Rapid discrimination of Nigella Sativa oil from different geographical origins using ATR-FTIR-unsupervised and supervised pattern recognition techniques
El Newehy, N., Omran, G., Harraz, F., Shawky, E., Beltagy, A. (2025). Rapid discrimination of Nigella Sativa oil from different geographical origins using ATR-FTIR-unsupervised and supervised pattern recognition techniques. EKB Journal Management System, 2(1), 44-53. doi: 10.21608/japs.2024.320326.1028
Nihal M. El Newehy; Gamal A. Omran; Fathallah M. Harraz; Eman Shawky; Amira M. Beltagy. "Rapid discrimination of Nigella Sativa oil from different geographical origins using ATR-FTIR-unsupervised and supervised pattern recognition techniques". EKB Journal Management System, 2, 1, 2025, 44-53. doi: 10.21608/japs.2024.320326.1028
El Newehy, N., Omran, G., Harraz, F., Shawky, E., Beltagy, A. (2025). 'Rapid discrimination of Nigella Sativa oil from different geographical origins using ATR-FTIR-unsupervised and supervised pattern recognition techniques', EKB Journal Management System, 2(1), pp. 44-53. doi: 10.21608/japs.2024.320326.1028
El Newehy, N., Omran, G., Harraz, F., Shawky, E., Beltagy, A. Rapid discrimination of Nigella Sativa oil from different geographical origins using ATR-FTIR-unsupervised and supervised pattern recognition techniques. EKB Journal Management System, 2025; 2(1): 44-53. doi: 10.21608/japs.2024.320326.1028

Rapid discrimination of Nigella Sativa oil from different geographical origins using ATR-FTIR-unsupervised and supervised pattern recognition techniques

Journal of Advanced Pharmaceutical Sciences
Volume 2, Issue 1, January 2025, Page 44-53  XML PDF (783.32 K)
Document Type: Original Article
DOI: 10.21608/japs.2024.320326.1028
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Authors
Nihal M. El Newehy email 1; Gamal A. Omran2; Fathallah M. Harraz3; Eman Shawky3; Amira M. Beltagy1
1Department of Pharmacognosy, Faculty of Pharmacy, Damanhour University
2Department of Biochemistry, Faculty of Pharmacy, Damanhour University
3Department of Pharmacognosy, Faculty of Pharmacy, Alexandria University
Abstract
Previous metabolomics studies have proven the efficiency of infrared (IR) spectroscopy as a tool for authenticity assessment. Attenuated total reflectance – Fourier transform infrared spectroscopy (ATR-FTIR), with principal component analysis (PCA) and bidirectional orthogonal projection to latent structures-discriminant analysis (O2PLS-DA), was used to create a model for the discrimination of N. sativa oil samples gathered from three geographical areas; Egypt, Ethiopia and Syria. It is reported that, for herbal drug treatments even from the equal species, the quality and efficacy are somewhat different according to their growing conditions. The unsupervised pattern recognition of variable authentic samples utilizing PCA and HCA (Hierarchical Cluster Analysis) revealed that each oil type was separately clustered from the others. 
The data matrix of ATR-FTIR was handled by the supervised pattern recognition technique O2PLS-DA to give a better clustering and a better separation between sample types than given by PCA. For the first time, this study built a partial least square (PLS) model used to predict thymoquinone concentration in any new N. sativa seed oil only by its ATR FT-IR spectrum. Furthermore, OPLS and its HCA model of authentic samples have been used to predict types of commercial oil samples obtained from the Egyptian market and compare them with sellers' claims.
As demonstrated in this study, the recommended method might be used to regularly evaluate the phytochemical variability in N. sativa seed oil varieties sourced from various regions, which could aid in meeting the demand for their quality and safety.  

Highlights

•    ATR-FTIR has been used for the quality assessment of N.sativa oils.
•    Multivariate analysis could discriminate oils from different origins.
•    OPLS and HCA models were built for authentic oil samples.
•     Models predict commercial oil types and compare them with sellers' claims. 
•    Only 29.6% of oil samples were considered well-claimed by sellers.

 

Keywords
Nigella sativa seed oil; ATR-FTIR; Geographical origin; Multivariate analysis
Supplementary Files
References
(1)    Burits M, Bucar F. Antioxidant activity of Nigella sativa essential oil. Phytotherapy research. 2000;14(5):323-8.
(2)    Al-Saleh IA, Billedo G, El-Doush II. Levels of selenium, dl-α-tocopherol, dl-γ-tocopherol, all-trans-retinol, thymoquinone and thymol in different brands of Nigella sativa seeds. Journal of Food Composition and Analysis. 2006;19(2):167-75.
(3)    Khoddami A, Ghazali HM, Yassoralipour A, Ramakrishnan Y, Ganjloo A. Physicochemical characteristics of nigella seed (Nigella sativa L.) oil as affected by different extraction methods. Journal of the American Oil Chemists' Society. 2011;88(4):533-40.
(4)    Cheikh-Rouhou S, Hentati B, Besbes S, Blecker C, Deroanne C, Attia H. Chemical composition and lipid fraction characteristics of Aleppo pine (Pinus halepensis Mill.) seeds cultivated in Tunisia. Revista de Agaroquimica y Tecnologia de Alimentos. 2006;12(5):407-15.
(5)    Salem ML, Hossain MS. In vivo acute depletion of CD8+ T cells before murine cytomegalovirus infection upregulated innate antiviral activity of natural killer cells. International journal of immunopharmacology. 2000;22(9):707-18.
(6)    Worthen DR, Ghosheh OA, Crooks P. The in vitro anti-tumor activity of some crude and purified components of blackseed, Nigella sativa L. Anticancer research. 1997;18(3A):1527-32.
(7)    Houghton PJ, Zarka R, de las Heras B, Hoult J. Fixed oil of Nigella sativa and derived thymoquinone inhibit eicosanoid generation in leukocytes and membrane lipid peroxidation. Planta medica. 1995;61(01):33-6.
(8)    Morsi NM. Antimicrobial effect of crude extracts of Nigella sativa on multiple antibiotics-resistant bacteria. Acta Microbiologica Polonica. 2000;49(1):63.
(9)    Salih B, Sipahi T, Dönmez EO. Ancient nigella seeds from Boyalı Höyük in north-central Turkey. Journal of ethnopharmacology. 2009;124(3):416-20.
(10)    Peter KV. Handbook of herbs and spices: Elsevier; 2012.
(11)    Malik U, Pal D. Nigella sativa (Black Cumin) Seed: A Natural Source of Antioxidant and Antiproliferative Agent.  Seeds: Anti-proliferative Storehouse for Bioactive Secondary Metabolites: Springer; 2024. p. 427-50.
(12)    Gupta I, Serva Peddha M. Characterization of polyphenols profile, antioxidant, and in vitro activities of Nigella sativa L.(black cumin) seed oleoresin. Journal of Food Measurement and Characterization. 2024;18(3):2205-15.
(13)    Roney M, Dubey A, Nasir MH, Huq AM, Tufail A, Tajuddin SN, et al. Computational evaluation of quinones of Nigella sativa L. as potential inhibitor of dengue virus NS5 methyltransferase. Journal of Biomolecular Structure and Dynamics. 2024;42(16):8701-11.
(14)    Sultana S, Asif HM, Akhtar N, Iqbal A, Nazar H, Rehman RU. Nigella sativa: Monograph. Journal of Pharmacognosy and Phytochemistry. 2015;4(4):103.
(15)    Luykx DM, Van Ruth SM. An overview of analytical methods for determining the geographical origin of food products. Food Chemistry. 2008;107(2):897-911.
(16)    Feudo GL, Macchione B, Naccarato A, Sindona G, Tagarelli A. The volatile fraction profiling of fresh tomatoes and triple concentrate tomato pastes as parameter for the determination of geographical origin. Food Research International. 2011;44(3):781-8.
(17)    Peres B, Barlet N, Loiseau G, Montet D. Review of the current methods of analytical traceability allowing determination of the origin of foodstuffs. Food Control. 2007;18(3):228-35.
(18)    Shawky E, El Newehy NM, Beltagy AM, Abd-Alhaseeb MM, Omran GA, Harraz FM. Fingerprint profile and efficacy-associated markers of Nigella sativa oil for geographical origin determination using targeted and untargeted HPTLC-multivariate analysis. Journal of Chromatography B. 2018;1087:108-17.
(19)    Singh I, Juneja P, Kaur B, Kumar P. Pharmaceutical applications of chemometric techniques. ISRN Analytical Chemistry. 2013;2013.
(20)    Tahir HE, Arslan M, Mahunu GK, Mariod AA, Hashim SB, Xiaobo Z, et al. The use of analytical techniques coupled with chemometrics for tracing the geographical origin of oils: A systematic review (2013–2020). Food Chemistry. 2022;366:130633.
(21)    Sammarco G, Dall’Asta C, Suman M. Near-infrared spectroscopy and multivariate statistical analysis as rapid tools for the geographical origin assessment of Italian hazelnuts. Vibrational Spectroscopy. 2023;126:103531.
(22)    Gu H-W, Yin X-L, Peng T-Q, Pan Y, Cui H-N, Li Z-Q, et al. Geographical origin identification and chemical markers screening of Chinese green tea using two-dimensional fingerprints technique coupled with multivariate chemometric methods. Food Control. 2022;135:108795.
(23)    Longobardi F, Ventrella A, Casiello G, Sacco D, Tasioula-Margari M, Kiritsakis A, et al. Characterization of the geographical origin of Western Greek virgin olive oils based on instrumental and multivariate statistical analysis. Food Chemistry. 2012;133(1):169-75.
(24)    Hamed S, Shaaban H, Ramadan A, Edris A. Potentials of enhancing the physicochemical and functional characteristics of Nigella sativa oil by using the screw pressing technique for extraction. Grasas y Aceites. 2017;68(2):e188-e.
(25)    Gouvinhas I, de Almeida JM, Carvalho T, Machado N, Barros AI. Discrimination and characterization of extra virgin olive oils from three cultivars in different maturation stages using Fourier transform infrared spectroscopy in tandem with chemometrics. Food chemistry. 2015;174:226-32.
(26)    Shen X, Ye S, Xu L, Hu R, Jin L, Xu H, et al. Study on baseline correction methods for the Fourier transform infrared spectra with different signal-to-noise ratios. Applied Optics. 2018;57(20):5794-9.
(27)    Grisanti E, Totska M, Huber S, Krick Calderon C, Hohmann M, Lingenfelser D, et al. Dynamic localized SNV, Peak SNV, and partial peak SNV: Novel standardization methods for preprocessing of spectroscopic data used in predictive modeling. Journal of Spectroscopy. 2018;2018(1):5037572.
(28)    Lee LC, Liong C-Y, Jemain AA. A contemporary review on Data Preprocessing (DP) practice strategy in ATR-FTIR spectrum. Chemometrics and Intelligent Laboratory Systems. 2017;163:64-75.
(29)    Socaciu C, Fetea F, Ranga F. IR and Raman spectroscopy-advanced and versatile techniques for agrifood quality and authenticity assessment. Bull Univ Agric Sci Vet Med Cluj-Napoca Agric. 2009;66:459-64.
(30)    Nurrulhidayah A, Man Y, Al-Kahtani H, Rohman A. Application of FTIR spectroscopy coupled with chemometrics for authentication of Nigella sativa seed oil. Journal of Spectroscopy. 2011;25(5):243-50.
(31)    Worley B, Powers R. PCA as a practical indicator of OPLS-DA model reliability. Current Metabolomics. 2016;4(2):97-103.
(32)    Galindo-Prieto B, Trygg J, Geladi P. A new approach for variable influence on projection (VIP) in O2PLS models. Chemometrics and Intelligent Laboratory Systems. 2017;160:110-24.

 

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