{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,9,8]],"date-time":"2026-09-08T01:15:59Z","timestamp":1788830159077,"version":"build-2803163510"},"reference-count":52,"publisher":"MDPI AG","issue":"4","license":[{"start":{"date-parts":[[2019,12,16]],"date-time":"2019-12-16T00:00:00Z","timestamp":1576454400000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"DOI":"10.13039\/100007771","name":"\u015al\u0105ski Uniwersytet Medyczny","doi-asserted-by":"publisher","award":["KNW-1-056\/K\/9\/O"],"award-info":[{"award-number":["KNW-1-056\/K\/9\/O"]}],"id":[{"id":"10.13039\/100007771","id-type":"DOI","asserted-by":"publisher"}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Pharmaceuticals"],"abstract":"<jats:p>Diclofenac belongs to the drug class non-steroidal anti-inflammatory drugs widely used in Europe as well as all over the world. Thus, it is important to conduct research on its quality control of available pharmaceutical preparations like for example enteric coated tablets. Among various analytical techniques, thin-layer chromatography (TLC) is ideal for this task due to their short time analysis, ease of operation and low cost. Hence, the aim of this study was to develop the optimal conditions of analysis and quantitative determination of diclofenac sodium in enteric tablets by using TLC in combination with densitometry. Of all chromatographic systems tested, the best is the one which consists of silica gel 60F254 and cyclohexane: chloroform:methanol:glacial acetic acid (6:3:0.5:0.5 v\/v) as the mobile phase, which allows the successful separation of examined diclofenac sodium as active component and the largest number (twelve) of its degradation products as potential impurities of its pharmaceutical products. This indicates that the newly developed method is more effective than previously reported assays by Starek and Krzek. Linearity range was found to be 4.00\u201318.00 \u03bcg\/spot for diclofenac sodium. The results of the assay of enteric tablet formulations equals 98.8% of diclofenac sodium in relation to label claim is in a good agreement with pharmaceutical requirements.<\/jats:p>","DOI":"10.3390\/ph12040183","type":"journal-article","created":{"date-parts":[[2019,12,17]],"date-time":"2019-12-17T05:50:08Z","timestamp":1576561808000},"page":"183","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":15,"title":["Application of Thin-Layer Chromatography in Combination with Densitometry for the Determination of Diclofenac in Enteric Coated Tablets"],"prefix":"10.3390","volume":"12","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-1916-1096","authenticated-orcid":false,"given":"Wioletta","family":"Parys","sequence":"first","affiliation":[{"name":"Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences in Sosnowiec, Medical University of Silesia in Katowice, Jagiello\u0144ska 4, 41-200 Sosnowiec, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2672-7489","authenticated-orcid":false,"given":"Alina","family":"Pyka-Paj\u0105k","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences in Sosnowiec, Medical University of Silesia in Katowice, Jagiello\u0144ska 4, 41-200 Sosnowiec, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0425-5468","authenticated-orcid":false,"given":"Ma\u0142gorzata","family":"Do\u0142owy","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences in Sosnowiec, Medical University of Silesia in Katowice, Jagiello\u0144ska 4, 41-200 Sosnowiec, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2019,12,16]]},"reference":[{"key":"ref_1","first-page":"1347","article-title":"The concomitant consumption of cod liver oil causes a reduction in the daily diclofenac sodium usage in rheumatoid arthritis patients: A pilot study","volume":"7","author":"Gupta","year":"2013","journal-title":"Int. J. Clin. Diag. Res."},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"244","DOI":"10.2165\/00003495-198835030-00004","article-title":"Diclofenac sodium: A reappraisal of its pharmacodynamic and pharmacokinetic properties, and therapeutic efficacy","volume":"35","author":"Todd","year":"1988","journal-title":"Drugs"},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"804","DOI":"10.18535\/jmscr\/v7i7.143","article-title":"Comparative study of anti-inflammatory effect of diclofenac and aceclofenac on human","volume":"7","author":"Jha","year":"2019","journal-title":"JMSCR"},{"key":"ref_4","first-page":"16","article-title":"Composition, preparation, analysis and stability studies of orthofen [diclofenac sodium] suppositories","volume":"38","author":"Budukova","year":"1989","journal-title":"Farmatsiya (Moscow)"},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"73","DOI":"10.1016\/j.ijcas.2013.05.001","article-title":"The development and validation of a thin-layer chromatography densitometry method for the analysis of diclofenac sodium tablets","volume":"4","author":"Kaale","year":"2013","journal-title":"Int. J. Chem. Anal. Sci."},{"key":"ref_6","first-page":"57","article-title":"Different spectrophotometric and TLC-densitometric methods for determination of diclofenac Na and lidocaine HCl","volume":"3","author":"Ali","year":"2014","journal-title":"Pharm. Innov. J."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"227","DOI":"10.1016\/S0731-7085(01)00622-7","article-title":"Densitometric determination of diclofenac, 1-(2,6-dichlorophenyl)indolin-2-one and indolin-2-one in pharmaceutical preparations and model solutions","volume":"28","author":"Starek","year":"2002","journal-title":"J. Pharm. Biomed. Anal."},{"key":"ref_8","first-page":"147","article-title":"Development and validation of HPTLC method for simultaneous determination of tolperisone hydrochloride and diclofenac sodium in combined dosage form","volume":"5","author":"Patel","year":"2013","journal-title":"Int. J. Pharm. Tech. Res."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"817","DOI":"10.1080\/10826076.2011.571149","article-title":"Sensitive quantification of diclofenac and ibuprofen using thin-layer chromatography coupled with a Vibrio fischeri bioluminescence assay","volume":"34","author":"Seigel","year":"2011","journal-title":"J. Liq. Chrom. Relat. Technol."},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"36","DOI":"10.1556\/JPC.16.2003.1.8","article-title":"Sensitive HPTLC method for monitoring dissolution profiles of diclofenac from different tablets containing combined diclofenac and acetaminophen","volume":"16","author":"Shah","year":"2003","journal-title":"J. Planar Chromatogr. Mod. TLC"},{"key":"ref_11","first-page":"301","article-title":"Development of validated HPTLC method for quantitation of diclofenac in diclofenac gels","volume":"45","author":"Panchal","year":"2008","journal-title":"Ind. Drugs"},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"443","DOI":"10.1556\/JPC.19.2006.6.7","article-title":"Simultaneous determination of diclofenac sodium and paracetamol in a pharmaceutical preparation and in bulk drug powder by high-performance thin-layer chromatography","volume":"19","author":"Dighe","year":"2006","journal-title":"J. Planar Chromatogr. Mod. TLC"},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"539","DOI":"10.1016\/S0731-7085(02)00131-0","article-title":"HPTLC determination of diclofenac sodium from serum","volume":"29","author":"Lala","year":"2002","journal-title":"J. Pharm. Biomed. Anal."},{"key":"ref_14","first-page":"123","article-title":"High performance thin layer chromatographic method for the determination of diclofenac sodium in pharmaceutical formulations","volume":"33","author":"Thongchai","year":"2006","journal-title":"Chiang Mai J. Sci."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"1284","DOI":"10.1002\/bmc.885","article-title":"Liquid chromatographic analysis of certain commercial formulations for non-opioid analgesics","volume":"21","author":"Bhushan","year":"2007","journal-title":"Biomed. Chromatogr."},{"key":"ref_16","first-page":"643","article-title":"Stability indicating thin-layer chromatographic determination of chlorzoxazone, diclofenac sodium and paracetamol as bulk drug: Application to forced degradation study","volume":"3","author":"Kulkarni","year":"2012","journal-title":"Der Pharmacia Sinica"},{"key":"ref_17","first-page":"1","article-title":"TLC method for simultaneous quantification of chlorzoxazone, paracetamol, famotidine and diclofenac potassium in their combined dosage form","volume":"4","author":"Chaholotiya","year":"2017","journal-title":"Austin Chromatogr."},{"key":"ref_18","first-page":"201","article-title":"Separation of co-existing paracetamol and diclofenac sodium on silica gel \u2019H\u2019 layers using surfactant mediated mobile phases: Identification of diclofenac sodium from human urine","volume":"57","author":"Mohammad","year":"2009","journal-title":"Farmacia"},{"key":"ref_19","first-page":"403","article-title":"Determination of diclofenac sodium and papaverine hydrovchloride in tablets by HPLC method","volume":"65","author":"Kasperek","year":"2008","journal-title":"Acta Poloniae Pharmaceutica"},{"key":"ref_20","first-page":"110","article-title":"Validated HPLC method for simultaneous quantitation of diclofenac sodium and misoprostol in bulk drug and formulation","volume":"1","author":"Dhaneshwar","year":"2010","journal-title":"Der Chemica Sinica"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"3245","DOI":"10.1016\/j.arabjc.2013.12.022","article-title":"A validated stability-indicating UPLC method for determination of diclofenac sodium in its pure form and matrix formulations","volume":"10","author":"Elzayat","year":"2017","journal-title":"Arab. J. Chem."},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"153","DOI":"10.1016\/j.jpha.2014.10.005","article-title":"Determination of diclofenac in pharmaceutical preparations by voltammetry and gas chromatography methods","volume":"5","author":"Yilmaz","year":"2015","journal-title":"J. Pharm. Anal."},{"key":"ref_23","first-page":"333","article-title":"Comparison between capillary electrophoresis and liquid chromatography for the determination of diclofenac sodium in a pharmaceutical tablet","volume":"85","author":"Steppe","year":"2002","journal-title":"J. AOAC Int."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"587","DOI":"10.1016\/S0731-7085(99)00052-7","article-title":"Spectrofluorometric determination of diclofenac in tablets and ointments","volume":"20","author":"Damiani","year":"1999","journal-title":"J. Pharm. Biomed. Anal."},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"261","DOI":"10.1016\/S0039-9140(00)00338-6","article-title":"Spectrofluorimetric determination of diclofenac in the presence of \u03b1-cyclodextrin","volume":"52","author":"Arancibia","year":"2000","journal-title":"Talanta"},{"key":"ref_26","first-page":"310","article-title":"Spectrophotometric determination of diclofenac sodium in pharmaceutical preparations","volume":"7","author":"Barry","year":"2009","journal-title":"J. Kerbala Univ."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"855","DOI":"10.1016\/j.farmac.2005.05.011","article-title":"A simple spectrophotometric method for determination of sodium diclofenac in pharmaceutical formulations","volume":"60","author":"Matin","year":"2005","journal-title":"Il Farmaco"},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"249","DOI":"10.1016\/S0731-7085(97)00028-9","article-title":"Flow extraction spectrophotometric method for the determination of diclofenac sodium in pharmaceutical preparations","volume":"16","author":"Sanz","year":"1997","journal-title":"J. Pharm. Biomed. Anal."},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"1975","DOI":"10.1039\/c1ay05197k","article-title":"Indirect determination of sodium diclofenac, sodium dipyrone and calcium gluconate in injection drugs using digital image-based (webcam) flame emission spectrometric method","volume":"3","author":"Lyra","year":"2011","journal-title":"Anal. Methods"},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"636","DOI":"10.1016\/j.talanta.2005.05.016","article-title":"Determination of diclofenac in pharmaceutical preparations using a potentiometric sensor immobilized in a graphite matrix","volume":"68","author":"Santini","year":"2006","journal-title":"Talanta"},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"109","DOI":"10.1016\/j.msec.2014.08.072","article-title":"A new potentiometric electrode incorporating functionalized \u03b2-cyclodextrins for diclofenac determination","volume":"45","author":"Lenik","year":"2014","journal-title":"Mater. Sci. Eng. C"},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"168","DOI":"10.1016\/j.msec.2015.09.097","article-title":"Gold nanoparticle\/multi-walled carbon nanotube modified glassy carbon electrode as a sensitive voltammetric sensor for the determination of diclofenac sodium","volume":"59","author":"Afkhami","year":"2016","journal-title":"Mater. Sci. Eng. C."},{"key":"ref_33","doi-asserted-by":"crossref","unstructured":"Da Cunha, C.E.P., Rodrigues, E.S.B., Fernandes Alecrim, M., Thomaz, D.V., Mac\u00eado, I.Y.L., Garcia, L.F., de Oliveira Neto, J.R., Moreno, E.K.G., Ballaminut, N., and de Souza Gil, E. (2019). Voltammetric evaluation of diclofenac tablets samples through carbon black-based electrodes. Pharmaceuticals, 12.","DOI":"10.3390\/ph12020083"},{"key":"ref_34","doi-asserted-by":"crossref","first-page":"369","DOI":"10.1023\/A:1010153014302","article-title":"DSC in the chemical analysis of drugs. Determination of diclofenac in pharmaceutical formulations","volume":"61","author":"Bucci","year":"2000","journal-title":"J. Therm. Anal. Calorim."},{"key":"ref_35","doi-asserted-by":"crossref","first-page":"776","DOI":"10.1016\/j.talanta.2005.06.015","article-title":"Determination of diclofenac in pharmaceutical preparations by diffuse reflectance photometry","volume":"68","author":"Tubino","year":"2006","journal-title":"Talanta"},{"key":"ref_36","unstructured":"USP (2011). The United States Pharmacopeia, United States Pharmacopeial Convention. [34th ed.]."},{"key":"ref_37","unstructured":"Polish Pharmaceutical Society (2017). Polish Pharmacopoeia, Polish Pharmaceutical Society. [11th ed.]."},{"key":"ref_38","unstructured":"TSO (2008). European Pharmacopoeia, The Stationery Office. [6th ed.]."},{"key":"ref_39","unstructured":"Anderson, J.L., Berthod, A., Pino, V., and Stalcup, A.M. (2015). Basic HPLC theory and definitions: Retention, thermodynamics, selectivity, zone spreading, kinetics, and resolution. Analytical Separation Science, Wiley-VCH Verlag GmbH & Co. KGaA. [1st ed.]."},{"key":"ref_40","doi-asserted-by":"crossref","first-page":"3383","DOI":"10.1007\/s00216-019-01813-2","article-title":"Investigation of factors influencing the separation of diastereomers of phosphorothioated oligonucleotides","volume":"411","author":"Enmark","year":"2019","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_41","unstructured":"ICH (2005). ICH Harmonised Tripartite Guideline: Validation of Analytical Procedures: Text and Methodology, Q2(R1), ICH. Available online: http:\/\/www.ich.org\/products\/guidelines\/efficacy\/article\/ efficacy-guidelines.html."},{"key":"ref_42","doi-asserted-by":"crossref","first-page":"358","DOI":"10.1016\/j.pharma.2016.07.001","article-title":"A novel stability-indicating UPLC method development and validation for the determination of seven impurities in various diclofenac pharmaceutical dosage forms","volume":"74","author":"Azougagha","year":"2016","journal-title":"Ann. Pharm. Fr."},{"key":"ref_43","doi-asserted-by":"crossref","first-page":"284","DOI":"10.1016\/j.ijpharm.2014.01.030","article-title":"The difficulties for a photolabile drug in topical formulations: The case of diclofenac","volume":"465","author":"Ioele","year":"2014","journal-title":"Int. J. Pharmaceut."},{"key":"ref_44","doi-asserted-by":"crossref","first-page":"589","DOI":"10.1590\/S1984-82502013000300021","article-title":"A simple method for the quantification of diclofenac potassium in oral suspension by high-performance liquid chromatography with UV-detection","volume":"49","author":"Rubim","year":"2013","journal-title":"Braz. J. Pharm. Sci."},{"key":"ref_45","doi-asserted-by":"crossref","first-page":"66","DOI":"10.1016\/j.jsps.2018.07.020","article-title":"Development and validation of a new HPLC analytical method for the determination of diclofenac in tablets","volume":"27","author":"Alquadeib","year":"2019","journal-title":"Saudi Pharm. J."},{"key":"ref_46","doi-asserted-by":"crossref","first-page":"173","DOI":"10.1556\/JPC.23.2010.3.1","article-title":"The frustrated reviewer\u2014Recurrent failures in manuscripts describing validation of quantitative TLC\/HPTLC procedures for analysis of pharmaceuticals","volume":"23","author":"Renger","year":"2010","journal-title":"J. Planar Chromatogr. Mod. TLC"},{"key":"ref_47","unstructured":"EMA Committee for Medicinal Products for Human Use (CHMP) (2011). Guideline on Bioanalytical Method Validation, European Medicines Agency (EMA)."},{"key":"ref_48","doi-asserted-by":"crossref","first-page":"323","DOI":"10.1016\/S1570-0232(03)00246-0","article-title":"Guidelines for analytical method development and validation of biotechnological synthesis of drugs. Production of a hydroxyprogesterone as model","volume":"791","author":"Lindholm","year":"2003","journal-title":"J. Chromatogr. B"},{"key":"ref_49","unstructured":"USP (1995). United States Pharmacopeia, United States Pharmacopeial Convention. [23th ed.]."},{"key":"ref_50","doi-asserted-by":"crossref","unstructured":"Konieczka, P. (2017). Namie\u015bnik, Assessment and Quality Control of Analytical Results (Polish), Scientific Publisher (PWN). Available online: https:\/\/www.poczytaj.pl\/ksiazka\/ocena-i-kontrola-jakosci-wynikow-pomiarow-analitycznych.","DOI":"10.1201\/9781315295015-2"},{"key":"ref_51","unstructured":"McNaught, A.D., and Wilkinson, A. (1997). Compendium of Chemical Terminology, Blackwell Scientific Publications. [2nd ed.]."},{"key":"ref_52","doi-asserted-by":"crossref","first-page":"455","DOI":"10.1007\/BF02268814","article-title":"Valey to peak ratio as a measure for the separation of two chromatographic peaks","volume":"4","author":"Christophe","year":"1971","journal-title":"Chromatographia"}],"container-title":["Pharmaceuticals"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1424-8247\/12\/4\/183\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,11]],"date-time":"2025-10-11T13:42:39Z","timestamp":1760190159000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1424-8247\/12\/4\/183"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2019,12,16]]},"references-count":52,"journal-issue":{"issue":"4","published-online":{"date-parts":[[2019,12]]}},"alternative-id":["ph12040183"],"URL":"https:\/\/doi.org\/10.3390\/ph12040183","relation":{},"ISSN":["1424-8247"],"issn-type":[{"value":"1424-8247","type":"electronic"}],"subject":[],"published":{"date-parts":[[2019,12,16]]}}}