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1H NMR-Based Metabolomics Approach Revealing Metabolite Variation of Black Turmeric (Curcuma caesia) Extracts and Correlation with Its Antioxidant and α-Glucosidase Inhibitory Activities

Nurul Najiha Ain Ibrahim1orcid tiny, Nurkhalida Kamal2orcid tiny, Ahmed Mediani2orcid tiny, Azliana Abu Bakar Sajak3orcid tiny, Soo Yee Lee4orcid tiny, Khozirah Shaari4orcid tiny and Hafeedza Abdul Rahman1,5*orcid tiny

1Department of Food Sciences, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

2Institute of Systems Biology (INBIOSIS), Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

3Department of Nutrition and Dietetics, Faculty of Medicine and Health Sciences, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia

4Laboratory of Natural Medicines and Products (NaturMeds) Institute of Bioscience, Universiti Putra Malaysia, 43400 Serdang, Selangor, Malaysia

5Centre of Excellence, Innovation Centre for Confectionery Technology (MANIS), Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

Article history:

Received: 5 March 2022

Accepted: 7 February 2023

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antioxidant activity; α-glucosidase inhibition; Curcuma caesia; extraction; metabolomics


Research background. Curcuma species (Zingiberaceae) are well known medicinal herbs in India and Southeast Asia. Despite various findings reporting their beneficial biological activities, very little information has been recorded on the Curcuma caesia. Thus, this study aims to determine the phenolic content, antioxidant and α-glucosidase inhibitory activity of both rhizome and leaves of C. caesia.

Experimental approach. Rhizome and leaves of C. caesia were dried with oven and freeze drying methods, and extracted with different ethanol/water ratios of 0/100, 50/50, 80/20 and 100/0. The bioactivities of C. caesia extracts were evaluated using in vitro tests; total phenolic content (TPC), antioxidant (DPPH and FRAP) and α-glucosidase inhibitory activity. Proton nuclear magnetic resonance (1H NMR)-based metabolomics approach was employed to differentiate the most active extracts based on their metabolite profiles and correlation with bioactivities.

Results and conclusions. The 100/0 freeze-dried rhizome extract was observed to have potent TPC, FRAP and α-glucosidase inhibitory activity with values of (45.38±2.10) mg GAE/g extract, (147.73±8.26) mg TAE/g extract and (265.46±38.62) µg/mL (IC50), respectively. Meanwhile, for DPPH scavenging activity, the 80/20 and 100/0 extracts of freeze-dried rhizome showed the highest activity with no significant difference between them. Hence, the freeze-dried rhizome extracts were selected for further metabolomics analysis. Principal component analysis (PCA) showed clear discrimination among the different extracts. Partial least square (PLS) analysis showed positive correlations between the metabolites, including xanthorrhizol derivative, l-hydroxy-1,7-bis(4-hydroxy-3-methoxyphenyl)-(6E)-6-heptene-3,4-dione, valine, luteolin, zedoardiol, β-turmerone, selina-4(15),7(11)-dien-8-one, zedoalactone B and germacrone, with the antioxidant and α-glucosidase inhibition activities. Meanwhile, curdione and 1-(4-hydroxy-3,5-dimethoxyphenyl)-7-(4-hydroxy-3-methoxyphenyl)-(lE,6E)-1,6-heptadiene3,4-dione were correlated with α-glucosidase inhibitory activity.

Novelty and scientific contribution. Novelty and scientific contribution. C. caesia rhizome and leaf extracts contained phenolic compounds and had varies antioxidant and α-glucosidase inhibitory capacities. These findings strongly suggests that the rhizomes of C. caesia are an invaluable natural source of active ingredients for applications in pharmaceutical and food industries.

*Corresponding author: +60122229365

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