{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,9,25]],"date-time":"2026-09-25T19:11:19Z","timestamp":1790363479032,"version":"4.1.0"},"reference-count":38,"publisher":"MDPI AG","issue":"12","license":[{"start":{"date-parts":[[2018,11,28]],"date-time":"2018-11-28T00:00:00Z","timestamp":1543363200000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Molecules"],"abstract":"<jats:p>A new, simple, and cost-effective TLC-densitometric method has been established for the simultaneous quantitative determination of acetylsalicylic acid and ascorbic acid in combined effervescent tablets. Separation was performed on aluminum silica gel 60F254 plates using chloroform-ethanol-glacial acid at a volume ratio of 5:4:0.03 as the mobile phase. UV densitometry was performed in absorbance mode at 200 nm and 268 nm for acetylsalicylic acid and ascorbic acid, respectively. The presented method was validated as per ICH guidelines by specificity, linearity, accuracy, precision, limit of detection, limit of quantification, and robustness. Method validations indicate a good sensitivity with a low value of LOD and LOQ of both examined active substances. The linearity range was found to be 1.50\u20139.00 \u03bcg\/spot and 1.50\u201313.50 \u03bcg\/spot for acetylsalicylic and ascorbic acid, respectively. A coefficient of variation that was less than 3% confirms the satisfactory accuracy and precision of the proposed method. The results of the assay of combined tablet formulation equal 97.1% and 101.6% in relation to the label claim that acetylsalicylic acid and ascorbic acid fulfill pharmacopoeial requirements. The developed TLC-densitometric method can be suitable for the routine simultaneous analysis of acetylsalicylic acid and ascorbic acid in combined pharmaceutical formulations. The proposed TLC-densitometry may be an alternative method to the modern high-performance liquid chromatography in the quality control of above-mentioned substances, and it can be applied when HPLC or GC is not affordable in the laboratory.<\/jats:p>","DOI":"10.3390\/molecules23123115","type":"journal-article","created":{"date-parts":[[2018,11,28]],"date-time":"2018-11-28T11:43:44Z","timestamp":1543405424000},"page":"3115","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":12,"title":["A Simple and Cost-Effective TLC-Densitometric Method for the Quantitative Determination of Acetylsalicylic Acid and Ascorbic Acid in Combined Effervescent Tablets"],"prefix":"10.3390","volume":"23","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-2672-7489","authenticated-orcid":false,"given":"Alina","family":"Pyka-Paj\u0105k","sequence":"first","affiliation":[{"name":"Department of Analytical Chemistry, School of Pharmacy with Division of Laboratory Medicine 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, School of Pharmacy with Division of Laboratory Medicine in Sosnowiec, Medical University of Silesia in Katowice, Jagiello\u0144ska 4, 41-200 Sosnowiec, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1916-1096","authenticated-orcid":false,"given":"Wioletta","family":"Parys","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, School of Pharmacy with Division of Laboratory Medicine in Sosnowiec, Medical University of Silesia in Katowice, Jagiello\u0144ska 4, 41-200 Sosnowiec, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Katarzyna","family":"Bober","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, School of Pharmacy with Division of Laboratory Medicine in Sosnowiec, Medical University of Silesia in Katowice, Jagiello\u0144ska 4, 41-200 Sosnowiec, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gra\u017cyna","family":"Janikowska","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, School of Pharmacy with Division of Laboratory Medicine 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":[[2018,11,28]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"20","DOI":"10.1016\/j.saa.2013.01.070","article-title":"A rapid method for the simultaneous determination of L- ascorbic acid and acetylsalicylic acid in aspirin C effervescent tablet by ultra performance liquid chromatography-tandem mass spectrometry","volume":"108","author":"Wabaidur","year":"2013","journal-title":"Spectrochim. Acta A Mol. Biomol. Spetrosc."},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"871","DOI":"10.1016\/S0731-7085(98)00225-8","article-title":"Simultaneous determination of salicylic acid and acetylsalicylic acid in aspirin delayed-release tablet formulations by second-derivative UV spectrophotometry","volume":"18","author":"Kokot","year":"1998","journal-title":"J. Pharm. Biomed. Anal."},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"469","DOI":"10.1016\/S0039-9140(98)00268-9","article-title":"Simultaneous determination of naproxen, salicylic acid and acetylsalicylic acid by spectrofluorimetry using partial least-squares (PLS) multivariate calibration","volume":"48","author":"Blanc","year":"1999","journal-title":"Talanta"},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"709","DOI":"10.1016\/S0014-827X(02)01265-X","article-title":"HPLC assay of acetylsalicylic acid, paracetamol, caffeine and phenobarbital in tablets","volume":"57","author":"Franeta","year":"2002","journal-title":"IL Farm."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"1346","DOI":"10.1080\/10826076.2012.676949","article-title":"Determination of acetylsalicylic acid in pharmaceutical drugs by TLC with densitometric detection in UV","volume":"35","author":"Pyka","year":"2012","journal-title":"J. Liq. Chromatogr. Relat. Technol."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"750","DOI":"10.1093\/jaoac\/91.4.750","article-title":"Simultaneous estimation of acetylsalicylic acid and clopidogrel bisulfate in pure powder and tablet formulations by high-performance column liquid chromatography and high-performance thin-layer chromatography","volume":"91","author":"Patel","year":"2008","journal-title":"J. AOAC Int."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"1169","DOI":"10.1016\/S0731-7085(00)00579-3","article-title":"Quantitative analysis of analgoantipyretics in dosage form using planar chromatography","volume":"24","author":"Franeta","year":"2001","journal-title":"J. Pharm. Biomed. Anal."},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"2405","DOI":"10.1080\/10826076.2013.790766","article-title":"Use of TLC for the quantitative determination of acetylsalicylic acid, caffeine, and ethoxybenzamide in combined tablets","volume":"36","author":"Pyka","year":"2013","journal-title":"J. Liq. Chromatogr. Relat. Technol."},{"key":"ref_9","unstructured":"Polish Pharmaceutical Society (2002). Polish Pharmacopoeia, Polish Pharmaceutical Society. (In Polish)."},{"key":"ref_10","unstructured":"United States Pharmacopeial Convention (2011). The United States Pharmacopoeia, United States Pharmacopeial Convention. [34th ed.]."},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"695","DOI":"10.1002\/bmc.2846","article-title":"Simultaneous determination of acetylsalicylic acid and salicylic acid in human plasma by isocratic high-pressure liquid chromatography with post-column hydrolysis and fluorescence detection","volume":"27","author":"Hobl","year":"2013","journal-title":"Biomed. Chromatogr."},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"309","DOI":"10.1016\/S0378-4347(97)00539-2","article-title":"Determination of acetylsalicylic acid and salicylic acid in skin and plasma by high-performance liquid chromatography","volume":"705","author":"Pirola","year":"1998","journal-title":"J. Chromatogr. B"},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"988","DOI":"10.1016\/j.clinbiochem.2013.04.007","article-title":"Low-dose acetylsalicylic acid therapy monitored with ultra high performance liquid chromatography","volume":"46","author":"Rubak","year":"2013","journal-title":"Clin. Biochem."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"12","DOI":"10.1016\/j.jchromb.2012.02.013","article-title":"Gas chromatography-mass spectrometry determination of pharmacologically active substances in urine and blood samples by use of a continuous solid-phase extraction system and microwave-assisted derivatization","volume":"891\u2013892","author":"Azzouz","year":"2012","journal-title":"J. Chromatogr. B"},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"1155","DOI":"10.1016\/S0731-7085(98)00081-8","article-title":"Assay of acetylsalicylic acid and three of its metabolites in human plasma and urine using non-aqueous capillary electrophoresis with reversed electroosmotic flow","volume":"17","author":"Hansen","year":"1998","journal-title":"J. Pharm. Biomed. Anal."},{"key":"ref_16","first-page":"429","article-title":"Simultaneous determination of guaiamar carbamate and acetylsalicylic acid by a chromatographic-densitometric method","volume":"55","author":"Krzek","year":"1998","journal-title":"Acta Pol. Pharm. Drug Res."},{"key":"ref_17","first-page":"79","article-title":"Application of cooper(II) chloride to indirect iodometric determination of the ascorbic acid in selected pharmaceuticals","volume":"53","author":"Rzeszutko","year":"1996","journal-title":"Acta Pol. Pharm. Drug Res."},{"key":"ref_18","first-page":"1069","article-title":"Kinetic spectrophotometric determination of ascorbic acid in pharmaceutical formulations","volume":"50","author":"Fathi","year":"2005","journal-title":"Anal. Chem."},{"key":"ref_19","first-page":"689","article-title":"Sensitive spectrophotometric determination of ascorbic acid in pharmaceutical samples and fruit extracts","volume":"44","author":"Srividya","year":"1999","journal-title":"Anal. Chem."},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"174","DOI":"10.1016\/j.talanta.2011.09.013","article-title":"Indirect method for spectrophotometric determination of ascorbic acid in pharmaceutical preparations with 2,4,6-tripyridyl-s-triazine by flow-injection analysis","volume":"96","author":"Biocic","year":"2012","journal-title":"Talanta"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"655","DOI":"10.2116\/analsci.21.655","article-title":"Atomic absorption spectrometry for the automatic indirect determination of ascorbic acid based on the reduction of manganese dioxide","volume":"21","author":"Noroozifar","year":"2005","journal-title":"Anal. Sci."},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"3492","DOI":"10.1016\/j.bios.2009.05.005","article-title":"Determination of ascorbic acid by polypyrrole potentiometric detector in ion chromatography","volume":"24","author":"Usta","year":"2009","journal-title":"Biosens. Bioelectron."},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"25","DOI":"10.1016\/j.plabm.2016.09.001","article-title":"Development and implementation of an HPLC-ECD method for analysis of vitamin C in plasma using single column and automatic alternating dual column regeneration","volume":"6","author":"Clark","year":"2016","journal-title":"Pract. Lab. Med."},{"key":"ref_24","first-page":"160","article-title":"Application of densitometric measurements for the determination of active ingredients in drugs","volume":"46","year":"1989","journal-title":"Acta Pol. Pharm. Drug Res."},{"key":"ref_25","first-page":"751","article-title":"Second derivative ultraviolet spectrophotometry and HPTLC for the simultaneous determination of vitamin C and dipyrone","volume":"55","author":"Aburjai","year":"2000","journal-title":"Pharmazie"},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"41","DOI":"10.1016\/j.jchromb.2005.10.018","article-title":"Rapid high-performance liquid chromatographic method for Vitamin C determination in human milk versus an enzymatic method","volume":"830","author":"Castellote","year":"2006","journal-title":"J. Chromatogr. B"},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"132","DOI":"10.1016\/j.jchromb.2005.07.008","article-title":"High-throughput analysis of Vitamin C in human plasma with the use of HPLC with monolithic column and UV-detection","volume":"824","author":"Karlsen","year":"2005","journal-title":"J. Chromatogr. B"},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"5995","DOI":"10.1016\/j.chroma.2011.06.009","article-title":"Method development and validation for optimised separation of salicylic, acetylsalicylic and ascorbic acid in pharmaceutical formulations by hydrophilic interaction chromatography and response surface methodology","volume":"1218","author":"Hatambeygi","year":"2011","journal-title":"J. Chromatogr. A"},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"2454","DOI":"10.1080\/10826076.2011.633679","article-title":"Simultaneous analysis of vitamin C and aspirin in Aspirin C effervescent tablets by high performance liquid chromatography- photodiode array detector","volume":"35","author":"Khan","year":"2012","journal-title":"J. Liq. Chromatogr. Relat. Technol."},{"key":"ref_30","unstructured":"ICH (2018, March 05). ICH Harmonised Tripartite Guideline: Validation of Analytical Procedures: Text and Methodology, Q2(R1). Available online: http:\/\/www.ich.org\/products\/guidelines\/efficacy\/article\/efficacy-guidelines.html."},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"173","DOI":"10.1556\/JPC.23.2010.3.1","article-title":"The frustrated reviewer\u2013recurrent 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_32","first-page":"71","article-title":"Application of the chromatographic and spectrophotometric method for the analytical control of L-ascorbic acid in the pharmaceutical and plant material","volume":"51","author":"Zawisza","year":"2000","journal-title":"Ann. Natl. Inst. Hyg."},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"1181","DOI":"10.1039\/AN9901501181","article-title":"Determination of the components of analgesic mixture using high-performance thin-layer chromatography","volume":"115","year":"1990","journal-title":"Analyst"},{"key":"ref_34","first-page":"143","article-title":"Determination of trace amounts of salicylic acid and acetylsalicylic acid in Polopiryna and other drugs containing acetylsalicylic acid","volume":"50","author":"Bartos","year":"1993","journal-title":"Acta Pol. Pharm."},{"key":"ref_35","first-page":"188","article-title":"Validaton of the quantitative planar chromatographic analysis of drug substances. III. Robustness testing in OPLC","volume":"8","year":"1995","journal-title":"J. Planar Chromatogr. Mod. TLC"},{"key":"ref_36","first-page":"349","article-title":"Validation and monitoring of quantitative thin layer chromatographic purity tests for bulk drug substances","volume":"8","year":"1995","journal-title":"J. Planar Chromatogr. Mod. TLC"},{"key":"ref_37","first-page":"167","article-title":"What every technologist should know about experiment design","volume":"9","author":"Hendix","year":"1979","journal-title":"Chem. Tech."},{"key":"ref_38","doi-asserted-by":"crossref","first-page":"829","DOI":"10.1080\/10826076.2011.571152","article-title":"Validation thin layer chromatography for the determination of naproxen in tablets and comparison with a pharmacopeil method","volume":"34","author":"Pyka","year":"2011","journal-title":"J. Liq. Chromatogr. Relat. Technol."}],"container-title":["Molecules"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1420-3049\/23\/12\/3115\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,11]],"date-time":"2025-10-11T15:33:02Z","timestamp":1760196782000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1420-3049\/23\/12\/3115"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2018,11,28]]},"references-count":38,"journal-issue":{"issue":"12","published-online":{"date-parts":[[2018,12]]}},"alternative-id":["molecules23123115"],"URL":"https:\/\/doi.org\/10.3390\/molecules23123115","relation":{},"ISSN":["1420-3049"],"issn-type":[{"value":"1420-3049","type":"electronic"}],"subject":[],"published":{"date-parts":[[2018,11,28]]}}}