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    Development of a molecularly imprinted polymer on silanized graphene oxide for the detection of 17-estradiol in wastewater
    (Wiley, 2024) Mughal, Zaib un Nisa; Aylaz, Gulgun; Shaikh, Huma; Memon, Shahabuddin; Andac, Muge
    This research article demonstrates the synthesis, characterization, and electrochemical evaluation of a molecularly imprinted polymer (MIP) on the surface of silanized graphene oxide (silanized GO), which is nanostructured and used to quantify 17-estradiol (E2) in wastewater. As characterization methods, X-ray diffraction (XRD), Raman spectroscopy, dynamic scattering light (DSL), scanning electron microscope (SEM), and Fourier transform infrared spectroscopy (FTIR) were utilized to examine the synthesized GO, silanized GO, MIP-GO composite, and non-imprinted polymer (NIP)-GO (NIP-GO) composite. FTIR results confirmed the successful synthesis of GO composites. Raman study confirmed the synthesis of monolayer silanized GO, MIP-GO composite, and NIP-GO composite. Surface morphology revealed that after polymerization, the surface of silanized GO sheet-like morphology is covered with nanoparticles. Adsorption kinetics studies revealed that adsorption follows the pseudo-second-order kinetics. Further, we studied the performance of a MIP-GO-based sensor by optimizing the effects of pH, scan rate, and incubation period. The linear calibration was achieved between the oxidation peak current and E2 concentration from 0.1 to 0.81 ppm, with a detection limit of 0.037 ppm. The selectivity of the MIP-GO composite was also checked by using other estrogens, and it was found that E2 is 3.3, 0.5, and 1.4 times more selective than equilin, estriol, and estrone, respectively. The composite was successfully applied to the wastewater samples for the detection of E2, and a good percentage of recoveries were achieved. It suggests that the reported composite can be applied to real samples.Practitioner Points An innovative electrochemical sensor was developed for selective detection of 17-estradiol through molecularly imprinted polymer fabricated on the surface of silanized GO (MIP-GO composite). The developed method was comprehensively validated and found to be linear in the range of 0.1 to 0.8 ppm of 17-estradiol, with 0.037 ppm of limit of detection and 0.1 ppm of limit of quantification, respectively. The developed MIP-GO-composite-based electrochemical sensor was found 3.3, 0.5, and 1.4 times more selective for 17-estradiol than equiline, estriol, and estrone, respectively. The applicability of a developed sensor was also checked on wastewater samples, and a good percent recovery was obtained. A glassy carbon electrode (GCE) is modified with MIP-GO composite, and it binds E2 due to specific binding sites and is detected by voltammetric detection. Furthermore, by increasing the concentration of E2, the peak current intensity increases simultaneously. image
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    Graphene oxide decorated with melamine-imprinted nanobeads for SERS detection of melamine in milk
    (Elsevier B.V., 2025) Nisa Mughal, Zaib un; Liman, Gorkem; Aylaz, Gulgun; Shaikh, Huma; Memon, Shahabuddin; Andac, Muge
    We present a novel, cost-effective SERS substrate for melamine detection in milk. Melamine is a nitrogen-rich compound illegally used to indicate high protein content. We developed a hybrid substrate based on molecularly imprinted polymer nanobeads functionalized with graphene oxide (MIP nanobeads@fGO). MIPs act as a door for selective detection and provide chemical enhancement. fGO achieves further chemical enhancement of the Raman signal by bond-making through functionalized moieties and electrostatic interaction with the ring moiety of fGO with melamine in SERS. Prior to polymerization, the molecular interaction between vinyl imidazole (VIM) as a functional monomer and melamine as a target molecule was modeled using AutoDockTools GUI (Graphical User Interface) and AutoGrid for molecular modelling simulations and grid calculations. From the clustering histogram, melamine and VIM molecules had the lowest binding energy of −0.77 kcal/mol. Also, the free energy of Melamine-VIM interaction at 298.15 K was −2729.21 kcal/mol, which is evidence that the interaction was energetically favorable. The fGO and MIP nanobeads@fGO were characterized by various techniques including FTIR and RAMAN spectroscopy, DSL and SEM. The SERS performance of MIP nanobeads@fGO was analyzed and showed excellent performance towards melamine with an EF of 1.3 × 106 and good reproducibility with an RSD of 8.3 %. A good correlation was observed between the –log concentration of melamine (μM) and the Raman intensity (a.u.) in a broad linear range from 7.9 E-5 μM to 7.9 E2 μM, with LOD and LOQ of 1.2 μM (0.15 ppm) and 3.6 μM (0.45 ppm), respectively. The USFDA and WHO introduced the tolerable level of melamine in milk and dairy products at no >2.5 ppm. Our LOD is below the tolerable limit, indicating that the MIP nanobeads@fGO substrate can be effectively used for food safety analysis in milk samples. © 2025