Author(s):
Neeladhri Karuna Kumari, Pallapati Suman, B. B. V. Sailaja
Email(s):
profsailajabbv@gmail.com
DOI:
10.52711/0974-360X.2026.00155 
Address:
Neeladhri Karuna Kumari1, Pallapati Suman2, B. B. V. Sailaja3*
1Department of Chemistry, Andhra University, Visakhapatnam, 530003, Andhra Pradesh, India.
1Dr Reddy’s Labs, Hyderabad, Telangana, India.
2Department of Chemistry, Andhra University, Visakhapatnam, 530003, Andhra Pradesh, India.
2Laurus Labs Ltd, Visakhapatnam, Andhra Pradesh, India.
3Department of Chemistry, Andhra University, Visakhapatnam, 530003, Andhra Pradesh, India.
*Corresponding Author
Published In:
Volume - 19,
Issue - 3,
Year - 2026
ABSTRACT:
Etoricoxib and its genotoxic impurities were identified using a variety of analytical techniques (UV, HPLC, HPTLC etc.) in accordance with previously published studies. The ICP-MS technique was also used to try and identify the heavy metals in other pharmacological compounds. In light of the lack of an analytical method for heavy metal detection in Etoricoxib, this investigation adopted the ICP-MS technique, incorporating a microwave-assisted acid digestion process to analyze eight elemental impurities: Al, Cd, Hg, Ni, As, Pb, V, and Fe.Heavy metals at the following concentrations were successfully detected by the developed analytical method,which demonstrated both sensitivity and speed:10ppm for aluminum, 0.75ppm for mercury, 0.75ppm for arsenic, 0.25ppm for lead, 0.25ppm for cadmium, 10ppm for iron, 10ppm for nickel, and 5.00ppm for vanadium. Additionally, it showed that it could measure these elemental impurities at concentrations as high as 200percent of the limit. The analytical technique revealed a linear relationship, supported by a correlation coefficient that surpassed 0.99. Recovery rates for heavy metals at three distinct concentrations, after the introduction of Etoricoxib samples, were determined to be within the acceptable limits of 70% to 150%. In terms of precision, the actual percentage RSD is less than 2%. Since ICP-MS heavy metal analysis is an effective technique, the suggested approach can be used to routinely quantitatively determine the eight elemental impurities in Etoricoxib.
Cite this article:
Neeladhri Karuna Kumari, Pallapati Suman, B. B. V. Sailaja. Determination of Elemental Impurities in Etoricoxib a Non-steroidal Anti-inflammatory Drug by using ICP-MS. Research Journal Pharmacy and Technology. 2026;19(3):1091-1. doi: 10.52711/0974-360X.2026.00155
Cite(Electronic):
Neeladhri Karuna Kumari, Pallapati Suman, B. B. V. Sailaja. Determination of Elemental Impurities in Etoricoxib a Non-steroidal Anti-inflammatory Drug by using ICP-MS. Research Journal Pharmacy and Technology. 2026;19(3):1091-1. doi: 10.52711/0974-360X.2026.00155 Available on: https://www.rjptonline.org/AbstractView.aspx?PID=2026-19-3-16
REFERENCES:
1. D.J. Cochrane, B. Jarvis and G.M. Keating. Etoricoxib. Drugs. 2002; 62: 2637–2651. doi: 10.2165/00003495-200262180-00006.
2. P.E. Lipsky, P.Brooks, L.J. Crofford, R. DuBois, D. Graham, L.S. Simon, L.B.van de Putte and S.B. Abramson, Unresolved issues in the role of cyclooxygenase-2 in normal physiologic processes and disease. Arch Intern Med. 2000; 160(7): 913-920. doi:10.1001/archinte.160.7.913.
3. K.F. Croom and M.A Siddiqui, Etoricoxib: a review of its use in the symptomatic treatment of osteoarthritis, rheumatoid arthritis, ankylosing spondylitis and acute gouty arthritis. Drugs.2009; 69(11): 1513-1532. doi:10.2165/00003495-200969110-00008.
4. H.S. Baraf. Efficacy of the newest COX-2 selective inhibitors in rheumatic disease. Current Pharmaceutical Design. 2007; 13(22): 2228-2236. doi: 10.2174/138161207781368819.
5. R.H. Hunt, S. Harper, D.J. Watson,C. Yu, H. Quan, M. Lee,J.K. Evans and B. Oxenius. The gastrointestinal safety of the COX-2 selective inhibitor etoricoxib assessed by both endoscopy and analysis of upper gastrointestinal events. The American Journal of Gastroenterology. 2003; 98(8): 1725–1733. doi: 10.1111/j.1572-0241.2003.07598.x.
6. Shital D. Uparwad, Sonali M. Khapne, Shweta R. Kokare, Gurappa K. Dyade. Chemo Metric Assisted Method Development for the Estimation of Paracetamol, Etoricoxib and Thiocolchicoside in Combined Formulation. Asian Journal of Pharmaceutical Analysis. 2024; 14(3): 51-66. doi: https://doi.org/10.52711/2231-5675.2024.00024.
7. Chaitanya A. Gulhane, Wrushali A. Panchale, Jagdish V. Manwar, Ravindra L. Bakal.Liquid Chromatographic Method for Simultaneous estimation of Thiocolchicoside and Etoricoxib from Tablet formulation. Asian Journal of Pharmaceutical Analysis. 2021; 11(2): 118-122. doi: 10.52711/2231-5675.2021.00020.
8. Indrani Bhattacharyya, Subhra Prakash Bhattacharyya, Subrata Sen and Tapas Ku Laha. Reverse Phase High Performance Liquid Chromatographic Method for the Analysis of Etoricoxib in Pharmaceutical Dosage Form. Asian J. Research Chem. 2009; 2(3): 297-299.
9. Chaple DR and Bhusari KP, Spectrophotometric Methods for the Determination of Etoricoxib in Pharmaceutical Formulations. Research J. Pharm. and Tech. 2009; 2 (3): 597-598.
10. Pratima K. Syal, Madhusmita Sahoo, Dipali M. Mehendre, Snehal S. Ingale. Simultaneous Spectrophotometric Determination of Drotaverine and Etoricoxib in Combined Tablet Dosage Form by Ratio Derivative and Absorption Corrected Method and its Application to Dissolution Study. Research J. Pharm. and Tech. 2011; 4(2): 298-301.
11. Poonam H. Chaube, Santosh V. Gandhi, Padmanabh B. Deshpande and Veena G. Kulkarni. High Performance Thin Layer Chromatographic Analysis of Paracetamol and Etoricoxib in Spiked Human Plasma. Research J. Pharm. and Tech. 2011; 4(8): 1303-1306.
12. Garlapati Manideep, Nazare Lobo John Shane, Girish Pai, Development and Validation of a UV Spectroscopic Method to Estimate Etoricoxib in Bulk and Tablet Formulation. Research J. Pharm. and Tech. 2018; 11(2): 758-760.
13. Nisha kumari, Amit Chaudhary, Kapil Kumar Verma, Kritika Verma, Geetanjali Saini, Manish Vyas, Bhupendra Singh. Development and validation of an analytical method for the simultaneous estimation of Etoricoxib and Thiocolchicoside in tablet dosage form by UV Spectrophotometric method. Research J. Pharm. and Tech. 2022; 15(7): 3051-3056. doi: 10.52711/0974-360X.2022.00510
14. Baheti KG, Shaikh S, Shah N, Dehghan MH. Validated simultaneous estimation of Paracetamol and Etoricoxib in bulk and tablet by HPTLC method. Inter J Res Pharma Biomed Sci. 2011; 2: 672–75.
15. M.J. Rose, N. Agrawal, E.J. Woolf and B.K. Matuszewski, Simultaneous determination of unlabeled and carbon‐13‐labeled etoricoxib, a new cyclooxygenase‐2 inhibitor, in human plasma using HPLC–MS/MS. Journal of Pharmaceutical Sciences. 2002; 91(2): 405-416. doi:10.1002/jps.10038
16. L. Bräutigam, J.U. Nefflen and G. Geisslinger. Determination of etoricoxib in human plasma by liquid chromatography-tandem mass spectrometry with electrospray ionisation. J Chromatogr B Analyt Technol Biomed Life Sci. 2003; 788(2): 309-315. doi:10.1016/s1570-0232(03)00034-5.
17. L.D. Sérgio, S.S Maximiliano da, S. Lucélia Magalhães da, O.M. Rui and B. Thiago, Validation of a capillary zone electrophoresis method for the comparative determination of etoricoxib in pharmaceutical formulations. Journal of Separation Science. 2008; 31: 169. doi: 10.1002/jssc.200700272.
18. B.N. Suhagia, H.M. Patel, S.A. Shah, I.S. Rathod and B.P. Marolia, spectrophotometric-estimation-of-etoricoxib-in-bulk-drug-dosage forms. Ind. J. Pharm.Sci. 2005; 67: 634-639.
19. U. Mandal, D. Senthil, A. Bose, K.V. Gowda, A. Ghose and T.K. Pal, Development and Validation of an HPLC Method for Analysis of Etoricoxib in Human Plasma. Ind. J. Pharma. Sci. 2006; 68(4): 485. doi: 10.4103/0250-474X.27823.
20. R. Hartman, A. Abrahim, A. Clausen, B. Mao, L.S. Crocker, Z. Ge, Development and Validation of an HPLC Method for the Impurity and Quantitative Analysis of Etoricoxib. Journal of Liquid Chromatography and Related Technologies. 2003; 26(15): 2551–2566. doi: 10.1081/JLC-120023800.
21. N.J. Shah, S.J. Shah, D.M. Patel and N.M. Patel, Development and validation of HPTLC method for the estimation of etoricoxib. Ind.. J. Pharm. Edu and Res. 2006; 68: 788. doi: 10.4103/0250-474X.31016.
22. G. Helen. Gika, T. Athina,M. Filippos, T. Georgios, D. Eudoxia, S.Lucas, N. Paul, S. Christopher and D.W. Ian, Determination of two COX-2 inhibitors in serum and synovial fluid of patients with inflammatory arthritis by ultra performance liquid chromatography–inductively coupled plasma mass spectroscopy and quadrupole time-of-flight mass spectrometry. Journal of Pharmaceutical and Biomedical Analysis. 2009; 49(3): 579-586. doi:10.1016/j.jpba.2008.12.006.
23. R. Nageswara Rao, M.V.N. Kumar Talluri.An overview of recent applications of inductively coupled plasma-mass spectrometry (ICP-MS) in determination of inorganic impurities in drugs and pharmaceuticals.Journal of Pharmaceutical and Biomedical Analysis. 2007;4 3(1): 1-13. doi: 10.1016/j.jpba.2006.07.004.
24. Ghantasala Preethi and K. Vinod Kumar. A review on the recent approaches for the analysis of elemental impurities by icp-based techniques. International Journal of Research in Pharmacy and Chemistry. 2021; 11(4): 140-158. doi:https://ijrpc.com/files/12-10-2021/06.pdf.
25. Wilschefski SC, Baxter MR. Inductively Coupled Plasma Mass Spectrometry: Introduction to Analytical Aspects. Clin Biochem Rev. 2019; 40(3): 115-133. doi: 10.33176/AACB-19-00024.
26. Rodushkin I, Engstrom E, Stenberg A, Baxter DC. Determination of low-abundance elements at ultra-trace levels in urine and serum by inductively coupled plasma-sector field mass spectrometry. Anal Bioanal Chem. 2004; 380: 247–57. doi: 10.1007/s00216-004-2742-7.
27. Yatai Li, Wei Guo, Zhiwei Wu, Lanlan Jin, Yiqiu Ke, Qinghai Guo, Shenghong Hu. Determination of ultra-trace rare earth elements in high-salt groundwater using aerosol dilution inductively coupled plasma-mass spectrometry (ICP-MS) after iron hydroxide co-precipitation. Microchemical Journal. 2016; 126: 194-199: doi: https://doi.org/10.1016/j.microc.2015.12.006.
28. Dan Xie, WeiChun Yang, Qin Lu. Method Development and Validation for Simultaneous Determination of 44Ca, 34S, 28Si and 18 Other Trace Elements in Pharmaceutical Packaging Materials’ Extractable Solutions by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Asian Journal of Pharmaceutical Analysis. 10(2): 51-66. doi: https://doi.org/10.5958/2231-5675.2020.00011.3.
29. Ajay Singh Raghuwanshi, Akash Ved, Shikhar Verma. Elemental Impurities Estimation in Adenosine Injection using ICP-MS. Research Journal of Pharmacy and Technology. 2025; 18(3): 1302-7. doi: 10.52711/0974-360X.2025.00189.
30. Suresh P. Kumar KR. Determination of elemental impurities of arsenic, cadmium, mercury, lead and palladium content in testosterone propionate by using ISP-MS. Asian J. Research Chem. 2021; 14(3): 195-2. doi: 10.52711/0974-4150.2021.00035.
31. G. Satish, T. Siva Rao, K. R. Srinivas and P. Suman, Pallapati Suman. Determination of elemental impurities in valproic acid an epilepsy drug by using ICP-MS. Journal of Trace Elements and Minerals. 2022; 2: 100036. doi: 10.1016/j.jtemin.2022.100036.