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Due to frequent side effects, it is usually co\u2010administered with an antihypertensive, such as propranolol and\/or an antidiuretic, such as furosemide. In this study, a highly sensitive HPLC\u2010FLD method was developed for the simultaneous determination of the three APIs in urine. For their analysis, a Nucleosil C8 column (250\u2009mm\u2009\u00d7\u20094.6\u2009mm, 5\u2009\u03bcm) at 50\u00b0C was used as the stationary phase and an isocratic system of methanol\u2013acetonitrile\u201320\u2009mM NaH\n                    <jats:sub>2<\/jats:sub>\n                    PO\n                    <jats:sub>4<\/jats:sub>\n                    at pH\u20093.6, 12:20:68\u2009v\/v\/v as the mobile phase. The calibration curves for the analytes were generated both in urine and in the pure diluent. The reliability of the method was evaluated according to ICH guidelines in terms of accuracy and repeatability. For sample purification, protein precipitation techniques involving the addition of organic solvents, acids, or salts, as well as the freezing\u2010out technique, were studied. Liquid\u2013liquid extraction, using various solvents, and solid\u2010phase extraction (SPE) were also tested, where the latter was found more suitable. SPE optimization was achieved using experimental design and a D\u2010optimal mixture design. Reliable analyte recoveries demonstrate the capability of the proposed method, making it a suitable tool for biological studies.\n                  <\/jats:p>","DOI":"10.1002\/bmc.70529","type":"journal-article","created":{"date-parts":[[2026,6,26]],"date-time":"2026-06-26T09:50:11Z","timestamp":1782467411000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Optimized SPE\u2010HPLC\u2010FLD Method for the Simultaneous Determination of Olaparib, Propranolol, and Furosemide in Human Urine"],"prefix":"10.1002","volume":"40","author":[{"given":"Georgios","family":"Kamaris","sequence":"first","affiliation":[{"name":"Laboratory of Pharmaceutical Analysis, Department of Pharmacy Aristotle University of Thessaloniki  Thessaloniki Greece"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Antonia","family":"Kalagia","sequence":"additional","affiliation":[{"name":"Laboratory of Pharmaceutical Analysis, Department 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