Simultaneous Electrochemical Determination of Nimesulide and Thiocolchicoside Using a Newly Electro-Activated Glassy Carbon Electrode

Sevilay Erdoğan Kablan; Büşra Uçar; İncilay Süslü; İsmail Murat Palabıyık

doi:10.17776/csj.1825279

Simultaneous Electrochemical Determination of Nimesulide and Thiocolchicoside Using a Newly Electro-Activated Glassy Carbon Electrode

Abstract

Nimesulide represents a well-established non-steroidal anti-inflammatory drug, while thiocolchicoside is extensively utilized as a muscle relaxant for the treatment of acute musculoskeletal pain and spasms. In this study, a new electrochemically activated glassy carbon electrode was designed and applied for the first time for the simultaneous voltammetric determination of nimesulide and thiocolchicoside. The cyclic voltammetry technique was used for electro-activation, with the activation process optimised in terms of the number and type of cycles, potential ranges, and different electrolytes. The surface properties of the glassy carbon electrode were evaluated using electrochemical impedance spectroscopy, cyclic voltammetry, and scanning electron microscopy, both before and after activation. A square wave voltammetric method was developed for the simultaneous quantification of nimesulide and thiocolchicoside in Britton-Robinson buffer solution at pH 7.00. The square wave voltammetric peak currents of nimesulide and thiocolchicoside were linear in the range 1.29-59.9 µM and 16.71-158.89 µM, respectively. The method exhibited detection limits of 0.40 µM (nimesulide) and 5.03 µM (thiocolchicoside). Validation, conducted under International Council for Harmonisation guidelines, confirmed sensitivity, linearity, precision, accuracy, recovery, robustness, and ruggedness. Determining the concentrations of nimesulide and thiocolchicoside in combined tablet formulations proved to be an effective use case for the developed method

Keywords

References

[1] Dey, T., Chatterjee, P., Bhattacharya, A., Pal, S., & Mukherjee, A. K. (2016). Three nimesulide derivatives: Synthesis, ab initio structure determination from powder X-ray diffraction, and quantitative analysis of molecular surface electrostatic potential. Crystal Growth & Design, 16(3), 1442–1452. https://doi.org/10.1021/acs.cgd.5b01476
[2] Tiwaskar, M., Charde, S., Balankhe, N., Hedge, A., Deodhar, M., Gondane, A., Pawar, D., & Sharma, A. (2025). Nimesulide: Critical appraisal of safety and efficacy in acute pain. Journal of the Association of Physicians of India, 73(3).
[3] Suleyman, H., Cadirci, E., Albayrak, A., & Halici, Z. (2008). Nimesulide is a selective COX-2 inhibitory, atypical non-steroidal anti-inflammatory drug. Current Medicinal Chemistry, 15(3), 278–283. https://doi.org/10.2174/092986708783497247
[4] Mustafa, A., Indiran, M. A., Ramalingam, K., Perumal, E., Shanmugham, R., Karobari, M. I., et al. (2024). Anticancer potential of thiocolchicoside and lauric acid loaded chitosan nanogel against oral cancer cell lines: A comprehensive study. Scientific Reports, 14(1), 9270. https://doi.org/10.1038/s41598-024-60123-x
[5] Tok, G., Erdem, Y., Yıldırım, E., Türkyılmaz, A., & Çifter, Ü. (2014). Determination of nimesulide and thiocolchicoside impurities in a topical gel product by UPC2. Chromatography Today, 22–24.
[6] Rajmane, V. S., Gandhi, S. V., Patil, U. P., & Sengar, M. R. (2010). High-performance thin-layer chromatographic determination of etoricoxib and thiocolchicoside in combined tablet dosage form. Journal of AOAC International, 93(3), 783–786. https://doi.org/10.1093/jaoac/93.3.783
[7] Aprile, S., Canavesi, R., Bianchi, M., Grosa, G., & Grosso, E. D. (2017). Development and validation of a stability-indicating HPLC-UV method for the determination of thiocolchicoside and its degradation products. Journal of Pharmaceutical and Biomedical Analysis, 137, 66–71. https://doi.org/10.1016/j.jpba.2017.01.011
[8] Acharjya, S. K., Mallick, P., Panda, P., & Annapurna, M. M. (2010). Spectrophotometric methods for the determination of thiocolchicoside in bulk and pharmaceutical dosage forms. Journal of Pharmaceutical Education and Research, 1(1), 51–56.

[9] Albayrak, M., Demirkaya-Miloglu, F., Senol, O., & Polatdemir, E. (2019). Design, optimization, and validation of chemometrics-assisted spectrophotometric methods for simultaneous determination of etodolac and thiocolchicoside in pharmaceuticals. Journal of Analytical Science and Technology, 10, 1–8. https://doi.org/10.1186/s40543-019-0177-y
[10] Altınöz, S., & Dursun, Ö. Ö. (2000). Determination of nimesulide in pharmaceutical dosage forms by second order derivative UV spectrophotometry. Journal of Pharmaceutical and Biomedical Analysis, 22(1), 175–182. https://doi.org/10.1016/S0731-7085(99)00263-6
[11] Patravale, V. B., D'Souza, S., & Narkar, Y. (2001). HPTLC determination of nimesulide from pharmaceutical dosage forms. Journal of Pharmaceutical and Biomedical Analysis, 25(3-4), 685–688. https://doi.org/10.1016/S0731-7085(00)00588-6
[12] Makukha, O. G., Ivashchenko, L. A., Zaporozhets, O. A., & Doroschuk, V. O. (2019). Cloud point extraction combined with HPLC–MS for the determination of nimesulide in biological samples. Chemical Papers, 73, 693–699. https://doi.org/10.1007/s11696-018-0622-6
[13] Sun, X., Xue, K. L., Jiao, X. Y., Chen, Q., Xu, L., Zheng, H., & Ding, Y. F. (2016). Simultaneous determination of nimesulide and its four possible metabolites in human plasma by LC–MS/MS and its application in a study of pharmacokinetics. Journal of Chromatography B, 1027, 139–148. https://doi.org/10.1016/j.jchromb.2016.05.034
[14] Uslu, B., & Ozkan, S. A. (2011). Electroanalytical methods for the determination of pharmaceuticals: A review of recent trends and developments. Analytical Letters, 44(16), 2644–2702. https://doi.org/10.1080/00032719.2011.551868
[15] Osteryoung, J. G., & Osteryoung, R. A. (1985). Square wave voltammetry. Analytical Chemistry, 57(1), 101–110. https://doi.org/10.1021/ac00279a004
[16] Bukkitgar, S. D., Shetti, N. P., Kulkarni, R. M., Halbhavi, S. B., Wasim, M., Mylar, M., Durgi, P. S., & Chirmure, S. S. (2016). Electrochemical oxidation of nimesulide in aqueous acid solutions based on TiO2 nanostructure modified electrode as a sensor. Journal of Electroanalytical Chemistry, 778, 103–109. https://doi.org/10.1016/j.jelechem.2016.08.016
[17] Shetti, N. P., Malode, S. J., Nayak, D. S., Bukkitgar, S. D., Bagihalli, G. B., Kulkarni, R. M., & Reddy, K. R. (2020). Novel nanoclay-based electrochemical sensor for highly efficient electrochemical sensing nimesulide. Journal of Physics and Chemistry of Solids, 137, 109210. https://doi.org/10.1016/j.jpcs.2019.109210
[18] Govindasamy, M., Mani, V., Chen, S. M., Maiyalagan, T., Selvaraj, S., Chen, T. W., Lee, S. Y., & Chang, W. H. (2017). Highly sensitive determination of non-steroidal anti-inflammatory drug nimesulide using electrochemically reduced graphene oxide nanoribbons. RSC Advances, 7(52), 33043–33051. https://doi.org/10.1039/C7RA04396C
[19] Bukkitgar, S. D., Shetti, N. P., Kulkarni, R. M., & Doddamani, M. R. (2016). Electro-oxidation of nimesulide at 5% barium-doped zinc oxide nanoparticle modified glassy carbon electrode. Journal of Electroanalytical Chemistry, 762, 37–42. https://doi.org/10.1016/j.jelechem.2015.12.016
[20] Shetti, N. P., Malode, S. J., Bukkitgar, S. D., Bagihalli, G. B., Kulkarni, R. M., Pujari, S. B., & Reddy, K. R. (2019). Electro-oxidation and determination of nimesulide at nanosilica modified sensor. Materials Science for Energy Technologies, 2(3), 396–400. https://doi.org/10.1016/j.mset.2019.04.004
[21] Murugan, P., Nagarajan, R. D., Sundramoorthy, A. K., Ganapathy, D., Atchudan, R., Nallaswamy, D., & Khosla, A. (2022). Electrochemical detection of $H_2O_2$ using an activated glassy carbon electrode. ECS Sensors Plus, 1(3), 034401. https://doi.org/10.1149/2752-5309/ac894b
[22] Karim, R., Sayem, M. H., Rahman, M. M., Hossain, M. M., & Hasnat, M. A. (2023). Simultaneous determination of ranitidine and metronidazole at low potential using an acid-activated glassy carbon electrode. ChemSelect, 8(1), e202204174. https://doi.org/10.1002/slct.202204174
[23] International Council for Harmonisation (ICH). (2005). Validation of analytical procedures: Text and methodology Q2 (R1). ICH Steering Committee.
[24] Bond, A. M. (2020). Modern polarographic methods in analytical chemistry. CRC Press.
[25] Furlanetto, S., Orlandini, S., Aldini, G., Gotti, R., Dreassi, E., & Pinzauti, S. (2012). Determination of nimesulide in human serum using a glassy carbon electrode modified with SiC nanoparticles. Microchimica Acta, 176, 493–499. https://doi.org/10.1007/s00604-011-0744-8
[26] Wang, C., Shao, X., Liu, Q., Qu, Q., Yang, G., & Hu, X. (2006). Differential pulse voltammetric determination of nimesulide in pharmaceutical formulation and human serum at glassy carbon electrode modified by cysteic acid/CNTs based on electrochemical oxidation of l-cysteine. Journal of Pharmaceutical and Biomedical Analysis, 42(2), 237–244. https://doi.org/10.1016/j.jpba.2006.03.031
[27] Łysoń, M., Górska, A., Paczosa-Bator, B., & Piech, R. (2021). Nimesulide determination on carbon black-nafion modified glassy carbon electrode by means of adsorptive stripping voltammetry. Electrocatalysis, 12(6), 641–649. https://doi.org/10.1007/s12678-021-00684-x
[28] Santos, A. M., Wong, A., Feitosa, M. H. A., Silva, L. P., Fatibello-Filho, O., & Moraes, F. C. (2022). Using carbon paste electrode modified with graphene and nanodiamond for the determination of nimesulide in biologic and environmental samples. Electroanalysis, 34(9), 1441–1449. https://doi.org/10.1002/elan.202100412
[29] Devarushi, U. S., Shetti, N. P., Malode, S. J., & Tuwar, S. M. (2019). Electro oxidation and analytical applications of nimesulide at graphene oxide and reduced graphene oxide modified carbon paste electrode. Materials Today: Proceedings, 18, 751–758. https://doi.org/10.1016/j.matpr.2019.06.485
[30] Wong, A., Santos, A. M., & Fatibello-Filho, O. (2017). Determination of piroxicam and nimesulide using an electrochemical sensor based on reduced graphene oxide and PEDOT:PSS. Journal of Electroanalytical Chemistry, 799, 547–555. https://doi.org/10.1016/j.jelechem.2017.06.048
[31] Deroco, P. B., Rocha-Filho, R. C., & Fatibello-Filho, O. (2018). A new and simple method for the simultaneous determination of amoxicillin and nimesulide using carbon black within a dihexadecylphosphate film as electrochemical sensor. Talanta, 179, 115–123. https://doi.org/10.1016/j.talanta.2017.10.057
[32] Goularte, R. B., Winiarski, J. P., Latocheski, E., & Jost, C. L. (2022). Novel analytical sensing strategy using a palladium nanomaterial-based electrode for nimesulide electrochemical reduction. Journal of Electroanalytical Chemistry, 920, 116622. https://doi.org/10.1016/j.jelechem.2022.116622
[33] Moscoso, R., Álvarez-Lueje, A., & Squella, J. A. (2020). Nanostructured interfaces containing MWCNT and nitro aromatics: A new tool to determine nimesulide. Microchemical Journal, 159, 105361. https://doi.org/10.1016/j.microc.2020.105361
[34] Rashak, A., & Karam, F. F. (2024). Highly sensitive determination of nimesulide using glassy carbon electrode enhanced graphene oxide-multi-walled carbon nanotubes. Chemical Review and Letters, 7(4), 719–730. https://doi.org/10.22034/CRL.2024.437941.1288
[35] Yue, X., Xu, X., Liu, C., & Zhao, S. (2022). Simultaneous determination of cefotaxime and nimesulide using poly (L-cysteine) and graphene composite modified glassy carbon electrode. Microchemical Journal, 174, 107058. https://doi.org/10.1016/j.microc.2021.107058
[36] Anupriya, J., Babulal, S. M., Chen, T. W., Chen, S. M., Kumar, J. V., Lee, J. W., ... & Yu, H. C. (2021). Facile hydrothermal synthesis of cubic zinc ferrite nanoparticles for electrochemical detection of anti-inflammatory drug nimesulide in biological and pharmaceutical sample. International Journal of Electrochemical Science, 16(7), 210772. https://doi.org/10.20964/2021.07.41
[37] Menon, S., & Kumar, K. G. (2017). Simultaneous voltammetric determination of acetaminophen and its fatal counterpart nimesulide by gold nano/L-cysteine modified gold electrode. Journal of The Electrochemical Society, 164(9), B482. https://doi.org/10.1149/2.0671709jes
[38] Shetti, N. P., Shanbhag, M. M., Malode, S. J., Srivastava, R. K., & Reddy, K. R. (2020). Amberlite XAD-4 modified electrodes for highly sensitive electrochemical determination of nimesulide in human urine. Microchemical Journal, 153, 104389. https://doi.org/10.1016/j.microc.2019.104389
[39] Ağın, F., & Serdaroğlu, V. (2016). Voltammetric determination of nimesulide using multiwalled carbon nanotubes modified carbon paste electrode. Turkish Journal of Pharmaceutical Sciences, 13(3), 335–341. https://doi.org/10.4274/tjps.2016.03
[40] Selcuk, O., Erkmen, C., Bozal-Palabiyik, B., & Uslu, B. (2021). Electroanalytical investigation and simultaneous determination of etodolac and thiocolchicoside at a non-modified glassy carbon electrode in anionic surfactant media. Electroanalysis, 33(5), 1290–1298. https://doi.org/10.1002/elan.202000676
[41] Locatelli, M., Kabir, A., Perrucci, M., Ulusoy, S., Ulusoy, H. I., & Ali, I. (2023). Green profile tools: Current status and future perspectives. Advances in Sample Preparation, 6, 100068. https://doi.org/10.1016/j.sampre.2023.100068
[42] Perrucci, M., De Laurenzi, V., Dainese, E., Locatelli, M., Ulusoy, H. I., Kabir, A., Ali, I., & Mansour, F. R. (2025). Green chemistry and green analytical chemistry. In Green Analytical Chemistry (pp. 1–14). Elsevier. https://doi.org/10.1016/B978-0-443-15954-5.00001-4

Details

Primary Language

English

Subjects

Electroanalytical Chemistry

Journal Section

Research Article

Authors

Sevilay Erdoğan Kablan ^*
0000-0002-6503-0142
Türkiye

Büşra Uçar
0009-0007-0416-1185
Türkiye

İncilay Süslü
0000-0003-0809-2766
Türkiye

İsmail Murat Palabıyık
0000-0003-2843-5690
Türkiye

Publication Date

February 27, 2026

Submission Date

November 17, 2025

Acceptance Date

February 10, 2026

Published in Issue

Year 2026 Volume: 47 Number: 1

DOI

https://doi.org/10.17776/csj.1825279

IZ

https://izlik.org/JA38JE37BF

Cite

RIS / Bibtex

APA

Erdoğan Kablan, S., Uçar, B., Süslü, İ., & Palabıyık, İ. M. (2026). Simultaneous Electrochemical Determination of Nimesulide and Thiocolchicoside Using a Newly Electro-Activated Glassy Carbon Electrode. Cumhuriyet Science Journal, 47(1), 128-138. https://doi.org/10.17776/csj.1825279