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A novel combination of celecoxib (CXP) and ciprofloxacin (CIP) has recently been used to enhance both motor performance and CNS cell morphology, alterations in the rate of disease progression, quality of life, and survival, which passed phase IIb RCT study. Celecoxib is classified as a non\u2010steroidal anti\u2010inflammatory drug; ciprofloxacin is a fluoroquinolone antibiotic that has a synergistic effect for the treatment of ALS, which is a severe neurological disorder. A new sustainable, simple, sensitive, and environmentally friendly synchronous spectrofluorimetric approach (SSF) was established to simultaneously estimate celecoxib and ciprofloxacin in pure form and biological fluids. The approach depends on synchronous fluorescence spectroscopy, where CXP and CIP were detected at 364 and 438\u2009nm, correspondingly, using \u0394\n                    <jats:italic>\u03bb<\/jats:italic>\n                    of 80\u2010nm utilizing sodium dodecyl sulphate (SDS) micellar system, which considerably improved synchronous fluorescence intensity. The approach was validated and revealed excellent linearity with concentrations varying from 10 to 10,000 and 5 to 20,000\u2009ng\/mL for CXP and CIP; correspondingly, CXP and CIP showed extremely low limits of detection (LODs) 0.58\u20130.24\u2009ng\/mL, which guarantee the sensitivity of the proposed approach. The suggested approach was successfully implemented to analyze the co\u2010administered pharmaceuticals in their pure form and actual human plasma after concurrent oral administration of both drugs, which may be employed in an inquiry on the pharmacokinetics and bioavailability of human plasma to the new coming PrimeC pharmaceutical formulation. Ultimately, the method's remarkable greenness was proved by evaluating its greenness profile using various assessment strategies. The findings revealed that the SSF approach is a sustainable and environmentally friendly analytical approach.\n                  <\/jats:p>","DOI":"10.1002\/bio.70222","type":"journal-article","created":{"date-parts":[[2025,6,24]],"date-time":"2025-06-24T23:10:26Z","timestamp":1750806626000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Innovative Synchronous Spectrofluorometric Method for Assessing a Novel Drug Combination in Amyotrophic Lateral Sclerosis: In\u00a0Vivo Human Application With Greenness and Sustainability Evaluation"],"prefix":"10.1002","volume":"40","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-1173-4654","authenticated-orcid":false,"given":"Amal\u00a0B.","family":"Ahmed","sequence":"first","affiliation":[{"name":"Pharmaceutical Chemistry Department, Faculty of Pharmacy Nahda University (NUB)  Beni\u2010Suef 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