Comparative Analysis of Dexamethasone Adulteration in Herbal Anti-Rheumatic Products Using HPLC, UV-Vis Spectrophotometer, and FTIR Coupled with Chemometrics
Anggita Rosiana Putri(1*), Ni Made Ajeng Gayatri Maitri Paramitha(2), Bachtiar Rifai Pratita Ihsan(3), Mazlina binti Mohd Said(4)
(1) Department of Pharmacy, Faculty of Medicine, Universitas Brawijaya, Jl. Veteran, Malang 65145, Indonesia; Drug Development and Analytical Methods Research Group, Faculty of Medicine, Universitas Brawijaya, Jl. Veteran, Malang 65145, Indonesia
(2) Department of Pharmacy, Faculty of Medicine, Universitas Brawijaya, Jl. Veteran, Malang 65145, Indonesia
(3) Department of Pharmacy, Faculty of Medicine, Universitas Brawijaya, Jl. Veteran, Malang 65145, Indonesia; Drug Development and Analytical Methods Research Group, Faculty of Medicine, Universitas Brawijaya, Jl. Veteran, Malang 65145, Indonesia
(4) Center of Drug and Herbal Research, Faculty of Pharmacy, Universiti Kebangsaan Malaysia, Kuala Lumpur 50300, Malaysia
(*) Corresponding Author
Abstract
Herbal anti-rheumatic products are widely consumed in Indonesia. Despite regulations prohibiting the use of active pharmaceutical ingredients (APIs) in traditional medicines, cases of adulteration are still reported nowadays. This study aimed to evaluate the applicability of high-performance liquid chromatography (HPLC), UV-vis spectrophotometry, and Fourier transform infrared (FTIR) spectroscopy combined with chemometrics analysis for the detection of dexamethasone in herbal anti-rheumatic products from Malang City. All analytical methods were validated and met the required performance criteria. The results showed that none of the analyzed herbal products contained dexamethasone. These findings demonstrate that the developed analytical approaches are reliable for detecting adulteration in herbal preparations and may serve as effective screening tools for routine quality control of herbal products.
Keywords
References
[1] Adnan, A., Navia, Z.I., Silvia, M., Antika, M., Suwardi, A.B., Baihaqi, B., and Yakob, M., 2022, Diversity of herbs and spices plants and their importance in traditional medicine in the South Aceh District, Indonesia, Biodiversitas, 23 (7), 3836–3843.
[2] Tim Riskesdas, 2019, Laporan Nasional Riskesdas 2018, Lembaga Penerbit Badan Penelitian dan Pengembangan Kesehatan, Jakarta, Indonesia.
[3] Lee, E.L., and Barnes, J., 2022, “Prevalence of Use of Herbal and Traditional Medicines” in Pharmacovigilance for Herbal and Traditional Medicines: Advances, Challenges and International Perspectives, Springer International Publishing, Cham, Switzerland, 15–25.
[4] Obahiagbon, E.G., and Ogwu, M.C., 2024, “Consumer Perception and Demand for Sustainable Herbal Medicine Products and Market” in Herbal Medicine Phytochemistry: Applications and Trends, Eds. Izah, S.C., Ogwu, M.C., and Akram, M., Springer International Publishing, Cham, Switzerland, 1919–1952.
[5] Frazaei, M.H., Nouri, R., Arefnezhad, R., Pour, P.M., Naseri, M., and Assar, S., 2024, A review of medicinal plants and phytochemicals for the management of gout, Curr. Rheumatol. Rev., 20 (3), 223–240.
[6] Sharma, A., and Goel, A., 2023, Pathogenesis of rheumatoid arthritis and its treatment with anti-inflammatory natural products, Mol. Biol. Rep., 50 (5), 4687–4706.
[7] Widyowati, R., Pratama, R.R., Sholikhah, I., and Jain, S.K., 2024, “Herbal Medicine and Rheumatic Disorders Management and Prevention” in Herbal Medicine Phytochemistry: Applications and Trends, Eds. Izah, S.C., Ogwu, M.C., and Akram, M., Springer International Publishing, Cham, Switzerland, 723–762.
[8] Rahayu, Y.Y.S., Araki, T., and Rosleine, D., 2020, Factors affecting the use of herbal medicines in the universal health coverage system in Indonesia, J. Ethnopharmacol., 260, 112974.
[9] BPOM, 2022, Peraturan Badan Pengawas Obat dan Makanan Nomor 32 Tahun 2022 tentang Kriteria dan Tata Laksana Registrasi Suplemen Kesehatan, National Agency of Drug and Food Control, Jakarta, Indonesia.
[10] Garza-Ocañas, L., Badillo-Castañeda, C.T., Montoya-Eguía, S.L., Saenz-Chávez, P.L., and Garza-Ulloa, H., 2013, Confirmación de dexametasona y diclofenaco por LC-MS-MS como adulterantes en un producto herbolario, Salud Publica Mex., 55 (5), 498–504.
[11] Pratiwi, R., Rahmawaty, A., and Hasanah, A.N., 2022, Simple analytical method on the determination of dexamethasone in herbal medicine, J. Spectrosc., 2022 (1), 5141647.
[12] Pratiwi, R., Charlie, V., Saptarini, N.M., and Rahayu, D., 2023, A polymer-based indicator for detecting dexamethasone in herbal medicine using polymethylmethacrylate (PMMA), Polymers, 15 (13), 2862.
[13] Saberi, N., Akhgari, M., Bahmanabadi, L., Bazmi, E., and Mousavi, Z., 2018, Determination of synthetic pharmaceutical adulterants in herbal weight gain supplements sold in herb shops, Tehran, Iran, Daru, J. Pharm. Sci., 26 (2), 117–127.
[14] Sadeghi, S., 2024, Investigating the detection of undeclared cyproheptadine in weight gain herbal supplements, creajensing, Int. J. Med. Toxicol. Forensic Med., 14 (2), E43922.
[15] BPOM, 2023, Temuan Obat Tradisional dan Suplemen Kesehatan Mengandung BKO serta Kosmetik Mengandung Bahan Dilarang/Berbahaya Tahun 2023, HM.01.1.2.12.23.50, National Agency of Drug and Food Control, Jakarta, Indonesia.
[16] Gad, A.G., Kelani, K.M., Mahmoud, A.M., and Arafa, R.M., 2025, TLC- smartphone for ofloxacin and dexamethasone determination in pharmaceutical formulation and rabbit aqueous humor, J. Chromatogr. B, 1254, 124485.
[17] Foschi, M., Di Donato, F., Biancolillo, A., D’Emilia, F., Maggi, M.A., and D’Archivio, A.A., 2025, A novel and simple method based on the chemometric treatment of UV–visible spectra of acetonitrile extracts to detect plant-derived adulterants in saffron (Crocus sativus L.), J. Food Compos. Anal., 137, 106973.
[18] Nemati, M., Zayer, A., and Hamidi, S., 2022, Amin-modified graphene oxide as a promising adsorbent for selective extraction of dexamethasone adulterant from herbal supplements, Turk. J. Chem., 46 (5), 1744–1754.
[19] Badulla, W.F., Bamahmood, E.S., and Banafa, S.H., 2024, Spectroscopic screening of dexamethasone and cyproheptadine adulteration in weight gaining products marketed in Aden, Yemen, Addict. Health, 16 (3), 178–187.
[20] Bandara, S.B., Urban, A., Liang, L.G., Parker, J., Fung, E., and Maier, A., 2021, Active pharmaceutical contaminants in dietary supplements: A tier-based risk assessment approach, Regul. Toxicol. Pharmacol., 123, 104955.
[21] Dahabiyeh, L.A., Malkawi, A.K., Wang, X., Colak, D., Mujamammi, A.H., Sabi, E.M., Li, L., Dasouki, M., and Abdel Rahman, A.M., 2020, Dexamethasone-induced perturbations in tissue metabolomics revealed by chemical isotope labeling LC-MS analysis, Metabolites, 10 (2), 42.
[22] Ciobotaru, O.R., Lupu, M.N., Rebegea, L., Ciobotaru, O.C., Duca, O.M., Tatu, A.L., Voinescu, C.D., Stoleriu, G., Earar, K., and Miulescu, M., 2019, Dexamethasone-chemical structure and mechanisms of action in prophylaxis of postoperative side effects, Rev. Chim., 70 (3), 843–847.
[23] Chen, N., Xie, Q.M., Song, S.M., Guo, S.N., Fang, Y., Fei, G.H., and Wu, H.M., 2024, Dexamethasone protects against asthma via regulating Hif-1α-glycolysis-lactate axis and protein lactylation, Int. Immunopharmacol., 131, 111791.
[24] Koning, A.S.C.A.M., Satoer, D.D., Vinkers, C.H., Zamanipoor Najafabadi, A.H., Biermasz, N.R., Nandoe Tewarie, R.D.S., Moojen, W.A., van Rossum, E.F.C., Dirven, C.M.F., Pereira, A.M., and van Furth, W.R., 2021, The DEXA-CORT trial: Study protocol of a randomised placebo-controlled trial of hydrocortisone in patients with brain tumour on the prevention of neuropsychiatric adverse effects caused by perioperative dexamethasone, BMJ Open, 11 (12), e054405.
[25] Soltani, A., Chugaeva, U.Y., Ramadan, M.F., Saleh, E.A.M., Al-Hasnawi, S.S., Romero-Parra, R.M., Alsaalamy, A., Mustafa, Y.F., Zamanian, M.Y., and Golmohammadi, M., 2023, A narrative review of the effects of dexamethasone on traumatic brain injury in clinical and animal studies: focusing on inflammation, Inflammopharmacology, 31 (6), 2955–2971.
[26] Arafa, E.S.A., Elgendy, N.O., Elhemely, M.A., Abdelaleem, E.A., and Mohamed, W.R., 2023, Diosmin mitigates dexamethasone-induced osteoporosis in vivo: Role of Runx2, RANKL/OPG, and oxidative stress, Biomed. Pharmacother., 161, 114461.
[27] Fallo, F., Di Dalmazi, G., Beuschlein, F., Biermasz, N.R., Castinetti, F., Elenkova, A., Fassnacht, M., Isidori, A.M., Kastelan, D., Korbonits, M., Newell-Price, J., Parati, G., Petersenn, S., Pivonello, R., Ragnarsson, O., Tabarin, A., Theodoropoulou, M., Tsagarakis, S., Valassi, E., Witek, P., and Reincke, M., 2022, Diagnosis and management of hypertension in patients with Cushing’s syndrome: a position statement and consensus, J. Hypertens., 40 (11), 2085–2101.
[28] Poludasari, S.K., and Sridevi, C.H., 2022, A case report on multiple adverse events associated with systemic usage of dexamethasone, J. Drug Delivery Ther., 12 (6), I–III.
[29] Fard, H.H., and Akhgari, M., 2018, Analytical perspectives of chemical adulterants in herbal sexual enhancer drugs, J. Pharm. Pharmacogn. Res., 6 (1), 45–53.
[30] Foroughi, M.H., Akhgari, M., Jokar, F., and Mousavi, Z., 2017, Identification of undeclared active pharmaceutical ingredients in counterfeit herbal medicines used as opioid substitution therapy, Aust. J. Forensic Sci., 49 (6), 720–729.
[31] Minh, D.T.C., Thi, L.A., May, N.T., Van Vu, L., Doanh, S.C., Van Chung, H., Phong, N.H., and Thanh Ha, P.T., 2025, Efficient on-site detection of simultaneous adulteration of paracetamol and chlorpheniramine in herbal products using thin-layer chromatography coupled to dynamic surface-enhanced Raman spectroscopy, Sep. Sci. Plus, 8 (5), 70064.
[32] Biancolillo, A., Scappaticci, C., Foschi, M., Rossini, C., and Marini, F., 2023, Coupling of NIR spectroscopy and chemometrics for the quantification of dexamethasone in pharmaceutical formulations, Pharmaceuticals, 16 (2), 309.
[33] Anwar, M.S., Khan, A., Khan, I., Khan, S.A., Ahmad, L., Kaleem, W.A., Mahzari, A., Al-Megrin, W.A.I., Almatroudi, A., Allemailem, K.S., and Khan, F.U., 2023, Evaluation of marketed herbal medicines for the simultaneous estimation of steroidal adulterants using FTIR and RP-HPLC-UV, Microchem. J., 190, 108745.
[34] Attia, K.A.M., El-Olemy, A., Abbas, A.E.F., and Eid, S.M., 2023, A sustainable data processing approach using ultraviolet-spectroscopy as a powerful spectral resolution tool for simultaneously estimating newly approved eye solution in the presence of extremely carcinogenic impurity aided with various greenness and whiteness assessment perspectives: Application to aqueous humor, J. Chem. Res., 47 (5), 17475198231195811.
[35] Rawat, K., Srivastava, A., Tandon, S., and Singh, G.P., 2023, Method validation for simultaneous determination of four neonicotinoids in vegetables by liquid chromatography, Anal. Sci., 39 (4), 431–439.
[36] AOAC, 2013, AOAC Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals, AOAC International, Rockville, MS, US.
[37] Shannon, M., Lafeuille, J.L., Frégière-Salomon, A., Lefevre, S., Galvin-King, P., Haughey, S.A., Burns, D.T., Shen, X., Kapil, A., McGrath, T.F., and Elliott, C.T., 2022, The detection and determination of adulterants in turmeric using Fourier-transform infrared (FTIR) spectroscopy coupled to chemometric analysis and micro-FTIR imaging, Food Control, 139, 109093.
[38] Liu, X., Liu, X., Wang, J., Zang, D., Yang, Y., Chen, Q. and Guo, D.A., 2025, Machine learning and chemometric methods for high-throughput authentication of 53 Root and Rhizome Chinese Herbal using ATR-FTIR fingerprints. J. Chromatogr. B., 1260, 124630.
[39] Liu, Y., Zhang, L., Zhang, X., Bian, X., and Tian, W., 2025, Modern spectroscopic techniques combined with chemometrics for process quality control of traditional Chinese medicine: A review, Microchem. J., 213, 113605.
[40] Nene, R., Pandey, S., Gidwani, B., Pandey, R.K., and Shukla, S.S., 2024, Fourier transform infra-red spectroscopy: Recent advances and prospective in analytical method development and validation, Res. J. Pharm. Technol., 17 (6), 2955–2958.
[41] Windarsih, A., Wijayanti, T., Irnawati, I., and Rohman, A., 2021, The use of 1H-NMR spectroscopy coupled with chemometrics for authentication of Curcuma xanthorrhiza adulterated with Curcuma aeruginosa, Key Eng. Mater., 884, 320–326.
[42] Steidle Neto, A.J., and Lopes, D.C., 2024, Chemometrics coupled with near infrared spectroscopy for detecting adulteration levels in herbal teas, J. Food Compos. Anal., 135, 106637.
[43] Fatmarahmi, D.C., Susidarti, R.A., Swasono, R.T., and Rohman, A., 2022, Application of FTIR-ATR spectroscopy in combination with multivariate analysis to analyze synthetic drugs adulterant in ternary mixtures of herbal medicine products, Indones. J. Pharm., 33 (1), 63–71.
[44] Putri, N.K.T.W., Putri, A.R., and Ihsan, B.R.P., 2026, Response surface methodology–based optimization of HPLC conditions for quantification of paracetamol in Indonesian traditional medicines (jamu), Malays. J. Sci., 45 (1), 33–44.
[45] Peikova, L., Tzankova, D., Smerikarova, M., Balkanski, S., and Zlatkov, A., 2022, Development of RP-HPLC methods for the analysis of Dexamethasone and Levofloxacin alone and in combinations used in the therapy of Covid-19, Pharmacia, 69 (4), 1075–1080.
[46] Shi, T., Zhu, M., Chen, Y., Yan, X., Chen, Q., Wu, X., Lin, J., and Xie, M., 2018, 1H NMR combined with chemometrics for the rapid detection of adulteration in camellia oils, Food Chem., 242, 308–315.
[47] Calle, J.L.P., Ferreiro-González, M., Ruiz-Rodríguez, A., Barbero, G.F., Álvarez, J.Á., Palma, M., and Ayuso, J., 2021, A methodology based on FT-IR data combined with random forest model to generate spectralprints for the characterization of high-quality vinegars, Foods, 10 (6), 1411.
Article Metrics
Copyright (c) 2026 Indonesian Journal of Chemistry

This work is licensed under a Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.
Indonesian Journal of Chemistry (ISSN 1411-9420 /e-ISSN 2460-1578) - Chemistry Department, Universitas Gadjah Mada, Indonesia.












