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The presence of guaifenesin\u2010related impurities and interference from co\u2010formulated analgesics further complicate its detection in pharmaceutical, biological, and environmental matrices. This review compiles peer\u2010reviewed English\u2010language studies indexed in Scopus, Web of Science, PubMed, ScienceDirect, and Google Scholar and provides a critical assessment of MT quantification methods developed over the past 25\u2009years. Evidence shows that optimized high\u2010performance liquid chromatography (HPLC), particularly fluorescence\u2010based systems, provides the highest sensitivity and selectivity, achieving sub\u2010ng\/mL detection and overcoming limitations of UV assays, such as signal suppression and narrow linear ranges. Electrochemical approaches using CNT\u2010, graphene\u2010, MOF\u2010, and magnetic\u2010nanocomposite\u2010modified electrodes enhance redox discrimination and enable nM\u2013\u03bcM detection. Chemometric\u2010assisted spectroscopic techniques offer rapid, low\u2010cost analysis suitable for simple formulations but lack reliability in complex matrices. Across all platforms, strict pH control, rapid processing, and selective extraction methods\u2014such as solid\u2010phase extraction (SPE), molecularly imprinted polymer (MIP), and dispersive liquid\u2013liquid microextraction (DLLME) remain essential to reduce degradation and matrix interference. Future progress will rely on miniaturized microfluidic systems, improved stability\u2010indicating chromatography, and intelligent electrochemical sensors capable of multiplex quantification in challenging samples.<\/jats:p>","DOI":"10.1002\/bmc.70419","type":"journal-article","created":{"date-parts":[[2026,3,17]],"date-time":"2026-03-17T16:51:27Z","timestamp":1773766287000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Evolving Analytical Methods for the Quantification of Methocarbamol: A Critical Review"],"prefix":"10.1002","volume":"40","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-1875-7760","authenticated-orcid":false,"given":"Hemn\u00a0A.\u00a0H.","family":"Barzani","sequence":"first","affiliation":[{"name":"Department of Medical Laboratory Science, College of Health Science Lebanese French University  Erbil Iraq"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3774-6071","authenticated-orcid":false,"given":"Rebaz\u00a0Anwar","family":"Omer","sequence":"additional","affiliation":[{"name":"Department of Chemistry, Faculty of Sciences and Health Koya University  Koya Kurdistan Region \u2013 F.R. 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