Multivariable analytical method based on NIR spectroscopy and chemometric tools to differentiate between '100% agave' and 'mixed' white tequila

Authors

Keywords:

Quality Control, Authentication, Food Fraud, Chemometrics, Near Infrared Spectroscopy

Abstract

Tequila, one of Mexico's most representative spirits, is threatened by adulteration and counterfeiting practices that affect both consumers and the industry. The distinction between the categories of '100% agave' and 'mixed' white Tequila is crucial to guarantee its quality, cultural and commercial value. In this study, a multivariate analytical method based on near infrared spectroscopy (NIR) and chemometric tools is proposed to address this problem, using advanced mathematical models, including principal component analysis (PCA), partial least squares regression (PLSR), k-nearest neighbors (kNN), partial least squares regression discriminant analysis (PLS-DA), soft independent modeling of class analogy (SIMCA) and support vector machine learning (SVM). Results show that the SVM and PLS-DA models achieved perfect classifications (sensitivity, specificity and precision = 1), evidencing their effectiveness in the authentication of Tequila categories. Additionally, the SVMR regression model demonstrated outstanding performance in predicting alcohol content, with a coefficient of determination (R²) of 1.0. This approach offers an efficient, fast and non-destructive alternative to traditional quality control methods such as chromatography. Its implementation in the tequila industry and routine laboratories can significantly improve fraud detection and guarantee product authenticity. This study highlights the potential of NIR spectroscopy and chemometrics as key tools to strengthen quality control in the spirits industry.

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Author Biographies

  • Pérez-Beltrán C.H., Faculty of Chemical Biological Sciences. UAS

    He is a Professor/Researcher at the Autonomous University of Sinaloa and holds a Ph.D. in Chemistry from the University of Granada, Spain. He is a member of the National System of Researchers (SNII) at the Candidate level and of the SSIT as an Honorary Researcher. He has published six articles in indexed journals and one in peer-reviewed journals, achieving a total of 64 citations and an h-index of 5 to date. He has participated in five national and international conferences. Throughout his career, he has conducted research related to the detection of food fraud using green analytical methods coupled with chemometric tools, as well as the use of chemometrics for the detection of cardiac and ocular diseases. Contact email: chperezb@uas.edu.mx

  • León-López L., Faculty of Chemical Biological Sciences, UAS

    She is a Professor/Researcher at the Autonomous University of Sinaloa and holds a Ph.D. in Food Science from the National Polytechnic Institute. She is a member of the National System of Researchers (SNII) at Level 1, an Honorary Researcher of the SSIT, and holds a PRODEP Profile. She has published 12 articles in indexed journals and 2 in peer-reviewed journals, achieving a total of 241 citations and an h-index of 6 to date. She has participated in 25 national and international conferences. Throughout her career, she has supervised 6 undergraduate theses and 3 master's theses in the fields of Agro-Food Biotechnology, Functional Foods, and Active Biomolecules of Agro-Food Interest. Contact email: lili.leon@uas.edu.mx

  • Jiménez Carvelo A. M., Department of Analytical Chemistry, Faculty of Sciences, University of Granada,

    She is a Ramón y Cajal researcher at the University of Granada, leading her own research line, CMQ-Food (https://cmq.ugr.es/). Recognized for two consecutive years (2023 and 2024) in the Stanford Ranking as an influential young researcher in the field of analytical chemistry. She received the Extraordinary Doctorate Award from the University of Granada (Spain) in September 2022. Since November 2022, she has been the delegate of the Spanish Society of Analytical Chemistry in the European Chemical Young Chemists Network (ECYN) of the European Chemical Society (EuChemS). Her research activity includes: 52 articles in JCR journals, 10 book chapters with internationally recognized publishers, editor of 2 books (ELSEVIER and SPRINGER), 4 research projects/contracts as Principal Investigator (PI), 2 supervised PhD theses, 13 master’s theses, and 12 bachelor’s theses.

  • Olmos-Espejel J. J., Multidisciplinary Research Unit, Faculty of Higher Studies Cuautitlán, UNAM.

    He is a Professor/Researcher at the Faculty of Higher Studies Cuautitlán, UNAM, and holds a Ph.D. in Chemical Sciences awarded by the National Autonomous University of Mexico. He has published 11 articles in indexed journals and 11 in peer-reviewed journals, achieving a total of 185 citations and an h-index of 5 to date. He has participated in 15 national and international conferences. Throughout his career, he has supervised 20 undergraduate theses in the field of Analytical Chemistry. As additional information, his expertise includes liquid and gas chromatography. Contact email: jjolmos@cuautitlan.unam.mx

  • Pérez-Caballero G., Multidisciplinary Research Unit, Faculty of Higher Studies Cuautitlán, UNAM.

    Professor/Researcher at UNAM - Retired, holding a Ph.D. awarded by UNAM. She is a member of the National System of Researchers (SNII) at Level 1. She has published 12 articles in indexed journals, achieving a total of 181 citations and an h-index of 5 to date. She has participated in 10 national and international conferences. Throughout her career, she has supervised 10 undergraduate theses, 8 master's theses, and 5 doctoral theses in the field of Analytical Chemistry. Contact email: perezcg@unam.mx

  • Cuevas-Rodriguez E. O., Faculty of Chemical Biological Sciences, UAS

    She is a Researcher at the Autonomous University of Sinaloa and holds a Ph.D. in Food Science awarded by Autonomous University of Querétaro. She is a member of the National System of Researchers (SNII) at Level 2, an Honorary Member of the SSIT, and holds a PRODEP Profile. She has published 53 articles in indexed journals and 10 in peer-reviewed journals, achieving a total of 800 citations and an h-index of 23 to date. She has participated in 50 national and international conferences. Throughout her career, she has supervised 5 undergraduate theses, 5 master's theses, and 2 doctoral theses in the field of Food Science. Contact email: edith.cuevas.r@uas.edu.mx

References

Arendse, E., Nieuwoudt, H., Magwaza, L. S., Nturambirwe, J. F. I., Fawole, O. A. and Opara, U. L. (2021). Recent advancements on vibrational spectroscopic techniques for the detection of authenticity and adulteration in horticultural products with specific focus on oils, juices and powders. Food and Bioprocess Technology 14, 1-22. https://doi.org/10.1007/s11947-020-02505-x

ASTM E2617-17. (2017). Standard practice for validation of empirically derived multivariate calibrations. ASTM International.

Bukovsky-Reyes, S. E. R., Lowe, L. E., Brandon, W. M. and Owens, J. E. (2018). Measurement of antioxidants in distilled spirits by a silver nanoparticle assay. Journal of the Institute of Brewing 124, 291-299. https://doi.org/10.1002/jib.496

Consejo Regulador del Tequila, CRT. (2016). Disponible en: https://crt.org.mx/. Acceso: Diciembre 12, 2024.

Contreras, U., Barbosa-García, O., Pichardo-Molina, J. L., Ramos-Ortíz, G., Maldonado, J. L., Meneses-Nava, M. A., Ornelas-Soto, N. E., López-de-Alba, P. L. (2010). Screening method for identification of adulterate and fake tequilas by using UV–VIS spectroscopy and chemometrics. Food Research International 43, 2356-2362. https://doi.org/10.1016/j.foodres.2010.09.001

Cuadros-Rodríguez, L., Pérez Castaño, E. and Ruiz Samblás, C. (2016). Quality performance metrics in multivariate classification methods for qualitative analysis. Trends in Analytical Chemistry 80, 612-624. https://doi.org/10.1016/j.trac.2016.04.02

Fernández-Lozano, C., Gestal-Pose, M., Pérez-Caballero, G., Revilla-Vázquez, A. L., and Andrade-Garda, J. M. (2019). Multivariate classification techniques to authenticate Mexican commercial spirits. In: Quality control in the beverage industry, (A. M. Grumezescu & A. M. Holban. https://doi.org/10.1016/B978-0-12-816681-9.00008-4, eds.), Pp. 259–288. Woodhead Publishing, Elsevier.

Hibbert, D. B. (2016). Introduction to multivariate data analysis and chemometrics. Analytical and Bioanalytical Chemistry 408(9), 2053-2054.

Jiménez-Carvelo, A. M., Martin-Torres, S., Cuadros-Rodríguez, L., González-Casado, A. (2021). Nontargeted fingerprinting approaches. In Food authentication and traceability, (C.M. Galankis, ed.), Pp. 163-193. Academic Press. https://doi.org/10.1016/B978-0-12-821104-5.00010-6

Keong Tan, W., Husin, Z., Luqman Yasruddin, M., Hakim Ismail, M. A. (2023). Recent technology for food and beverage quality assessment: a review. Journal of Food Science and Technology 60, 1681-1694. https://doi.org/10.1007/s13197-022-05439-8

Kolomiets, O. A., Lachenmeier, D. W., Hoffmann, U. and Siesler, H. W. (2010) Quantitative determination of quality parameters and authentication of vodka using near infrared spectroscopy. Journal of Near Infrared Spectroscopy 18, 59-67. https://doi.org/10.1255/jnirs.866

Livermore, D., Wang, Q. and Jackson, R. S. (2003). Understanding near infrared spectroscopy and its applications in the distillery. In The alcohol textbook, a reference for the beverage, fuel and industrial alcohol industries, (K.A. Jacques, T.P. Lyons and D.R. Kelsall, eds.), Pp. 145-170. Nottingham University Press. Disponible en: https://edisciplinas.usp.br/pluginfile.php/2993570/mod_resource/content/1/The_Alcohol_Textbook-%204%20Ed.pdf Acceso: Diciembre 12, 2024.

Norma Mexicana NMX-V-004-NORMEX-2018. Bebidas alcohólicas-Determinación de furfural- Métodos de ensayo (prueba). Organismo Nacional de Normalización Sociedad Mexicana de Normalización y Certificación, S.C. Comité Técnico de Normalización Nacional para Bebidas Alcohólicas.

Norma Mexicana NMX-V-005-NORMEX-2018. Bebidas alcohólicas-Determinación de aldehídos, ésteres, metanol, y alcoholes superiores-Métodos en ensayo (prueba). Organismo Nacional de Normalización Sociedad Mexicana de Normalización y Certificación, S.C. Comité Técnico de Normalización Nacional para Bebidas Alcohólicas.

Norma Oficial Mexicana NOM-006-SCFI-2012, Bebidas alcohólicas-Tequila-Especificaciones. Comité Consultivo Nacional de Normalización de Seguridad al Usuario, Información Comercial y Prácticas de Comercio (CCNNSUICPC).

Pérez-Beltrán, C. H., Pérez-Caballero, G., Andrade, J. M., Cuadros-Rodríguez, L., Jiménez-Carvelo, A. M. (2022). Non-targeted spatially offset Raman spectroscopy-based vanguard analytical method to authenticate spirits: White Tequilas as a case study. Microchemical Journal 183, 108126. https://doi.org/10.1016/j.microc.2022.108126

Pérez-Beltrán, C. H., Zúñiga-Arroyo, V. M., Andrade, J. M., Cuadros-Rodríguez, L., Pérez-Caballero, G., Jiménez-Carvelo, A. M. (2021). A sensor-based methodology to differentiate pure and mixed White Tequilas based on fused infrared spectra and multivariate data treatment. Chemosensors 9, 1-13. https://doi.org/10.3390/chemosensors9030047

Peña-Alvares, A., Capella, S., Juárez, R. and Labastida, C. (2006). Determination of terpens in tequila by solid pase microextraction-gas chromatography-mass spectrometry. Journal of Chromatography 1134, 291-297. https://doi.org/10.1016/j.chroma.2006.09.005

Pontes, M., Santos, S., Araujo, M., Almeida, L., Lima, R., Gaiao, E. and Souto, U. (2006). Classification of distilled alcoholic beverages and verification of adulteration by near infrared spectrometry. Food Research International 39, 182-189. https://doi.org/10.1016/j.foodres.2005.07.005

Soto-Romero, L., Gutiérrez-Osnaya, L. J. and Trejo-Fragoso, L. (2016) Revisión de los compuestos responsables del olor y sabor del Tequila. Investigación y Desarrollo en Ciencia y Tecnología de Alimentos 1, 910-915. http://www.fcb.uanl.mx/IDCyTA/files/volume1/1/10/157.pdf

Tirado-Kulieva, V. A., Hernandez-Martinez, E. and Suomela, J. P. (2022). Non-destructive assessment of vitamin C in food: a review of the main findings and limitations of vibrational spectroscopic techniques. European Food Research and Technology 248, 2185 – 2195. https://doi.org/10.1007/s00217-022-04023-w

Valcárcel, M. and Cárdenas, S. (2005). Vanguard-rearguard analytical strategies. Trends in Analytical Chemistry 24, 67–74. https://doi.org/10.1016/j.trac.2004.07.016

Vallejo-Córdoba, B., González-Córdova, A. F. and Estrada-Montoya, M. C. (2004). Tequila volatile characterization and ethyl ester determination by solid phase microextraction gas chromatography/mass spectrometry analysis. Journal of Agricultural and Food Chemistry 52, 5567-5571. https://doi.org/10.1021/jf0499119

Warren-Vega, W. M., Fonseca-Aguiñaga, R., González-Gutiérrez, L. V. and Romero-Cano, L. A. (2023). A critical review on the assessment of the quality and authenticity of tequila by different analytical techniques: Recent advances and perspectives. Food Chemistry 408, 135223. https://doi.org/10.1016/j.foodchem.2022.135223

Wise, B. M., Gallagher, N. B., Bro, R., Shaver, J. M., Winding, W. and Koch, R. S. (2006). Chemometrics Tutorial for PLS_Toolbox and Solo. Eigenvector Research, Inc. Wenatchee, WA, USA.

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Published

2025-01-29

Data Availability Statement

The data were obtained from the author's doctoral thesis

Issue

No. 3 (2025): QUIBIOUAS Revista de Ciencias Químico Biológicas

Section

Scientific articles

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Copyright (c) 2025 QUIBIOUAS, Journal of Biological Chemical Sciences

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How to Cite

Pérez Beltrán , C. H., León López, L. ., Jiménez Carvelo, A. M. ., Olmos Espejel, J. de J., Pérez Caballero, G., & Cuevas Rodríguez, E. O. (2025). Multivariable analytical method based on NIR spectroscopy and chemometric tools to differentiate between ’100% agave’ and ’mixed’ white tequila. QUIBIOUAS, Journal of Biological Chemical Sciences, 3, 8-17. https://revistas.uas.edu.mx/index.php/QBU/article/view/953