Author(s):
Zaineb Z. Abduljaleel, Khalid K. Al-Kinani
Email(s):
zainab.abd2200@copharm.uobaghdad.edu.iq
DOI:
10.52711/0974-360X.2025.00625
Address:
Zaineb Z. Abduljaleel1,2*, Khalid K. Al-Kinani2
1Ministry of Health, Karbala Health Directorate, Karbala, Iraq.
2Department of Pharmaceutics, College of Pharmacy, University of Baghdad, Baghdad, Iraq.
*Corresponding Author
Published In:
Volume - 18,
Issue - 9,
Year - 2025
ABSTRACT:
A simple, sensitive, and robust spectrophotometric method was developed and validated for the quantification of acemetacin in phosphate buffer pH 6.8 and ethanol. Linearity was achieved in the range of 5–55µg/mL with regression coefficient 0.9996 for phosphate buffer and 0.9996 for ethanol. The method demonstrated low limits of detection and quantification, which were 0.29µg/mL and 0.89µg/mL for phosphate buffer, and 1.248µg/mL and 3.78µg/mL for ethanol, respectively. Accuracy studies revealed mean recoveries of 97.65%–103.68% in phosphate buffer and 96.52%–101.68% in ethanol, with relative standard deviations below 0.78%, ensuring method reliability. Precision assessments, including intraday and interday studies, confirmed the reproducibility of the method with RSD values <3%, in compliance with FDA and ICH guidelines. The excellent sensitivity, accuracy, and precision of the proposed method make it a valuable tool for the reliable determination of acemetacin in both buffer- and ethanol-based analytical systems.
Cite this article:
Zaineb Z. Abduljaleel, Khalid K. Al-Kinani. Development and Validation of UV Spectrophotometric Method for The Determination of Acemetacin. Research Journal of Pharmacy and Technology. 2025;18(9):4363-8. doi: 10.52711/0974-360X.2025.00625
Cite(Electronic):
Zaineb Z. Abduljaleel, Khalid K. Al-Kinani. Development and Validation of UV Spectrophotometric Method for The Determination of Acemetacin. Research Journal of Pharmacy and Technology. 2025;18(9):4363-8. doi: 10.52711/0974-360X.2025.00625 Available on: https://www.rjptonline.org/AbstractView.aspx?PID=2025-18-9-45
REFERENCE:
1. Aputen AD, Elias MG, Gilbert J, et al. Versatile platinum (iv) prodrugs of naproxen and acemetacin as chemo-anti-inflammatory agents. Cancers. 2023; 15(9): 2460. https://doi.org/10.3390/cancers15092460
2. Çağlar EŞ, Okur ME, Aksu B, Ustündağ Okur N. Transdermal delivery of acemetacin loaded microemulsions: preparation, characterization, in vitro–ex vivo evaluation and in vivo analgesic and anti-inflammatory efficacy. Journal of Dispersion Science and Technology. 2024; 45(4): 662-672. https://doi.org/10.1080/01932691.2023.2175691
3. Ribeiro H, Rodrigues I, Napoleão L, et al. Non-steroidal anti-inflammatory drugs (NSAIDs), pain and aging: Adjusting prescription to patient features. Biomedicine and Pharmacotherapy. 2022; 150: 112958. https://doi.org/10.1016/j.biopha.2022.112958
4. Teng M, Li J, Li Z, Zhang G, Zhao P, Fu Q. Recrystallization mediates the gelation of amorphous drugs: The case of acemetacin. Pharmaceutics. 2023; 15(1): 219. https://doi.org/10.3390/pharmaceutics15010219
5. Sabri LA, Hussein AA. Comparison between conventional and supersaturable self-nanoemulsion loaded with nebivolol: preparation and in-vitro/ex-vivo evaluation. Iraqi J Pharm Sci. 2020; 29(1): 216-225. https://doi.org/10.31351/vol29iss1pp216-225
6. Hou J, Zhao P, Wang Y, Jiang X, Fu Q. Co-Amorphization of Acemetacin with Basic Amino Acids as Co-Formers for Solubility Improvement and Gastric Ulcer Mitigation. Pharmaceutics. 2024; 16(6): 745. https://doi.org/10.3390/pharmaceutics16060745
7. Zouvelekis D, Yannakopoulou K, Mavridis IM, Antoniadou-Vyza E. The self-association of the drug acemetacin and its interactions and stabilization with β-cyclodextrin in aqueous solution as inferred from NMR spectroscopy and HPLC studies. Carbohydrate research. 2002; 337(15): 1387-1395. https://doi.org/10.1016/S0008-6215(02)00174-X
8. Shehata TM, Abdallah MH, Ibrahim MM. Proniosomal oral tablets for controlled delivery and enhanced pharmacokinetic properties of acemetacin. AAPS PharmSciTech. 2015; 16: 375-383. https://doi.org/10.1208/s12249-014-0233-5
9. Abdul Aziz BI, Rajab NA. Preparation and in-vitro evaluation of mucoadhesive clotrimazole vaginal hydrogel. Iraqi J Pharm Sci. 2017; 23: 1. https://doi.org/10.31351/vol23iss1pp19-25
10. Jaafer H, Al-Kinani KK. Formulation and Evaluation of Idebenone Microemulsion as a Potential Approach for the Transmucosal Drug Delivery Systems. Iraqi Journal of Pharmaceutical Sciences (P-ISSN 1683-3597 E-ISSN 2521-3512). 2024; 33(1): 79-88. https://doi.org/10.31351/vol33iss1pp79-88
11. Gupta A, Pathak S. Assessment of Analytical Techniques for Precise Quantification of Four Antiviral Drugs in Pharmaceutical Research and Development: A Comprehensive Review. Current Pharmaceutical Analysis. 2024; 20(6): 409-424. https://doi.org/10.2174/0115734129302705240703052227
12. Mansour FR, Abdallah IA, Bedair A, Hamed M. Analytical methods for the determination of quercetin and quercetin glycosides in pharmaceuticals and biological Samples. Critical Reviews in Analytical Chemistry. 2023: 1-26. https://doi.org/10.1080/10408347.2023.2269421
13. Gardouh AR, Srag El-Din ASG, Salem MSH, Moustafa Y, Gad S. Starch Nanoparticles for Enhancement of Oral Bioavailability of a Newly Synthesized Thienopyrimidine Derivative with Anti-Proliferative Activity Against Pancreatic Cancer. Drug Des Devel Ther. 2021/07/16 2021; 15(null): 3071-3093. https://doi.org/10.2147/DDDT.S321962
14. Anandakumar K, Varadharajan K, Rao TAP, Sujatha K. Estimation of Balsalazide in bulk and in formulation by UV-Visible spectrophotometry. Research Journal of Pharmacy and Technology. 2008; 1(4): 472-474.
15. Ala Allah AK, Abd Alhammid SN. Preparation and characterization of azelnidipine-loaded D-α-tocopheryl polyethylene glycol succinate (TPGS)/solutol micelles. Article. Review of Clinical Pharmacology and Pharmacokinetics, International Edition. 2024; 38: 51-54. https://doi.org/10.61873/JYHN9753
16. Al-Tamimi D, Al-Kinani K, Taher S, Hussein A. Effect of Food on the Pharmacokinetics of Fluoxetine in Healthy Male Adult Volunteers(Conference Paper )#. Iraqi Journal of Pharmaceutical Sciences. 02/18 2023; 31(Suppl.): 153-161. https://doi.org/10.31351/vol31issSuppl.pp153-161
17. Ramadhan SH, Al-Kinani KK. Statistical Optimization and Characterization of Nimodipine Transferosomes. Al-Rafidain Journal of Medical Sciences . 2024; 9(14) 7(1(Special)):S77-83. https://doi.org/10.54133/ajms.v7i1(Special).1015
18. Khudhair AS, Abdalkarim Sabri L. Preparation and evaluation of topical hydrogel containing ketoconazole-loaded bilosomes. Article. Acta Pharmaceutica Sciencia. 2024; 62(4): 762-777. https://doi.org/10.23893/1307-2080.aps6250
19. Pattanayak P, Chaudury YP, Sharma R, Mohapatra P, Setty DK. Simultaneous spectrophotometric estimation of Nitazoxanide and Ofloxacin in combained tablet dosage form. Research Journal of Pharmacy and Technology. 2009; 2(2): 291-293.
20. Srag El-Din AS. Azithromycin loaded chitosan nanoparticles preparation and in-vitro characterization. Delta University Scientific Journal. 2022; 5(2)
21. Karthikeyan R, Thangabalan B, Prabahar AE, Kumar PV. New Spectrophotometric Methods for the Determination of Imatinib in Bulk Drug and in Pharmaceutical Formulations. Research Journal of Pharmacy and Technology. 2009; 2(3): 578-581.
22. Al-Jarsha HYM, Ghareeb MM. Validation of UV-visible spectrophotometric method for niclosamide in different media. Article. Tropical Journal of Pharmaceutical Research. 2024; 23(5): 871-880. http://dx.doi.org/10.4314/tjpr.v23i5.9
23. Abd-Alhammid SN, Saleeh HH. Formulation and evaluation of flurbiprofen oral film. Iraqi J Pharm Sci. 2014; 23(1): 53-59. https://doi.org/10.31351/vol23iss1pp53-59
24. Alhajjeh R, Al-Ali H. Application of FTIR Spectroscopy method for The Quantification of Ascorbic Acid in Bulk Materials and Pharmaceutical Formulation. Iraqi Journal of Pharmaceutical Sciences. 2023; 32(3): 186-194. https://doi.org/10.31351/vol32iss3pp186-194
25. Guideline IHT. Validation of analytical procedures: text and methodology. Q2 (R1). 2005; 1: 1-15.
26. Bhavna, Ojha A, Bhargava S. Chapter 3 - International Council for Harmonisation (ICH) guidelines. In: Ali J, Baboota S, eds. Regulatory Affairs in the Pharmaceutical Industry. Academic Press; 2022: 47-74.
27. Abed HN, Hussein AA. Ex-vivo absorption study of a novel dabigatran etexilate loaded nanostructured lipid carrier using non-everted intestinal SAC model. Iraqi J Pharm Sci. 2019; 28(2): 37-45. https://doi.org/10.31351/vol28iss2pp37-45
28. Rapalli VK, Kaul V, Gorantla S, et al. UV Spectrophotometric method for characterization of curcumin loaded nanostructured lipid nanocarriers in simulated conditions: Method development, in-vitro and ex-vivo applications in topical delivery. Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy. 2020; 224: 117392. https://doi.org/10.1016/j.saa.2019.117392
29. Prabahar AE, Kalaichelvi R, Thangabalan B, Karthikeyan R, Prabhakar C, Kumar PV. Validated spectroscopic method for estimation of sumatriptan succinate in pure and from tablet formulation. Research Journal of Pharmacy and Technology. 2009; 2(3): 495-497.
30. Chaudhary A, Singh A, Verma PK. Method development and validation of potent pyrimidine derivative by UV-VIS spectrophotometer. Organic and Medicinal Chemistry Letters. 2014; 4(1): 1-6.
31. Nanda R, Gaikwad J, Prakash A. Simultaneous spectrophotometric estimation of tolterodine in pharmaceutical dosage form. Research Journal of Pharmacy and Technology. 2009; 2(2): 312-314.
32. Hadi H, Mouayed M. Spectrophotometric Determination of Nitrofurantoin Drug in its Pharmaceutical Formulations Using MBTH as a Coupling Reagent. Iraqi Journal of Pharmaceutical Sciences. 2016: 7-14. https://doi.org/10.31351/vol25iss2pp7-14
33. Darweesh SA. Spectrophotometric Determination of Cefixime Following Simple Diazotization and Coupling with?-Naphthol. Iraqi Journal of Pharmaceutical Sciences. 2017: 1-6. https://doi.org/10.31351/vol26iss2pp1-6
34. Ahmed MJ. Spectrophotometric Determination of Chlordiazepoxide in Pharmaceutical Formulations via Oxidative Coupling Reaction with Phenothiazine. Iraqi Journal of Pharmaceutical Sciences. 2018: 7-14. https://doi.org/10.31351/vol27iss2pp7-14
35. Singh R, Saraf S. Spectrophotometric Estimation of Omeprazole in Pharmaceutical Dosage Form. Research Journal of Pharmacy and Technology. 2008; 1(3): 276-277.
36. Sable P, Chaulang G, Bhosale A, Chaudhari P. Novel spectrophotometric estimation of olanzepine using hydrotropic solubilizing agents. Research Journal of Pharmacy and Technology. 2009; 2(2): 297-300.
37. Riley CM, Nguyen KL. Specification of drug substances and products: development and validation of analytical methods. Elsevier. 2024.
38. Skoog DA, Holler FJ, Crouch SR. Textbook, Principles of Instrumental Analysis. Cengage Learning Core ac Uk https://core ac Uk/download/pdf/232277508 pdf. 2019;
39. Pillai S, Singhvi I, Kar M. Simultaneous Estimation of Atorvastatin calcium and Nicotinic acid from Tablet Formulation. Research Journal of Pharmacy and Technology. 2008; 1(2): 83-85.
40. Gardouh AR, El-Din ASS, Mostafa Y, Gad S. Starch Nanoparticles Preparation and Characterization by in situ combination of Sono-precipitation and Alkali hydrolysis under Ambient Temperature. Research Journal of Pharmacy and Technology. 2021; 14(7): 3543-3552.
41. Kakde R, Kotak V, Barsagade A, Chaudhary N, Kale D. Spectrophotometric method for simultaneous estimation of amlodipine besylate and bisoprolol fumarate in pharmaceutical preparations. Research Journal of Pharmacy and Technology. 2008; 1(4): 513-515.
42. Radhi ZA, Ghareeb MM. Preparation and evaluation of extended release ocular inserts of rebamipide for local effect using casting technique. Iraqi J Pharm Sci. 2018; 28: 24-36. https://doi.org/10.31351/vol28iss1pp24-36
43. Valarmathy J, Samueljoshua L, Rathinavel G, Thanuja CS, Sivakumar T. RP-HPLC Method development and validation for assay of Levetiracetam in tablet dosage Form. Research Journal of Pharmacy and Technology. 2008; 1(4): 395-397.
44. Shabir GA. Validation of high-performance liquid chromatography methods for pharmaceutical analysis: Understanding the differences and similarities between validation requirements of the US Food and Drug Administration, the US Pharmacopeia and the International Conference on Harmonization. Journal of Chromatography A. 2003/02/14/ 2003; 987(1): 57-66. https://doi.org/10.1016/S0021-9673(02)01536-4