Rapid authentication measurement of cinnamon powder using FT-NIR and FT-IR spectroscopic techniques

Main Article Content

J. Yasmin
M.R. Ahmed
S. Lohumi
C. Wakholi
H. Lee
C. Mo
B.-K. Cho


food adulteration, powder food, cinnamon, Fourier transform infrared spectroscopy, Fourier transform nearinfrared spectroscopy


Owing to the worldwide demand for cinnamon spices, true cinnamon (Cinnamomum verum) powder is often being adulterated with another inferior quality of cinnamon known as cassia cinnamon (Cinnamomum aromaticum). This study employed Fourier transform near-infrared (FT-NIR) and Fourier transform infrared (FT-IR) spectroscopic analysis to determine the spectral differences in assorted percentages after mixing with adulterants. The absorbance spectra of total 195 samples were collected of true, cassia and various adulterated samples (5-50 wt % adulterate) with 15 replicates for each sample. Independent component analysis was integrated with FT-NIR and FT-IR spectroscopic data for the detection of an unknown cinnamon mixture as a blind source separation tool that revealed distinctive peak difference. The partial least square regression (PLSR) models with spectral preprocessing methods were applied to predict the presence of cassia cinnamon in true cinnamon powder. The PLSR model for the FT-NIR and FT-IR data predicted adulteration with an R2p of 0.97 with a root-mean square error of prediction (RMSEP) of 2.2% and an R2p of 0.96 with an RMSEP of 2.5% respectively after applying Savitzky-Golay 2nd derivative as preprocessing. Thus, the predictive value of FT-NIR data was greater than the FT-IR data. In addition, the ratio of standard error of performance to standard deviation (RPD>2.5) and the range error ratio (RER>10) values were also calculated for both of the spectroscopic techniques to predict model accuracy for the independent validation set. The ? coefficient curve from the PLSR models also revealed the spectral peak differences among the samples concentrated with various amount of cassia cinnamon powder. These methods proved that FT-NIR and FT-IR spectroscopic techniques combined with multivariate analysis could be utilised as a controlled procedure or as an alternative rapid detection method to identify adulterated cinnamon powder.

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Ahmed, M.R., Yasmin, J., Lee, W.H., Mo, C. and Cho, B.K., 2017. Imaging technologies for nondestructive measurement of internal properties of agricultural products: a review. Journal of Biosystems Engineering 42(3): 199-216.
Allen, R.W., Schwartzman, E., Baker, W.L., Coleman, C.I. and Phung, O.J., 2013. Cinnamon use in Type 2 diabetes: an updated systematic review and meta-analysis. Annals of Family Medicine 11: 452-459.
Appendino, G., Cravotto, G., Tagliapietra, S., Ferraro, S., Nano, G.M. and Pal, G., 1991. The chemistry of coumarin derivatives. Part 3†. Synthesis of 3-alkyl-4-hydroxycoumarins by reductive fragmentation of 3,3'-alkyiidene-4,4'-dihydroxybis[coumarins]. Helvetica Chimica Acta 74: 1451-1458.
Bhau, B.S., Gogoi, G., Baruah, D., Ahmed, R., Hazarika, G., Borah, B., Gogoi, B., Sarmah, D.K., Nath, S.C. and Wann, S.B., 2015. Development of an effective and efficient DNA isolation method for Cinnamomum species. Food Chemistry 188: 264-270.
Celignis Analytical, 2018. Near infrared spectroscopy. Available at:http://www.celignis.com/NIR.php
Chen, J. and Wang, X.Z., 2001. A new approach to near-infrared spectral data analysis using independent component analysis. Journal of Chemical Information and Computer Sciences 41: 992-1001.
Chen, P., Sun, J. and Ford, P., 2014. Differentiation of the four major species of cinnamons (C. burmannii, C. verum, C. cassia, and C. loureiroi) using a Flow Injection Mass Spectrometric (FIMS) fingerprinting method. Journal of Agriculture and Food Chemistry 62: 2516-2521.
Cho, B.K., Lohoumi, S., Choi, C., Yang, S. and Kang, S., 2016. Study on rapid measurement of wood powder concentration of wood-plastic composites using FT-NIR and FT-IR spectroscopy techniques. Korean Wood Science Technology 44: 852-863.
Cinnamon Vogue, 2018. Cinnamon used in North America. Available at:https://tinyurl.com/y5o85shq
Clifford, G.D., 2007. Blind source separation: PCA and ICA. Massachusetts Institute of Technology, Cambridge, MA, USA.
Delfosse, N. and Loubaton, P., 1995. Adaptive blind separation of independent sources: a deflation approach. Signal Processing 45: 59-83.
Dhanya, K., Syamkumar, S. and Sasikumar, B., 2009. Development and application of SCAR marker for the detection of papaya seed adulteration in traded black pepper powder. Food Biotechnology23: 97-106.
European Council, 1988. Council Directive of 22 June 1988 on the approximation of the laws of the member states relating to flavourings for use in foodstuffs and to source materials for their production. Official Journal L 184: 61-66.
European Food Safety Authority, 2004. Opinion of the scientific panel on food additives, flavourings, processing aids and materials in contact with food (AFC) related to Coumarin. Available at:https://efsa.onlinelibrary.wiley.com/doi/epdf/10.2903/j.efsa.2004.104
Gende, L.B., Floris, I., Fritz, R. and Eguaras, M.J., 2008. Antimicrobial activity of cinnamon (Cinnamomum zeylanicum) essential oil and its main components against paenibacillus larvae from argentine. Bulletin of Insectology 61: 1-4.
German Federal Institute of Risk Assessment, 2012. FAQ on coumarin in cinnamon and other foods. Available at:https://tinyurl.com/pcz5qo3
Haughey, S.A., Galvin-King, P., Ho, Y.C., Bell, S.E.J. and Elliott, C.T., 2015. The feasibility of using near infrared and Raman spectroscopic techniques to detect fraudulent adulteration of chili powders with Sudan dye. Food Control 48: 75-83.
He, Z.D., Qiao, C.F., Han, Q.B., Cheng, C.L., Xu, H.X., Jiang, R.W., But, P.P.H. and Shaw, P.C., 2005. Authentication and quantitative analysis on the chemical profile of Cassia Bark (cortex cinnamomi) by high-pressure liquid chromatography. Journal of Agriculture and Food Chemistry 53: 2424-2428.
Hyvärinen, A. and Oja, E., 2000. Independent component analysis: algorithms and applications. Neural Networks 13: 411-430.
Ko, A.Y., Rahman, M.M., El-Aty, A.M.A., Jang, J., Choi, J.H., Mamun, M.I.R. and Jae-Han, S., 2014. Identification of volatile organic compounds generated from healthy and infected powdered chili using solvent-free solid injection coupled with GC/MS: application to adulteration. Food Chemistry 156: 326-332.
Lee, J., Yoo, C. and Lee, I., 2004. Statistical process monitoring with independent component analysis. Journal of Process Control 14: 467-485.
Lee, S.C., Chiou, S.J., Yen, J.H., Lin, T.Y., Hsieh, K.T. and Yang, J.C., 2010. DNA barcoding Cinnamomum osmophloeum KanehBased on the partial non-coding ITS2 region of ribosomal genes. Journal of Food and Drug Analysis 18: 128-135.
Lim, J.G., Kim, G.Y., Mo, C.Y., Oh, K.M., Kim, G.S., Yoo, H.C., Ham, H.H., Kim, Y.T., Kim, S.M. and Kim, M.S., 2017. Rapid and nondestructive discrimination of Fusarium Asiaticum and Fusarium Graminearum in hulled barley (Hordeum vulgare L.) using near-infrared spectroscopy. Journal of Biosystems Engineering 42: 301-313.
.Liu, F., Jiang, Y. and He, Y., 2009. Variable selection in visible/near infrared spectra for linear and nonlinear calibrations: a case study to determine soluble solids content of beer. Analytica Chimica Acta 635: 45-52.
Lohumi, S., Joshi, R., Kandpal, L.M., Lee, H., Kim, M.S., Cho, H., Mo, C., Seo, Y.W., Rahman, A. and Cho, B.K., 2017. Quantitative analysis of Sudan dye adulteration in paprika powder using FTIR spectroscopy. Food Additives and Contaminants: Part A 34: 678-686.
Lohumi, S., Kandpal, L.M., Seo, Y.W. and Cho, B.K., 2016. Net analyte signal-based quantitative determination of fusel oil in Korean alcoholic beverage using FT-NIR spectroscopy. Journal of Biosystems Engineering 41: 208-220.
Lu, T., Sheng, H.G., Wu, J., Cheng, Y., Zhu, J.M. and Chen, Y., 2012. Cinnamon extract improves fasting blood glucose and glycosylated hemoglobin level in Chinese patients with type 2 diabetes. Nutrition Research 32: 408-412.
Lu, X., Al-Qadiri, H.M., Lin, M. and Rasco, B.A., 2011. Application of mid-infrared and Raman spectroscopy to the study of bacteria. Food and Bioprocess Technology 4: 919-935.
Lungarini, S., Aureli, F. and Coni, E., 2008. Coumarin and cinnamaldehyde in cinnamon marketed in Italy: a natural chemical hazard. Food Additives and Contaminants: Part A 25: 1297-1305.
Medicinal News Today, 2017. What are the health benefits of cinnamon? Available at:https://www.medicalnewstoday.com/articles/266069.php
Mo, C., Lim, J., Kwon, S.W., Lim, D.K., Kim, M.S., Kim, G., Kang, J., Kwon, K.D. and Cho, B.K., 2017. Hyperspectral imaging and partial least square discriminant analysis for geographical origin discrimination of white rice. Journal of Biosystems Engineering 42: 293-300.
Parthasarathy, V.A., Chempakam, B. and Zachariah, T.J. (eds.), 2008. Chemistry of spices. Biddles Ltd., Oxfordshire, UK, 124 pp.
Parvathy, V.A., Swetha, V.P., Sheeja, T.E., Leela, N.K., Chempakam, B. and Sasikumar, B., 2014. DNA barcoding to detect chilli adulteration in traded black pepper powder. Food Biotechnology 28: 25-40.
Petrakis, E.A., Cagliani, L.R., Polissiou, M.G. and Consonni, R., 2015. Evaluation of saffron (Crocus sativus L.) adulteration with plant adulterants by 1H NMR metabolite fingerprinting. Food Chemistry 173: 890-896.
Qin, J., Kim, M.S., Chao, K. and Cho, B.K., 2017. Raman chemical imaging technology for food and agricultural application. Journal of Biosystems Engineering 42: 170-189.
Raters, M. and Matissek, R., 2008. Analysis of coumarin in various foods using liquid chromatography with tandem mass spectrometric detection. European Food Research and Technology 227: 637-642.
Rinnan, Å., Berg, F.V.D. and Engelsen, S.B., 2009. Review of the most common pre-processing techniques for near-infrared spectra. TrAC Trends in Analytical Chemistry 28: 1201-1222.
Savitzky, A. and Golay, M.J.E., 1964. Smoothing and differentiation of data by simplified least squares procedures. Analytical Chemistry 36: 1627-1638.
Scholl, P.F., Samantha M.F. and Magdi, M.M., 2014. Rapid turbidimetric detection of milk powder adulteration with plant proteins. Journal of Agriculture and Food Chemistry 62: 1498-1505.
See, C., Bilonick, R.A., Feuer, W. and Galor, A., 2013. Comparison of two methods for composite score generation in dry eye syndrome. Investigative Ophthalmology & Visual Science 54: 6280-6286.
Senanayake, U.M., Lee, T.H. and Wills, R.B.H., 1978. Volatile constituents of cinnamon (Cinnamomum zeylanicum) oils. Journal of Agriculture and Food Chemistry 26: 822-824.
Seo, Y.W., Ahn, C.K., Lee, W.H., Park, E., Mo, C. and Cho, B.K., 2016. Non-destructive sorting techniques for viable pepper (Capsicum annuum L.) seeds using Fourier transform near-infrared and Raman spectroscopy. Journal of Biosystems Engineering 41: 51-59.
Sliškovi?, D., Grbi?, R. and Hocenski, Ž., 2012. Multivariate statistical process monitoring. Tehni ki vjesnik ? 19: 33-41.
Sproll, C., Ruge, W., Andlauer, C., Godelmann, R. and Lachenmeier, D.W., 2008. HPLC analysis and safety assessment of coumarin in foods. Food Chemistry 109: 462-469.
Starr, C., Morgan, A.G. and Smith, D.B., 1981. An evaluation of near infra-red reflectance analysis in some plant breeding programmes. Journal of Agricultural Science 97: 107-118.
Swetha, V.P., Parvathy, V.A., Sheeja, T.E. and Sasikumar, B., 2014a. Isolation and amplification of genomic DNA from barks of Cinnamomum spp. Turkish Journal of Biology 38: 151-155.
Swetha, V.P., Parvathy, V.A., Sheeja, T.E. and Sasikumar, B., 2014b. DNA barcoding for discriminating the economically important Cinnamomum verum from its adulterants. Food Biotechnology 28: 183-194.
The People’s Pharmacy, 2013. Cinnamon offers health benefits but also carries serious risks. Available at: https://www.peoplespharmacy.com/2013/12/30/cinnamon-offers-health-benefits-but-also-carries-serious-risks/
US Government, 2011. US Code 9. Chapter 21: Federal Food, Drug, and Cosmetic Act. Subchapter IV, §342(b). US Government Publishing Office, Washington, DC, USA. Available at: https://tinyurl.com/y3ngktj3
Uses & Benefits.com, 2016. Different types of cinnamon – what you need to know. Available at: http://uses-and-benefits.com/cinnamon/types-of-cinnamon
Whitfield, P., Parry-Strong, A., Walsh, E., Weatherall, M. and Krebs, J.D., 2016. The effect of a cinnamon, chromium- and magnesium-formulated honey on glycaemic control, weight loss and lipid parameters in type 2 diabetes: an open-label cross-over randomised controlled trial. European Journal of Nutrition 55: 1123-1131.
Williams, P. and Norris, K. (eds.) 2001. Near-infrared technology in the agricultural and food industries, 2nd edition. American Association of Cereal Chemists, St. Paul, MN, pp. 145-169.
Woehrlin, F., Fry, H., Abraham, K. and Preiss-Weigert, A., 2010. Quantification of flavoring constituents in cinnamon: high variation of coumarin in cassia bark from the German retail market and in authentic samples from Indonesia. Journal of Agriculture and Food Chemistry 58: 10568-10575.
Ypma, A. and Pajunen, P., 1999. Rotating machine vibration analysis with second-order independent component analysis. In: Proceedings of the first International Workshop on Independent Component Analysis and Signal Separation, Ica’99. Aussois, France, pp. 37-42.