Author(s): Ivan O. Surzhikov, Vasyl A. Chornyi, Volodymyr A. Mishchenko, Victoriya A. Georgiyants

Email(s): vgeor@nuph.edu.ua

DOI: 10.52711/0974-360X.2026.00511   

Address: Ivan O. Surzhikov1, Vasyl A. Chornyi1,2, Volodymyr A. Mishchenko1, Victoriya A. Georgiyants1*
1National University of Pharmacy, Kharkiv, Ukraine
2JSC Farmak, Kyiv, Ukraine.
*Corresponding Author

Published In:   Volume - 19,      Issue - 8,     Year - 2026


ABSTRACT:
This study aimed at developing and validating a high-performance liquid chromatography (HPLC) procedure to assay of ibuprofen, caffeine, methylparaben and propylparaben in a fixed-combinated syrup. Method was optimized in terms of the composition of mobile phase, wavelengths of the detection and chromatographic conditions to allow successful resolution of the entire analytes. The chromatographic separation was performed on a Zorbax SB-C18 column (150 × 4.6mm, 5µm) using gradient elution with a mobile phase consisting of potassium dihydrogen phosphate buffer (pH 2.2) and acetonitrile. The flow rate was 1.0mL/min, the column temperature was maintained at 25°C, and detection was carried out at 210nm, 254nm, and 273nm depending on the analyte. Method validation was carried out in compliance with the terms of the State Pharmacopoeia of the Ukraine and ICH Q2(R2), which involved such parameters as specificity, linearity, accuracy, precision, and robustness. This method was very selective and linear in the confidence interval of 70% to a 130 percent concentration; it showed good accuracy (98.0 to 102.0 percent). The procedure was also resistant to slight changes in the analyses, and intra- and inter-day accuracy were found to be within the range of the acceptable (%RSD <2.0). The approach proposed is applicable to the quality control of the multicomponent drug syrups in routine procedures.


Cite this article:
Ivan O. Surzhikov, Vasyl A. Chornyi, Volodymyr A. Mishchenko, Victoriya A. Georgiyants. Simultaneous Determination of Ibuprofen, Caffeine and Preservatives in Combined Sirup. Research Journal of Pharmacy and Technology. 2026;19(8):3617-4. doi: 10.52711/0974-360X.2026.00511

Cite(Electronic):
Ivan O. Surzhikov, Vasyl A. Chornyi, Volodymyr A. Mishchenko, Victoriya A. Georgiyants. Simultaneous Determination of Ibuprofen, Caffeine and Preservatives in Combined Sirup. Research Journal of Pharmacy and Technology. 2026;19(8):3617-4. doi: 10.52711/0974-360X.2026.00511   Available on: https://www.rjptonline.org/AbstractView.aspx?PID=2026-19-8-28


REFERENCES: 
1.    Gonchar A, Sholoiko N. Consumption analysis of two-component fixed combinations of medicines for arterial hypertension treatment in Ukraine as one of the stages for evaluation of their reimbursement prospects. ScienceRise Pharm Sci. 2022; (4(38)): 19–27. Available from: https://journals.uran.ua/sr_pharm/article/view/263733 [cited 2025 Jul 22].
2.    Ruban O, Zupanets I, Kolisnyk T, Shebeko S, Vashchenko O, Zimin S, et al. Pharmacological and biopharmaceutical studies of paracetamol and N-acetyl-D-glucosamine combination as an analgetic drug. ScienceRise Pharm Sci. 2022; (1(35)): 28–36. doi:10.15587/2519-4852.2022.253474.
3.    Tsyvunin V, Shtrygol S, Havrylov I, Shtrygol D, Reus A. SGLT-2 inhibitors as potential anticonvulsants: empagliflozin, but not dapagliflozin, renders a pronounced effect and potentiates the sodium valproate activity in pentylenetetrazole-induced seizures. ScienceRise Pharm Sci. 2022; (5(39)): 83–90. doi:10.15587/2519-4852.2022.266065.
4.    Orlenko D, Yakovenko V, Vyshnevska L. Research on the development of dental gel technology with metronidazole benzoate and hyaluronic acid. ScienceRise Pharm Sci. 2019; (6(22)): 24–29. doi:10.15587/2519-4852.2019.189949.
5.    Wilkins CA, Hamman H, Hamman JH, Steenekamp JH. Fixed-dose combination formulations in solid oral drug therapy: advantages, limitations, and design features. Pharmaceutics. 2024; 16(2): 178. doi:10.3390/pharmaceutics16020178.
6.    Deeks ED. Fixed-dose ibuprofen/famotidine: a review of its use to reduce the risk of gastric and duodenal ulcers in patients requiring NSAID therapy. Clin Drug Investig. 2013 Sep; 33(9): 689–97. doi:10.1007/s40261-013-0113-x.
7.    Bello AE, Kent JD, Grahn AY, Ball J, Holt RJ, et al. One-year open-label safety evaluation of the fixed combination of ibuprofen and famotidine with a prospective analysis of dyspepsia. Curr Med Res Opin. 2015 Mar; 31(3): 397–405. doi:10.1185/03007995.2014.999152.
8.    Uno R, Ohkawa K, Kojima H, Haraguchi T, Ozeki M, Kawasaki I, et al. Masking the taste of fixed-dose combination drugs: particular NSAIDs can efficiently mask the bitterness of famotidine. Chem Pharm Bull (Tokyo). 2023; 71(2): 148–53. doi:10.1248/cpb.c22-00679.
9.    Kushner P, McCarberg BH, Wright WL, Aldoori W, Gao P, Iqbal A, et al. Ibuprofen/acetaminophen fixed-dose combination as an alternative to opioids in management of common pain types. Postgrad Med. 2024 Aug; 136(6): 594–602. doi:10.1080/00325481.2024.2382671.
10.    Castagno E, Parri N, D'Avino A, Ferrari E, Marchisio PG, Messia V, et al. Paracetamol and ibuprofen fixed-dose combination for the management of acute mild-to-moderate pain in children: strengthening and enhancing of result of Nominal Group Technique through Delphi consensus. Ital J Pediatr. 2024 Oct 29; 50(1): 223. doi:10.1186/s13052-024-01791-x.
11.    Parri N, Silvagni D, Chiarugi A, Cortis E, D'Avino A, Lanari M, et al. Paracetamol and ibuprofen combination for the management of acute mild-to-moderate pain in children: expert consensus using the Nominal Group Technique (NGT). Ital J Pediatr. 2023 Mar 21; 49(1): 36. doi:10.1186/s13052-023-01445-4.
12.    Abushanab D, Al-Badriyeh D. Efficacy and safety of ibuprofen plus paracetamol in a fixed-dose combination for acute postoperative pain in adults: meta-analysis and a trial sequential analysis. CNS Drugs. 2021 Jan; 35(1): 105–20. doi:10.1007/s40263-020-00777-7.
13.    Predel HG, Ebel-Bitoun C, Lange R, Weiser T. A randomized, placebo- and active-controlled, multi-country, multi-center parallel group trial to evaluate the efficacy and safety of a fixed-dose combination of 400 mg ibuprofen and 100 mg caffeine compared with ibuprofen 400 mg and placebo in patients with acute lower back or neck pain. J Pain Res. 2019 Sep 23; 12: 2771–83. doi:10.2147/JPR.S217045.
14.    Forderreuther S, Lampert A, Hitier S, Lange R, Weiser T. The impact of baseline pain intensity on the analgesic efficacy of ibuprofen/caffeine in patients with acute postoperative dental pain: post hoc subgroup analysis of a randomised controlled trial. Adv Ther. 2020 Jun; 37(6): 2976–87. doi:10.1007/s12325-020-01297-y.
15.    Obaydo RH, Alhaj Sakur A. A green analytical method using algorithm (PCCA) for extracting components’ contribution from severely overlapped spectral signals in pharmaceutical mixtures. Res J Pharm Technol. 2019; 12(9): 4332-8.
16.    Altinawe YS, Younes OM. Eco-friendly HPLC method for the determination of ranolazine using cyclodextrin as a green additive to mobile phase. Res J Pharm Technol. 2024; 17(3): 1217-20.
17.    Koppuravuri NP, Yenduri S, Varalakshmi HN. Judging the greenness of analytical method using ecological footprints: a green metric approach. Res J Pharm Technol. 2024; 17(12): 6132-6.
18.    Bezruk I, Kotvitska A, Korzh I, Materiienko A, Gubar S, Budanova L, et al. Combined approach to the choice of chromatographic methods for routine determination of hederacoside C in ivy leaf extracts, capsules, and syrup. Sci Pharm. 2020; 88(2): 24. doi:10.3390/scipharm88020024.
19.    Halka L, Kucher T, Kryskiw L, Piponski M, Horyn M, Poliak O, et al. Full green assay of rosuvastatin utilizing sulphophtalein dyes: application to tablet analysis. ScienceRise Pharm Sci. 2024; (4(50)): 4–13. doi:10.15587/2519-4852.2024.310564.
20.    Belikova A, Ivanauskas L, Sidorenko L, Chorny V, Kononenko A, Koval A, et al. Greening of the method for simultaneous determining the enisamium iodide and tilorone dihydrochloride using GC-FID assay. ScienceRise Pharm Sci. 2023; (6(46)): 47–52. doi:10.15587/2519-4852.2023.295120.
21.    Chornyi V, Chorna O, Georgiyants V. Development and validation of the method for simultaneous determination of benzydamine hydrochloride and methylparaben in dosage form by HPLC. ScienceRise Pharm Sci. 2020; (3(25)): 12–19. doi:10.15587/2519-4852.2020.206579.
22.    Sabarwal N, Jain S, Agarwal DD. Development and validation of RP-UPLC method for simultaneous determination of amiloride and hydrochlorothiazide using green assessment in bulk and pharmaceutical dosage form. Res J Pharm Technol. 2025; 18(4): 1837-40.
23.    Verma K, Rastogi S, Dahiya M, Singh GP, Chauhan J, Tomar P, et al. Development and validation of RP-HPLC method using UV detection for simultaneous quantification of amlodipine besylate and nebivolol hydrochloride in fixed-dose combination tablets. Res J Pharm Technol. 2024; 17(2): 523-8
24.    Piponski M, Beneta A, Stefkov G, Cvetkovikj Karanfilova I, Horyn M, Zarivna N, et al. Approaches to the development of new simple rapid HPLC–photodiode array method for the simultaneous determination of levomenthol and ibuprofen in gel pharmaceutical formulation. Sci Synth Chem Pharm. 2025 May 19. doi:10.1002/sscp.70061.
25.    Nguyen Anh Thu. Quantification of acetaminophen, caffeine and ibuprofen in solid dosage forms by UV spectroscopy coupled with multivariate analysis. Asian J Pharm Anal. 2021; 11(2): 127–32.
26.    Chabukswar AR, Thakur VG, Kandale PV, Sharma SN, Kuchekar BS, Sonawane VN. Development and validation of UV-spectrophotometric method for the simultaneous determination of paracetamol, ibuprofen and caffeine in pharmaceutical dosage form. Asian J Res Chem. 2014; 7(12): 1019–22.
27.    Sattar MA, Lakshmi MS, Jyothi DS, Sudha MB, Krishna MKS. Development and validation of a HPLC method for the estimation of tizanidine and ibuprofen in bulk and dosage forms. Asian J Pharm Anal. 2022;12(4):248–52.
28.    Battu PR, Reddy MS. RP-HPLC method for simultaneous estimation of paracetamol and ibuprofen in tablets. Asian J Res Chem. 2009; 2(1): 70–2.
29.    Panchale WA, Suroshe R, Rathod MS, Pandhare YL. Chromatographic analysis of famotidine, paracetamol and ibuprofen from tablet formulation. Res J Pharm Technol. 2019; 12(1): 231–6.
30.    Alqarni M, Shakeel F, Alshehri S, Foudah A, Aljarba T, Abdel Bar F, Alam P. Simultaneous estimation of ibuprofen, caffeine, and paracetamol in commercial products using a green reverse-phase HPTLC method. Green Process Synth. 2024; 13(1): 20230220. doi:10.1515/gps-2023-0220.
31.    Zambakjian C, Sakur AA. A new gas chromatographic method development and validation for the simultaneous determination of ibuprofen and caffeine in bulk and pharmaceutical dosage form. Futur J Pharm Sci. 2020; 6: 110. doi:10.1186/s43094-020-00123-0.
32.    Darkwah EK, Acquah K, Lambon PS, Ameko DK, Akanji O, Ayim JS. Simultaneous quantification of acetaminophen, caffeine, and ibuprofen in fixed dose combination drug using HPLC with UV detection. J Adv Med Pharm Sci. 2019 Apr 3 [cited 2025 Jun 17];20(2):1–19. Available from: https://journaljamps.com/index.php/JAMPS/article/view/370.
33.    State Pharmacopoeia of Ukraine. Vol. 1. Kharkiv: SE “Ukrainian Scientific Pharmacopoeial Center for Quality of Medicines”; 2015. p. 11148.
34.    Validation of Analytical Procedures Q2 (R2) (2023). ICH. Available at: https://database.ich.org/sites/default/files/ICH_Q2%28R2%29_Guideline_2023_1130.pdf Last accessed: 22.07.2025

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