{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,6,24]],"date-time":"2026-06-24T13:51:34Z","timestamp":1782309094542,"version":"3.54.5"},"reference-count":26,"publisher":"Walter de Gruyter GmbH","issue":"4","license":[{"start":{"date-parts":[[2025,12,1]],"date-time":"2025-12-01T00:00:00Z","timestamp":1764547200000},"content-version":"unspecified","delay-in-days":0,"URL":"http:\/\/creativecommons.org\/licenses\/by-nc-nd\/4.0"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":[],"published-print":{"date-parts":[[2025,12,1]]},"abstract":"<jats:title>Abstract<\/jats:title>\n                  <jats:p>Glucocorticoids are a group of drugs increasingly used in modern medical practice due to their pronounced anti--inflammatory and immunosuppressive properties. In this study, prednisolone disodium phosphate and prednisolone acetate were analysed, with the aim of developing and validating an HPLC method in accordance with ICH Q2(R2) guidelines and quantifying their content in the active pharmaceutical ingredient powder and a model in--house sample. By applying the HPLC-DAD method with gradient elution, effective separation of the analytes was achieved. The method met all validation parameter requirements. The obtained results showed that the content of both analytes in the tested samples (bulk API powders and in-house prepared model formulation) was within the prescribed limits according to current pharmacopoeial standards. The proposed HPLC-DAD method was assessed for its applicability and environmental profile utilizing a range of green and blue metric tools. This comprehensive evaluation confirms that the method adheres to green analytical principles, making it suitable for sustainable pharmaceutical analysis.<\/jats:p>","DOI":"10.2478\/acph-2025-0032","type":"journal-article","created":{"date-parts":[[2026,1,13]],"date-time":"2026-01-13T11:03:29Z","timestamp":1768302209000},"page":"577-595","source":"Crossref","is-referenced-by-count":0,"title":["Application of green analytical principles in the HPLC analysis of prednisolone derivatives: Method optimization and validation for nasal powder formulations"],"prefix":"10.2478","volume":"75","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-1695-6950","authenticated-orcid":false,"given":"Daniela Amid\u017ei\u0107","family":"Klari\u0107","sequence":"first","affiliation":[{"name":"University of Zagreb Faculty of Pharmacy and Biochemistry , Department of Pharmaceutical Analysis , Zagreb , Croatia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6634-6130","authenticated-orcid":false,"given":"Jelena","family":"Kova\u010di\u0107","sequence":"additional","affiliation":[{"name":"University of Zagreb Faculty of Pharmacy and Biochemistry , Department of Pharmaceutical Analysis , Zagreb , Croatia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9892-6674","authenticated-orcid":false,"given":"Ilija","family":"Klari\u0107","sequence":"additional","affiliation":[{"name":"Public Health Br\u010dko DC , Br\u010dko Bosnia and Herzegovina"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0003-4950-8454","authenticated-orcid":false,"given":"Petra","family":"Bajt","sequence":"additional","affiliation":[{"name":"University of Zagreb Faculty of Pharmacy and Biochemistry , Center for Translational Research and Innovation in Pharmacy , Zagreb , Croatia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Lana","family":"Pribol\u0161an","sequence":"additional","affiliation":[{"name":"University of Zagreb Faculty of Pharmacy and Biochemistry , Department of Pharmaceutical Analysis , Zagreb , Croatia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Erika","family":"Kri\u017eani\u0107","sequence":"additional","affiliation":[{"name":"University of Zagreb Faculty of Pharmacy and Biochemistry , Department of Pharmaceutical Technology , Zagreb , Croatia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8139-5803","authenticated-orcid":false,"given":"Laura Ni\u017ei\u0107","family":"Nodilo","sequence":"additional","affiliation":[{"name":"University of Zagreb Faculty of Pharmacy and Biochemistry , Department of Pharmaceutical Technology , Zagreb , Croatia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3944-697X","authenticated-orcid":false,"given":"Ana","family":"Mornar","sequence":"additional","affiliation":[{"name":"University of Zagreb Faculty of Pharmacy and Biochemistry , Department of Pharmaceutical Analysis , Zagreb , Croatia"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"374","published-online":{"date-parts":[[2026,1,13]]},"reference":[{"key":"2026062413321717503_j_acph-2025-0032_ref_001","doi-asserted-by":"crossref","unstructured":"D. M. Williams, Clinical pharmacology of corticosteroids, Respircare 63(6) (2018) 655\u2013670; https:\/\/doi.org\/10.4187\/respcare.06314","DOI":"10.4187\/respcare.06314"},{"key":"2026062413321717503_j_acph-2025-0032_ref_002","doi-asserted-by":"crossref","unstructured":"T. K. Bergmann, K. A. Barraclough, K. J. Lee and C. E. Staatz, Clinical pharmacokinetics and pharmacodynamics of prednisolone and prednisone in solid organ transplantation, Clin. Pharmacokinet. 51 (2012) 711\u2013741; https:\/\/doi.org\/10.1007\/s40262-012-0007-8","DOI":"10.1007\/s40262-012-0007-8"},{"key":"2026062413321717503_j_acph-2025-0032_ref_003","doi-asserted-by":"crossref","unstructured":"I. S\u00e6ves, P. D. Line and S. Bergan, The pharmacokinetics of prednisolone and prednisone in adult liver transplant recipients early after transplantation, Ther. Drug Monit. 34(4) (2012) 452\u2013459; https:\/\/doi.org\/10.1097\/FTD.0b013e31825ee3f8","DOI":"10.1097\/FTD.0b013e31825ee3f8"},{"key":"2026062413321717503_j_acph-2025-0032_ref_004","doi-asserted-by":"crossref","unstructured":"S. A. Gaballa, U. B. Kompella, O. Elgarhy, A. M. Alqahtani, B. Pierscionek, R. G. Alany and H. Abdelkader, Corticosteroids in ophthalmology: Drug delivery innovations, pharmacology, clinical applications, and future perspectives, Drug Deliv. Transl. Res. 11 (2021) 866\u2013893; https:\/\/doi.org\/10.1007\/s13346-020-00843-z","DOI":"10.1007\/s13346-020-00843-z"},{"key":"2026062413321717503_j_acph-2025-0032_ref_005","doi-asserted-by":"crossref","unstructured":"L. Ni\u017ei\u0107, I. Ugrina, D. \u0160poljari\u0107, V. Sar\u0161on, M. S. Ku\u010duk, I. Pepi\u0107 and A. Hafner, Innovative sprayable in situ gelling fluticsone suspension: Development and optimization of nasal deposition, Int. J. Pharm. 563 (2019) 445\u2013456; https:\/\/doi.org\/10.1016\/j.ijpharm.2019.04.015","DOI":"10.1016\/j.ijpharm.2019.04.015"},{"key":"2026062413321717503_j_acph-2025-0032_ref_006","doi-asserted-by":"crossref","unstructured":"L. Ni\u017ei\u0107 Nodilo, I. Ugrina, D. \u0160poljari\u0107, D. Amid\u017ei\u0107 Klari\u0107, C. Jakobu\u0161i\u0107 Brala, M. Perku\u0161i\u0107, I. Pepi\u0107, J. Lovri\u0107, V. Sar\u0161on, M. Safund\u017ei\u0107 Ku\u010duk, D. Zadravec, L. Kalogjera and A. Hafner, A dry powder platform for nose-to-brain delivery of dexamethasone: Formulation development and nasal deposition studies, Pharmaceutics 13(6) (2021) Article ID 795 (30 pages); https:\/\/doi.org\/10.3390\/pharmaceutics13060795","DOI":"10.3390\/pharmaceutics13060795"},{"key":"2026062413321717503_j_acph-2025-0032_ref_007","doi-asserted-by":"crossref","unstructured":"L. Ni\u017ei\u0107 Nodilo, M. Perku\u0161i\u0107, I. Ugrina, D. \u0160poljari\u0107, C. Jakobu\u0161i\u0107 Brala, D. Amid\u017ei\u0107 Klari\u0107, J. Lovri\u0107, V. Sar\u0161on, M. Safund\u017ei\u0107 Ku\u010duk, D. Zadravec, L. Kalogjera, I. Pepi\u0107 and A. Hafner, In situ gelling nanosuspension as an advanced platform for fluticasone propionate nasal delivery, Eur. J. Pharm. Biopharm. 175 (2022) 27\u201342; https:\/\/doi.org\/10.1016\/j.ejpb.2022.04.009","DOI":"10.1016\/j.ejpb.2022.04.009"},{"key":"2026062413321717503_j_acph-2025-0032_ref_008","doi-asserted-by":"crossref","unstructured":"M. Perku\u0161i\u0107, L. Ni\u017ei\u0107 Nodilo, I. Ugrina, D. \u0160poljari\u0107, C. Jakobu\u0161i\u0107 Brala, I. Pepi\u0107, J. Lovri\u0107, G. Matija\u0161i\u0107, M. Greti\u0107, D. Zadravec, L. Kalogjera and A. Hafner, Tailoring functional spray-dried powder platform for efficient donepezil nose-to-brain delivery, Int. J. Pharm. 624 (2022) Article ID 122038 (15 pages); https:\/\/doi.org\/10.1016\/j.ijpharm.2022.122038","DOI":"10.1016\/j.ijpharm.2022.122038"},{"key":"2026062413321717503_j_acph-2025-0032_ref_009","unstructured":"R. Kashyap, E. V. S. Subrahmanyam and A. R. Sharbaraya, Development and validation of UV spectroscopy method for the estimation of prednisolone in bulk and dosage form, J. Chem. Pharm. Res. 4(2) (2012) 1090\u20131096."},{"key":"2026062413321717503_j_acph-2025-0032_ref_010","doi-asserted-by":"crossref","unstructured":"S. Mazurek and R. Szostak, Quantitative determination of prednisone in tablets by infrared attenuated total reflection and Raman spectroscopy, J. AOAC Int. 95(3) (2012) 744\u2013750; https:\/\/doi.org\/10.5740\/jaoacint.sge_mazurek","DOI":"10.5740\/jaoacint.SGE_Mazurek"},{"key":"2026062413321717503_j_acph-2025-0032_ref_011","unstructured":"European Pharmacopoeia, 11th ed., European Directorate for the Quality of Medicines & Health-Care, Strasbourg 2022; last access date September 1, 2024."},{"key":"2026062413321717503_j_acph-2025-0032_ref_012","doi-asserted-by":"crossref","unstructured":"V. K. Prasad, B. Ho and C. Haneke, Simultaneous determination of prednisolone acetate, prednisolone, prednisone, cortisone and hydrocortisone in swine plasma using solid-phase and liquid--liquid extraction techniques, J. Chromatogr. B: Biomed. Sci. Appl. 378 (2016) 305\u2013316; https:\/\/doi.org\/10.1016\/S0378-4347(00)80727-6","DOI":"10.1016\/S0378-4347(00)80727-6"},{"key":"2026062413321717503_j_acph-2025-0032_ref_013","doi-asserted-by":"crossref","unstructured":"N. S. Abdelhamid, M. A. Magdy, B. H. Anwar and N. F. Farid, US FDA-validated TLC method with four greenness assessment evaluations for simultaneous determination of prednisolone and esomeprazole in spiked human plasma, Biomed. Chromatogr. 36(5) (2022) e5343; https:\/\/doi.org\/10.1002\/bmc.5343","DOI":"10.1002\/bmc.5343"},{"key":"2026062413321717503_j_acph-2025-0032_ref_014","doi-asserted-by":"crossref","unstructured":"I. A. Ionita, D. M. Fast and F. Akhlaghi, Development of a sensitive and selective method for the quantitative analysis of cortisol, cortisone, prednisolone and prednisone in human plasma, J. Chromatogr. B 877(8\u20139) (2009) 765\u2013772; https:\/\/doi.org\/10.1016\/j.jchromb.2009.02.019","DOI":"10.1016\/j.jchromb.2009.02.019"},{"key":"2026062413321717503_j_acph-2025-0032_ref_015","doi-asserted-by":"crossref","unstructured":"H. Shibasaki, H. Nakayama, T. Furuta, Y. Kasuya, M. Tsuchiya, A. Soejima, A. Yamada and T. Nagasawa, Simultaneous determination of prednisolone, prednisone, cortisol, and cortisone in plasma by GC-MS: Estimating unbound prednisolone concentration in patients with nephrotic syndrome during oral prednisolone therapy, J. Chromatogr. B 870(2) (2008) 164\u2013169; https:\/\/doi.org\/10.1016\/j.jchromb.2008.03.003","DOI":"10.1016\/j.jchromb.2008.03.003"},{"key":"2026062413321717503_j_acph-2025-0032_ref_016","doi-asserted-by":"crossref","unstructured":"M. Fin\u0161gar, A. Perva-Uzunali\u0107, H. Behr, N. Ledinek, Z. Knez and Z. Novak, An improved reversed-phase high-performance liquid chromatography method for the analysis of related substances of prednisolone in active ingredient, ACS Omega 5(14) (2020) 7987\u20138000; https:\/\/doi.org\/10.1021\/acsomega.0c00037","DOI":"10.1021\/acsomega.0c00037"},{"key":"2026062413321717503_j_acph-2025-0032_ref_017","unstructured":"International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH), ICH Q2(R2) Guideline on Validation of Analytical Procedures, Current Step 5 version, June 2024; https:\/\/www.ema.europa.eu\/en\/documents\/scientific-guideline\/ich-q2r2-guideline-validation-analytical-procedures-step-5-revision-1_en.pdf; last access date September 1, 2024"},{"key":"2026062413321717503_j_acph-2025-0032_ref_018","doi-asserted-by":"crossref","unstructured":"F. Pena-Pereira, W. Wojnowski and M. Tobiszewski, AGREE-analytical GREEnness metric approach and software, Anal. Chem. 92(14) (2020) 10076\u201310082; https:\/\/doi.org\/10.1021\/acs.anal-chem.0c01887","DOI":"10.1021\/acs.analchem.0c01887"},{"key":"2026062413321717503_j_acph-2025-0032_ref_019","doi-asserted-by":"crossref","unstructured":"W. Wojnowski, M. Tobiszewski, F. Pena-Pereira and E. Psillakis, AGREEprep \u2013 Analytical greenness metric for sample preparation, Trends Anal. Chem. 149 (2022) Article ID 16553 (9 pages); https:\/\/doi.org\/10.1016\/j.trac.2022.116553","DOI":"10.1016\/j.trac.2022.116553"},{"key":"2026062413321717503_j_acph-2025-0032_ref_020","doi-asserted-by":"crossref","unstructured":"F. R. Mansour, K. M. Omer and J. P\u0142otka-Wasylka, A total scoring system and software for complex modified GAPI (ComplexMoGAPI) application in the assessment of method greenness, Green Anal. Chem. 10 (2024) Article ID 100126 (4 pages); https:\/\/doi.org\/10.1016\/j.greeac.2024.100126","DOI":"10.1016\/j.greeac.2024.100126"},{"key":"2026062413321717503_j_acph-2025-0032_ref_021","doi-asserted-by":"crossref","unstructured":"N. Manousi, W. Wojnowski, J. P\u0142otka-Wasylka and V. F. Samanidou, Blue applicability grade index (BAGI) and software: A new tool for the evaluation of method practicality, Green Chem. 25 (2023) 7598\u20137604; https:\/\/doi.org\/10.1039\/d3gc02347h","DOI":"10.1039\/D3GC02347H"},{"key":"2026062413321717503_j_acph-2025-0032_ref_022","unstructured":"British Pharmacopoeia, The Stationery Office, London 2023; last access date September 1, 2024"},{"key":"2026062413321717503_j_acph-2025-0032_ref_023","unstructured":"United States Pharmacopeia \u2013 National Formulary (USP 43\u2013NF 38), United States Pharmacopeial Convention, Rockville, MD 2020; last access date September 1, 2024"},{"key":"2026062413321717503_j_acph-2025-0032_ref_024","doi-asserted-by":"crossref","unstructured":"M. K\u0105tny and M. Frankowski, Impurities in drug products and active pharmaceutical ingredients, Crit. Rev. Anal. Chem. 47(3) (2017) 187\u2013193; https:\/\/doi.org\/10.1080\/10408347.2016.1242401","DOI":"10.1080\/10408347.2016.1242401"},{"key":"2026062413321717503_j_acph-2025-0032_ref_025","doi-asserted-by":"crossref","unstructured":"J. Kova\u010di\u0107, D. Amid\u017ei\u0107 Klari\u0107, N. Turk, \u017d. Krznari\u0107 and A. Mornar, Development and validation of stability-indicating method of etrasimod by HPLC\/DAD\/MS\/MS technique with greenness profiling, Heliyon 10(3) (2024) Article ID (14 pages) e34066; https:\/\/doi.org\/10.1016\/j.heliyon.2024.e34066","DOI":"10.1016\/j.heliyon.2024.e34066"},{"key":"2026062413321717503_j_acph-2025-0032_ref_026","doi-asserted-by":"crossref","unstructured":"J. Kova\u010di\u0107, D. Amid\u017ei\u0107 Klari\u0107, N. Turk, \u017d. Krznari\u0107, E. Riordan and A. Mornar, The stability-indicating ultra high-performance liquid chromatography with diode array detector and tandem mass spectrometry method applied for the forced degradation study of ritlecitinib: An appraisal of green and blue metrics, Pharmaceuticals 18(1) (2025) Article ID 124 (18 pages); https:\/\/doi.org\/10.3390\/ph18010124","DOI":"10.3390\/ph18010124"}],"container-title":["Acta Pharmaceutica"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/reference-global.com\/pdf\/10.2478\/acph-2025-0032","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2026,6,24]],"date-time":"2026-06-24T13:33:10Z","timestamp":1782307990000},"score":1,"resource":{"primary":{"URL":"https:\/\/reference-global.com\/article\/10.2478\/acph-2025-0032"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2025,12,1]]},"references-count":26,"journal-issue":{"issue":"4","published-online":{"date-parts":[[2026,1,13]]},"published-print":{"date-parts":[[2025,12,1]]}},"alternative-id":["10.2478\/acph-2025-0032"],"URL":"https:\/\/doi.org\/10.2478\/acph-2025-0032","relation":{},"ISSN":["1846-9558"],"issn-type":[{"value":"1846-9558","type":"electronic"}],"subject":[],"published":{"date-parts":[[2025,12,1]]}}}