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Keywords
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Polymerization
,Microliter electrochemical cell
,Magnetic solid phase extraction
,Saliva
,Central composite design
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Abstract
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In this study, a green magnetic hydrogel composite based on a polymeric deep eutectic solvent (PDES) was
synthesized via thermal frontal polymerization and employed as an efficient adsorbent for the extraction of
doxorubicin (DOX) from saliva samples. The PDES was prepared from menthol and acrylic acid, while acrylic
acid-coated Fe3O4 nanoparticles (Fe3O4@AA NPs) acted as a magnetic core and contributed to network formation
through acrylic acid functionalities.
The resulting Fe3O4@AA-PDES composite was comprehensively characterized. Following extraction, DOX was
determined by differential pulse voltammetry using a simple carbon ceramic electrode (CCE) integrated into a
microliter-scale electrochemical cell, enabling direct analysis without electrode modification or pretreatment and
resulting in operational simplicity and good reproducibility. Experimental variables affecting extraction efficiency
were optimized using central composite design. Under optimized conditions, the method exhibited a wide
linear range (50–1000 ng/mL), a low detection limit (15.72 ng/mL), and high precision and accuracy, confirming
its reliability for DOX quantification in saliva. Successful application to saliva samples demonstrates the method's
relevance for noninvasive therapeutic drug monitoring of DOX. In addition, environmental assessment using the
ComplexMoGAPI and AGREE metrics confirmed that the overall workflow complies strongly with green
analytical chemistry principles, supporting its practical applicability for sustainable bioanalytical
determinations.
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