Background:
Recently, superparamagnetic and electromagnetic nano-materials have been extensively
studied and their potential applications have also been investigated in various fields. In this regard, currently,
Fe3O4 NPs are valuable candidates as diagnostic agents such as magnetic resonance imaging, enzyme immobilization,
biosensing and cell labeling, and therapeutic probes, including drug delivery, bacteria detection, magnetic
separation, and hyperthermia agents.
Objective:
In this study, electrochemical synthesis of Cu2+ cations-doped superparamagnetic magnetite nanoparticles
(Cu-SMNPs) and their in situ surface coating with saccharides (i.e., glucose, sucrose and starch) are reported. The
prepared glucose/Cu-SMNPs, sucrose/Cu-SMNPs and starch/Cu-SMNPs samples are characterized by structural,
magnetic and morphological analyses by XRD, FT-IR, FE-SEM, EDAX and VSM. The suitability of the prepared
samples for biomedical use is also proved.
Methods:
A simple cathodic electrochemical set-up was used to fabricate the iron oxide samples. The bath electrolyte
was one litre deionized water containing 1.5g iron chloride, 3g iron nitrate, 0.5g copper chloride and 0.5g
saccharide (i.e., glucose or sucrose or starch). The cathode and anode electrodes were connected to a DC power
supply (PROVA 8000) as the power source. The deposition experiments were conducted at 10 mA cm-2 for 30
min. For the preparation of glucose/Cu-SMNPs, sucrose/Cu-SMNPs and starch/Cu-SMNPs samples, three electrodeposition
experiments were carried out in three similar baths with only a change in the dissolved saccharide
type. The prepared SMNPs samples were characterized by structural, morphological and magnetic analyses including
X-ray powder diffraction (XRD, a Phillips PW-1800 diffractometer Smart Lab), field-emission scanning
electron microscopy (FE-SEM, Mira 3-XMU with accelerating voltage of 100 kV), transmission electron microscopy
(TEM, model Zeiss EM900 with an accelerating voltage of 80 kV), fourier transform infrared (FT-IR, a
Bruker Vector 22 Fourier transformed infrared spectrometer) and vibrating sample magnetometers (VSM, model
Lakeshore 7410).
Results:
Three types of metal-cations doped superparamagnetic magnetite nanoparticles (SMNPs), glucosegrafted
Cu2+-doped MNPs (glucose/Cu-SMNPs), sucrose-grafted Cu2+-doped SMNPs (sucrose/Cu-SMNPs) and
starch-grafted Cu2+-doped SMNPs (starch/Cu-SMNPs), were prepared for the first time. Fourier-transform infrared
spectroscopy, field-emission scanning electron microscopy and energy dispersive X-ray techniques proved the presence
of saccharide capped layer on the surface of deposited SMNPs and also copper cations doping on their crystal
structures. Superparamagnetic behaviors, including low coercivity and remanence values, were observed for all the
prepared samples.
Conclusion:
SMNPs capped with saccharides (i.e., glucose, sucrose and starch) were successfully synthesized via
one-pot simple deposition procedures. These particles showed suitable superparamagnetic properties with negligible
remanence values and proper saturation magnetization, thus proving that they all have required physicochemical
and magnetic characteristics for biomedical purposes.
Automated Scanning Electron Microscopy and Energy Dispersive x‐ray Spectroscopy (SEM/EDS) for detection and quantification of Gadolinium (Gd) in tissues