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Herein, dendrimer-modified montmorillonite (Mt)-decorated poly-Ɛ-caprolactone (PCL) and chitosan (CHIT)-based nanofibers were prepared. Mt was modified with a poly(amidoamine) generation 1 (PAMAMG1) dendrimer, and the obtained PAMAMG1–Mt was incorporated into the PCL–CHIT nanofiber’s structure. The PCL–CHIT/PAMAMG1–Mt nanofibers were conjugated with glutamate oxidase (GluOx) to design a bio-based detection system for monosodium glutamate (MSG). PAMAMG1–Mt was added to the PCL–CHIT backbone to provide a multipoint binding side to immobilize GluOx via covalent bonds. After the characterization of PCL–CHIT/PAMAMG1–Mt/GluOx, it was calibrated for MSG. The linear ranges were determined from 0.025 to 0.25 mM MSG using PCL–CHIT/Mt/GluOx and from 0.0025 to 0.175 mM MSG using PCL–CHIT/PAMAMG1–Mt/GluOx (with a detection limit of 7.019 µM for PCL–CHIT/Mt/GluOx and 1.045 µM for PCL–CHIT/PAMAMG1–Mt/GluOx). Finally, PCL–CHIT/PAMAMG1–Mt/GluOx was applied to analyze MSG content in tomato soup without interfering with the sample matrix, giving a recovery percentage of 103.125%. Hence, the nanofiber modification with dendrimer-intercalated Mt and GluOx conjugation onto the formed nanocomposite structures was performed, and the PCL–CHIT/PAMAMG1–Mt/GluOx system was successfully developed for MSG detection.

Multifunctional electrospun nanofibers (ENs) with improved properties have increased attention nowadays. Their insoluble forms in water with decreased hydrophobicity are desired for the immobilization of biological molecules. Also, the addition of functional groups on the backbone provides the conjugation of biomolecules onto the surface of ENs via covalent bonds to increase their stability. Here, poly­(vinylidene fluoride) (PVDF) was chosen to prepare a platform, which is insoluble in water, and polyethylenimine (PEI) was used to add amine groups on the surface of ENs to bind biological molecules via covalent conjugation. So, PVDF-PEI nanofibers were prepared on a glassy carbon electrode to immobilize an antimethamphetamine antibody (Anti-METH) as a model biomolecule. The obtained PVDF-PEI/Anti-METH was used for the bioelectrochemical detection of methamphetamine (METH), a common illicit drug. Bioelectrochemical detection of METH on PVDF-PEI/Anti-METH-coated electrodes was carried out by voltammetry in the range of 2.0–50 ng/mL METH. Moreover, the effect of dansyl chloride (DNC) derivatization of METH on the sensitivity of PVDF-PEI/Anti-METH was tested. Finally, METH analysis was carried out in synthetic body fluids. The obtained results showed that PVDF-PEI ENs can be adopted as an immobilization matrix for the biorecognition elements of biobased detection systems, and the derivative of METH (METH-DNC) increased the sensitivity of PVDF-PEI/Anti-METH.