Abstract In the present study, multifunctional core‐shell fibre mats were designed by co‐electrospinning. These core‐shell fibre mats have three different functionalities: 1) they are magnetic, 2) they change their optical properties with the pH of the media, and 3) they are sensitive to O 2 . The shell is formed by a fluorescent pH‐sensitive co‐polymer which was previously synthesised and characterized by our research group. The core is a suspension formed by magnetic nanoparticles in a solution made up by a lipophilic indicator dye (oxygen indicator; PtOEP) and, poly‐methyl methacrylate, in THF. The magnetic nanoparticles were prepared by encapsulation of magnetite within a cross‐linked polymeric matrix (MMA‐co‐EDMA). To our knowledge, this is the first time that three functionalities (magnetic properties, sensitivity to pH, and response to O 2 concentration) were successful conjugated on the same micro‐ or nano‐material via a facile one‐step process with high yield and cost effectiveness. The morphology of the well‐organized core‐shell fibres were characterized by high resolution scanning electron microcopy (HRSEM), transmission electron microcopy (TEM), and confocal laser microscopy. The luminescent properties of core‐shell fibre mats were analysed and successfully used for simultaneously monitoring pH (from 6 to 8) and O 2 , showing complete reversibility, high sensitivity (i.e., K sv = 7.07 bar −1 for determining O 2 in aqueous media), high magnetic susceptibility, and short response times.
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