sweedy, M.Y., and Abd Algwad, A. 2023. Fatty acid analysis of soft cheese using gas chromatography as a prospective method for the detection of cheese adulterations with vegetable oil. Journal of Advanced Veterinary Research 13(6): 1011–1016.
Siddiqui, S.A., Salman, S.H.M., Redha, A.A., Zannou, O., Chabi, I.B., Oussou, K.F., Bhowmik, S., Nirmal, N.P., and Maqsood, S. 2024. Physicochemical and nutritional properties of different non--bovine milk and dairy products: a review. International Dairy Journal 148: 105790. 10.1016/j.idairyj.2023.105790
Smaoui, S., Tarapoulouzi, M., Agriopoulou, S., D’Amore, T., and Varzakas, T. 2023. Current state of milk, dairy products, meat and meat products, eggs, fish and fishery products authentication and chemometrics. Foods 12(23): 4254. 10.3390/foods12234254
Tarapoulouzi, M., Agriopoulou, S., Artemi, A. (2024). Quality Schemes and Geographical Indicators in the Cheese Agribusiness and the Case of the Cypriot Traditional Cheese Halloumi. In: Galati, A., Fiore, M., Thrassou, A., Vrontis, D. (eds) Agribusiness Innovation and Contextual Evolution, Volume I. Palgrave Intersections of Business and the Sciences, in association with Gnosis Mediterranean Institute for Management Science. Palgrave Macmillan, Cham, Switzerland, pp. 155–182. 10.1007/978-3-031-45738-8_7
Tarapoulouzi, M., Entrenas, J.A., Pérez-Marín, D., Pashalidis, I., and Theocharis, C.R. 2024b. A preliminary study on determining seasonal variations in halloumi cheese using near-infrared spectroscopy and chemometrics. Processes 12(7): 1517. 10.3390/pr12071517
Tarapoulouzi, M., Kokkinofta, R., and Theocharis, C.R. 2020. Chemometric analysis combined with FTIR spectroscopy of milk and halloumi cheese samples according to species’ origin. Food Science & Nutrition 8(7): 3262–3273. 10.1002/fsn3.1603
Tarapoulouzi, M., Logan, N., Hardy, M., Montgomery, H., Haughey, S.A., Elliott, C.T., and Theocharis, C.R. 2024c. A pre-trial study to identify species of origin in halloumi cheese utilising chemometrics with near-infrared and hyperspectral imaging technologies. Analytica 5(1): 17–27. 10.3390/analytica5010002
Tarapoulouzi, M., and Theocharis, C.R. 2022. Discrimination of Cheddar, Kefalotyri, and Halloumi cheese samples by the chemometric analysis of Fourier transform infrared spectroscopy and proton nuclear magnetic resonance spectra. Journal of Food Process Engineering 45(7): e13933. 10.1111/jfpe.13933
Tarapoulouzi, M., and Theocharis, C.R. 2023. Discrimination of Anari cheese samples in comparison with halloumi cheese samples regarding the origin of the species by FTIR measurements and chemometrics. Analytica 4(3): 374–384. 10.3390/analytica4030027
Tsagkaris, A.S., Kalogiouri, N., Hrbek, V., and Hajslova, J. 2023. Spelt authenticity assessment using a rapid and simple Fourier transform infrared spectroscopy (FTIR) method combined to advanced chemometrics. European Food Research and Technology 249(2): 441–450. 10.1007/s00217-022-04128-2
Visconti, L.G., Diniz, P.H.G.D., de Sousa Fernandes, D.D., Rodriguez, M.S., and Di Anibal, C.V. 2024. Authentication of grated hard cheeses and quantification of adulteration by FT-NIR spectroscopy and multivariate analysis. International Dairy Journal 158: 106035. 10.1016/j.idairyj.2024.106035
Wang, L., Han, M., Li, X., Zhang, N., and Cheng, H. 2021. Review of classification methods on unbalanced data sets. IEEE Access 9: 64606–64628. 10.1109/ACCESS.2021.3074243
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