Sains
Malaysiana 55(10)(2026): 1714-1724
http://doi.org/10.17576/jsm-2026-5510-10
Pendekatan
Metabolomik berasaskan ¹H NMR bagi Analisis Profil Metabolit Daun Dillenia
suffruticosa: Implikasi Kepolaran Pelarut terhadap Potensi Anti-Vibrio
(¹H NMR-Based
Metabolomic Approach for Metabolite Profiling of Dillenia suffruticosa Leaves: Implications of Solvent Polarity on Anti-Vibrio Potential)
AZIZUL ISHA1,*, NORAZNITA SHARIFUDDIN2,
MAZNI ABU ZARIN3, YAYA RUKAYADI1 & AHMAD FAIZAL
ABDULL RAZIS1
1Natural Medicines and
Products Research Laboratory, Institute of Bioscience, Universiti Putra
Malaysia, 43400 UPM Serdang, Selangor, Malaysia
2Aquatic Animal Health
and Therapeutics Laboratory, Institute of Bioscience, Universiti Putra
Malaysia, 43400 UPM Serdang, Selangor, Malaysia
3Laboratory of Vaccine
and Biomolecules, Institute of Bioscience, Universiti Putra Malaysia, 43400 UPM
Serdang, Selangor, Malaysia
Diserahkan: 4 November 2025/Diterima: 28
September 2026
*Pengarang untuk surat-menyurat; email:
azizul_isha@upm.edu.my
ABSTRAK
Ancaman kerintangan antimikrob patogen Vibrio kian menjejaskan industri akuakultur dan keselamatan makanan dunia. Justeru,
kajian ini menilai sifat antibakteria ekstrak daun Dillenia suffruticosa terhadap empat patogen Vibrio (V. vulnificus, V.
parahaemolyticus, V. campbellii dan V. harveyi) menggunakan
pendekatan metabolomik ¹H NMR bagi merungkai korelasi antara komposisi
metabolit dengan bioaktivitinya. Aktiviti antibakteria ekstrak berbeza
kepolaran (etanol 70% (v/v), aseton, kloroform dan heksana) dinilai melalui
resapan cakera, kepekatan perencatan minimum (MIC) dan kepekatan bakterisid
minimum (MBC). Ekstrak kloroform menunjukkan perencatan terkuat dengan zon
perencatan 20.52 ± 0.44 mm (V. parahaemolyticus) dan nilai MIC serendah
0.039 mg/mL (V. vulnificus). Ekstrak etanol 70% (v/v) dan aseton
berkesan sederhana, manakala heksana paling lemah. Spektrum ¹H NMR mendedahkan
pelbagai metabolom termasuk asid amino, asid organik, gula, triterpenoid,
sterol dan sebatian fenol. Analisis multivariat (Analisis Komponen Utama (PCA)
dan Kuasa Dua Terkecil Separa (PLS)) membezakan ekstrak berdasarkan jenis
pelarut. Biplot PLS mendedahkan korelasi positif kaempferol, sarkosina dan asid
organik terhadap perencatan V. vulnificus, V. campbellii dan V.
harveyi. Walau bagaimanapun, korelasi negatif majoriti sebatian fenol
terhadap V. parahaemolyticus membuktikan rintangan tinggi patogen
tersebut terhadap ekstrak hidrofilik. Metabolit ini diketahui berupaya
mengganggu pembentukan biofilem, pengesanan kuorum, pergerakan sel serta laluan
virulens Vibrio, sekali gus menyokong asas mekanistik aktiviti tersebut.
Kesimpulannya, korelasi profil metabolomik dan bioaktiviti memberi pemahaman
menyeluruh tentang pengaruh kepolaran pelarut terhadap pemulihan metabolit.
Kajian ini menyerlahkan keupayaan D. suffruticosa sebagai sumber agen
antibakteria bagi menangani isu akuakultur dan keselamatan makanan.
Kata kunci: Aktiviti antibakteria; Dillenia
suffruticosa; metabolit bioaktif; metabolomik ¹H NMR; Vibrio spp.
ABSTRACT
The
threat of antimicrobial resistance among Vibrio pathogens is
increasingly threatening the aquaculture industry and global food security.
Therefore, this study evaluates the antibacterial properties of Dillenia
suffruticosa leaf extracts against four Vibrio pathogens (V.
vulnificus, V. parahaemolyticus, V. campbellii, and V.
harveyi) utilizing a ¹H-NMR metabolomics approach to elucidate the
correlation between metabolite composition and its bioactivity. The
antibacterial activity of extracts with varying polarities (70% (v/v) ethanol,
acetone, chloroform, and hexane) was evaluated through agar well diffusion,
minimum inhibitory concentration (MIC), and minimum bactericidal concentration
(MBC) assays. The chloroform extract exhibited the strongest inhibition, with
an inhibition zone of 20.52 ± 0.44 mm (V. parahaemolyticus) and an MIC
value as low as 0.039 mg/mL (V. vulnificus). The 70% (v/v) ethanol and
acetone extracts were moderately effective, while the hexane extract was the
weakest. The ¹H-NMR spectra showed a diverse metabolome, including amino acids,
organic acids, sugars, triterpenoids, sterols, and phenolic compounds.
Multivariate analysis (Principal Component Analysis (PCA) and Partial Least
Squares (PLS)) differentiated the extracts based on the type of solvent. The
PLS biplot showed a positive correlation of kaempferol, sarcosine, and organic
acids with the inhibition of V. vulnificus, V. campbellii, and V.
harveyi. However, the negative correlation of the majority of phenolic
compounds against V. parahaemolyticus proved the high resistance of this
pathogen towards hydrophilic extracts. These metabolites are known to interfere
with Vibrio biofilm formation, quorum sensing, cell motility, and
virulence pathways, thus supporting the mechanistic basis for the observed
activity. In conclusion, the correlation between metabolomic profiling and
bioactivity provides a comprehensive understanding of the influence of solvent
polarity on metabolite recovery. This study highlights the capability of D.
suffruticosa as a source of antibacterial agents to address aquaculture and
food safety issues.
Keywords:
Antibacterial activity; bioactive metabolites; Dillenia suffruticosa; 1H-NMR
metabolomics; Vibrio spp.
RUJUKAN
Abubakar,
S., Al-Mansoub, M.A., Murugaiyah, V. & Chan, K.L. 2019. The phytochemical
and anti-inflammatory studies of Dillenia suffruticosa leaves. Phytotherapy
Research 33(3): 660-675. https://doi.org/10.1002/ptr.6255
Adamczak,
A., Ożarowski, M. & Karpiński, T.M. 2019. Antibacterial activity
of some flavonoids and organic acids widely distributed in plants. Journal
of Clinical Medicine 9(1): 109. https://doi.org/10.3390/jcm9010109
Ahmed,
M.J., Murtaza, G. & Ahmed, F. 2024. Antimicrobial activity of phenolic and
flavonoid enriched extracts of Dolomiaea macrocephala (Asteraceae): A
medicinal plant from western Kashmir Himalayas. Pakistan Journal of Botany 56(6): https://doi.org/10.30848/PJB2024-6(2)
Elshamy,
S., Kuhnert, N., El-Shazly, M., Ziemah, J. & Handoussa, H. 2025.
Comparative metabolomic study of twelve Acacia species by
UHPLC-q-TOF-ESI-MS coupled with chemometrics in correlation with antibacterial
activity. Fitoterapia 181: 106378. https://doi.org/10.1016/j.fitote.2025.106378
Eriksson,
L., Johansson, E., Kettaneh-Wold, N. & Wold, S. 2001. Multi- and
Megavariate Data Analysis: Principles and Applications. Umetrics Academy,
Umeå.
Goh, M.P.Y.,
Ahmad, N., Yasin, H.M. & Jama, A.M. 2021. Antioxidant, antibacterial and
cytotoxic activity of the Dillenia suffruticosa leaves against the lung
(A549) and cervical (CaSki) cancer cell lines. Natural Product Journal 12(4): 87-94. https://doi.org/10.2174/2210315510666210203150610
He, Y.,
Jin, L., Sun, F., Hu, Q. & Chen, L. 2016. Antibiotic and heavy-metal
resistance of Vibrio parahaemolyticus isolated from fresh shrimps in
Shanghai fish markets, China. Environmental Science and Pollution Research 23(15): 15033-15040. https://doi.org/10.1007/s11356-016-6614-4
Hu, Q.
& Chen, L. 2016. Virulence and antibiotic and heavy metal resistance of Vibrio
parahaemolyticus isolated from crustaceans and shellfish in Shanghai,
China. Journal of Food Protection 79(8): 1371-1377. https://doi.org/10.4315/0362-028X.JFP-16-031
Indrianingsih,
A.W., Styaningrum, P., Suratno, Windarsih, A., Suryani, R., Noviana, E. &
Itoh, K. 2024. The effect of extraction method on biological activity and
phytochemical content of Artocarpus heterophyllus (jackfruit) leaves
extract concurrent with its principal component analysis. Process
Biochemistry 143: 135-147. https://doi.org/10.1016/j.procbio.2024.04.034
Jayaraman,
S., Rajendhran, N., Kannan, M.A. & Ramasamy, T. 2024. Quercetin disrupts
biofilm formation and attenuates virulence of Aeromonas hydrophila. Archives
of Microbiology 206(7): 326. https://doi.org/10.1007/s00203-024-04034-z
Lawrence,
R., Tripathi, P. & Jeyakumar, E. 2009. Isolation, purification and
evaluation of antibacterial agents from Aloe vera. Brazilian Journal
of Microbiology 40(4): 906-915. https://doi.org/10.1590/S1517-838220090004000023
Martina,
S.M., Cabalquinto, G.P. & Lumogdang, L. 2024. Taxonomic description and
antibacterial activity of Dillenia sp. against Escherichia coli. Biotropia 31(3): 422-431. https://doi.org/10.11598/btb.2024.31.3.2320
Miklasińska-Majdanik,
M., Kępa, M., Wojtyczka, R.D., Idzik, D. & Wąsik, T.J. 2018.
Phenolic compounds diminish antibiotic resistance of Staphylococcus aureus clinical strains. International Journal of Environmental Research and Public
Health 15(10): 2321. https://doi.org/10.3390/ijerph15102321
Ming, D.,
Wang, D., Cao, F., Xiang, H., Mu, D., Cao, J., Li, B., Zhong, L., Dong, X.,
Zhong, X., Wang, L. & Wang, T. 2017. Kaempferol inhibits the primary
attachment phase of biofilm formation in Staphylococcus aureus. Frontiers
in Microbiology 8: 2263. https://doi.org/10.3389/fmicb.2017.02263
Nadirah,
M., Wee, T. & Najiah, M. 2013. Differential responses of Vibrio sp.
to young and mature leaf extracts of Terminalia catappa L. International
Food Research Journal 20: 961-966.
Roy, P.K.,
Park, S.H., Song, M.G. & Park, S.Y. 2022a. Antimicrobial efficacy of
quercetin against Vibrio parahaemolyticus biofilm on food surfaces and
downregulation of virulence genes. Polymers 14(18): 3847. https://doi.org/10.3390/polym14183847
Roy, P.K.,
Song, M.G., Jeon, E.B., Kim, S.H. & Park, S.Y. 2022b. Antibiofilm efficacy
of quercetin against Vibrio parahaemolyticus biofilm on food-contact
surfaces in the food industry. Microorganisms 10(10): 1902. https://doi.org/10.3390/microorganisms10101902
Rukayadi,
Y., Lee, K., Han, S., Yong, D. & Hwang, J.K. 2009. In vitro activities of Panduratin A against clinical Staphylococcus strains. Antimicrobial
Agents and Chemotherapy 53(10): 4529-4532. https://doi.org/10.1128/AAC.00624-09
Saha, S.,
Aggarwal, S. & Singh, D.V. 2023. Attenuation of quorum sensing system and
virulence in Vibrio cholerae by phytomolecules. Frontiers in
Microbiology 14: 1133569. https://doi.org/10.3389/fmicb.2023.1133569
Shah,
M.D., Gnanaraj, C., Khan, M.S. & Iqbal, M. 2015. Dillenia suffruticosa L. impedes carbon tetrachloride-induced hepatic damage by modulating oxidative
stress and inflammatory markers in rats. Journal of Environmental Pathology,
Toxicology and Oncology 34(2): 133-152. https://doi.org/10.1615/jenvironpatholtoxicoloncol.2015013306
Taguri,
T., Tanaka, T. & Kouno, I. 2004. Antimicrobial activity of 10 different
plant polyphenols against bacteria causing food-borne disease. Biological
and Pharmaceutical Bulletin 27(12): 1965-1969. https://doi.org/10.1248/bpb.27.1965
Tan, Z.,
Deng, J., Ye, Q. & Zhang, Z. 2022. The antibacterial activity of
natural-derived flavonoids. Current Topics in Medicinal Chemistry 22(12): 1009-1019. https://doi.org/10.2174/1568026622666220221110506
Tomotake,
H., Koga, T., Yamato, M., Kassu, A. & Ota, F. 2006. Antibacterial activity
of citrus fruit juices against Vibrio species. Journal of Nutritional
Science and Vitaminology 52(2): 157-160. https://doi.org/10.3177/jnsv.52.157
Yakop, F.,
Sheikh Abdul Hamid, M.H., Ahmad, N., Abdul Majid, M., Pillai, M.K. & Taha,
H. 2020. Phytochemical screening, antioxidant and antibacterial activities of
extracts and fractions of Dillenia suffruticosa leaves. Malaysian
Applied Biology 49(1): 121-130. https://doi.org/10.55230/mabjournal.v49i1.1663
Yamanaka,
F., Hatano, T., Ito, H., Taniguchi, S., Takahashi, E. & Okamoto, K. 2008.
Antibacterial effects of guava tannins and related polyphenols on Vibrio and Aeromonas species. Natural Product Communications 3(5): 711-720. https://doi.org/10.1177/1934578X0800300509
Yang, L.,
Yu, P., Wang, J., Zhao, T., Zhao, Y., Pan, Y. & Chen, L. 2024. Genomic and
transcriptomic analyses reveal multiple strategies for Vibrio
parahaemolyticus to tolerate sub-lethal concentrations of three
antibiotics. Foods 13(11): 1674. https://doi.org/10.3390/foods13111674