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Simultaneous analysis of these analytes in dosage forms and biofluids using rapid, sensitive, and selective methods would be highly beneficial. Herein, we report the first direct, label\u2010free spectrofluorometric method for simultaneously quantifying methocarbamol (MET) and aspirin (ASP) in coformulated tablets and spiked human urine. The method utilizes excitation at 274\u2009nm with independent emission detection at 300\u2009nm for MET and 402\u2009nm for ASP, using methanol as the diluting solvent. The assay was rectilinear over ranges of 0.10\u20130.80\u2009\u03bcg\/mL for MET and 0.05\u20130.50\u2009\u03bcg\/mL for ASP with detection limits of 14.9 and 10.6\u2009ng\/mL for MET and ASP, respectively. The method was validated in compliance with ICH regulations. The approach was applied efficiently to assay both analytes in their tablets and spiked human urine with high % recoveries (98%\u2013103%) and low RSD (1.7%\u20133.3%). In addition, the sustainability and practicality of the developed method were assessed using the RGB\u201012 whiteness algorithm, indicating the whiteness of the developed method. The method's greenness was also confirmed using three greenness metrics that showed excellent eco\u2010friendliness of the developed method.<\/jats:p>","DOI":"10.1002\/bio.70139","type":"journal-article","created":{"date-parts":[[2025,3,11]],"date-time":"2025-03-11T13:00:54Z","timestamp":1741698054000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Label\u2010Free Spectrofluorometric Method for Simultaneous Estimation of Methocarbamol and Aspirin in Biological and Pharmaceutical Matrices: Whiteness and Greenness Evaluation"],"prefix":"10.1002","volume":"40","author":[{"given":"Heba\u00a0Abd","family":"El\u2010Aziz","sequence":"first","affiliation":[{"name":"Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy Mansoura University  Mansoura Egypt"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5426-5993","authenticated-orcid":false,"given":"Abdallah\u00a0M.","family":"Zeid","sequence":"additional","affiliation":[{"name":"Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy Mansoura University  Mansoura Egypt"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2025,3,5]]},"reference":[{"key":"e_1_2_8_2_1","doi-asserted-by":"publisher","DOI":"10.1007\/s40122-021-00235-2"},{"key":"e_1_2_8_3_1","article-title":"Skeletal Muscle Spasms","volume":"13","author":"Pergolizzi Jr J.","year":"2021","journal-title":"Cureus Journal of Medical Science"},{"key":"e_1_2_8_4_1","doi-asserted-by":"publisher","DOI":"10.1002\/jor.25508"},{"key":"e_1_2_8_5_1","doi-asserted-by":"publisher","DOI":"10.1097\/01.mjt.0000134786.50087.d8"},{"volume-title":"Clarke's Analysis of Drugs and Poisons","year":"2006","author":"Moffat A. 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