Developing an exclusive sensor based on molecularly imprinted polymer/Multi-walled carbon nanotubes/Fe3O4@Au nanocomposite for the selective determination of an anti-cancer drug imatinib.

Determination of pharmaceuticals especially anticancer drugs is one of the important issues in environmental and medical investigation and creating good information about human health. The presence sturdy introducing an electroanalytical sensor based on molecularly imprinted polymer (MIP)/Multi-walled carbon nanotubes (MWCNTs)/Au@Fe3O4 nanoparticles modified carbon paste electrode (PE) to determine imatinib (IMA). The MIP/MWCNTs/Au@Fe3O4/PE showed catalytic activity and also a sensitive strategy to sensing IMA in the concentration range 1-1000 µM with a limit of detection of 0.013 µM. The MIP/MWCNTs/Au@Fe3O4/PE has shown interesting results in the analysis of IMA in real samples, and the interference investigations results show the high selectivity of the MIP/MWCNTs/Au@Fe3O4/PE in the monitoring of IMA in complex fluids such as tablet and blood serum and results approved by F-test and t-test as statistical methods.

Cu-BTC MOF/ionic liquid nanocomposite as novel catalyst to electrochemical monitoring of digoxin in pharmaceutical and environmental samples.

There is no effective environmental treatment strategy that does not include monitoring for pharmaceutical compounds in environmental and biological fluids. The widespread presence of pharmaceutical-based pollutants in water sources is a significant public health concern. The treatment process relies heavily on maintaining a stable digoxin concentration in bodily fluids. Finding the correct dose for this medication appears to be crucial. In this research, an easy and high sensibility electrochemical sensor was developed to determine digoxin based on a paste electrode (CPE) that was modified with Cu-BTC MOF and ion liquid ((IL); 1-Methyl-3-Butyl-imidazolinium bromide in this case) using voltammetric methods in 0.1 M phosphate buffer solution (PBS) at pH 5.0. The sensor's selectivity was significantly increased by using Cu-BTC MOF and IL to detect digoxin. The characteristics of the electrode modifiers were evaluated by SEM, XRD and EDS techniques. The LDR was found to be 0.1-40 µM and the LOD of 0.08 µM, respectively.

Survey of antibacterial activity and release kinetics of gold-decorated magnetic nanoparticles of Fe0 conjugated with sulfamethoxazole against Escherichia coli and Staphylococcus aureus.

Drug delivery of antibiotics with magnetic nanoparticles improved by coating metals such as gold and silver has recently been studied. This work describe a simple method to synthesize modified magnetic nanoparticles which have high ability to modify the customary formulation of antibiotics such as sulfamethoxazole (SMX) and pursuant study of adsorption-desorption (release) of this drug. These synthesized nanoparticles were characterized by different methods, including field emission scanning electron microscopy, energy dispersive X-ray spectroscopy and mapping, Fourier-transform infrared spectroscopy, X-ray diffraction, vibrating-sample magnetometry, thermogravimetric analysis and zeta potential test. Present assay showed a well correlation with the introduced carrier for the drug. Also the hypothesis were proved by some adsorption isotherm models and drug kinetics studies of carriers with different drug release kinetics models. This study confirmed the adsorption isotherm models and kinetics of drug sorbate are Temkin and Pseudo-First-Order Lagergren models, respectively; the kinetics of drug release from this carrier is based on Zero-Order model. The values of MIC in antibacterial test for pure SMX and SMX conjugated nanoparticles against Escherichia coli were calculated to be 14 and 2.5 µg/mL, respectively, and these values against Staphylococcus aureus were 24 and 1.25 µg/mL, respectively.

Facile Synthesis of NiO/ZnO nanocomposite as an effective platform for electrochemical determination of carbamazepine.

The pharmaceutical science demand for sustainable and selective electrochemical sensors which exhibit ultrasensitive capabilities for the monitoring of different drugs. In an attempt to build a useful electrochemical sensor, we describe a most efficient method for the fabrication of NiO/ZnO nanocomposite through aqueous chemical growth method. The successfully synthesized NiO/ZnO nanocomposite is successfully employed to modify a glassy carbon electrode in order to build a sensitive and reliable electrochemical sensor for the detection of carbamazepine (CBZ), an anticonvulsant drug. The morphological texture, functionalities and crystalline structure of prepared nanocomposite were determined via FTIR, XRD, EDX, TEM, and SEM analysis. In order to examine the charge transfer kinetics, the cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were used to exploit the electrochemical properties of the synthesized nanocomposite. The NiO/ZnO nanocomposite exhibited excellent electron transfer kinetics and less resistive behavior than the individual NiO and ZnO nanoparticles. The differential pulse voltammetry and cyclic voltammetry tools were used for the fluent determination of CBZ. Certain parameters were optimized to develop an effective method including optimum scan rate 60 mV/s, potential range from 0.4 to 1.4 V and BRB as supporting electrolyte with pH 3. The developed sensor showed exceptional response for CBZ under the linear dynamic range from 5 to 100 µM. The limit of detection of proposed NiO/ZnO sensor for the CBZ was calculated to be 0.08 µM. The analytical approach of prepared electrochemical sensor was investigated in different pharmaceutical formulation with acceptable percent recoveries ranging from 96.7 to 98.6%.

Simple turn-off fluorescence sensor for determination of raloxifene using gold nanoparticles stabilized by chitosan hydrogel.

It is essential to develop a simple, applicable, and reliable assay to anticancer drug raloxifene (RAF) because of its significant usage and side effect due to entering residue in the environment. Fluorescence sensors developed and widely used because of them high selectivity, fast-response, and highly-sensitivity. The gold nanoparticles using chitosan hydrogel was synthesized and applied as a fluorescence sensor to determine the trace amount of RAF. The characterization methods including DLS, FE-SEM, EDX, XRD, and FT-IR were performed to confirm the synthesized structure. This sensor turned off the fluorescent signals proportional to RAF concentrations at 400 nm. The RAF can be detected in the linear range from 5 × 10-7 to 5 × 10-5 M. Limits of detection and quantification were obtained as 34 × 10-8 and 11 × 10-7 M as well as the relative standard deviation calculated as 1.63% in RAF measuring. The effective parameters on quenching efficiency were studied by central composite design (CCD) with response surface methodology (RSM). The effective parameters in RAF determination, include analyte concentration, temperature, contact time, and pH, were obtained as 35 µM, 30 °C, 8 min, and pH = 8.5. The sensor was applied to determine the RAF concentrations in biological and environmental samples with satisfactory recoveries between 97.5% and 109%.

Magnetic nanoparticles based on cerium MOF supported on the MWCNT as a fluorescence quenching sensor for determination of 6-mercaptopurine.

In this study, a new magnetic nanocomposite was developed as an efficient and fast-response fluorescence quenching sensor for determination of anticancer drug 6-mercaptopurine (6-MP). For this purpose, the needle-shape fluorescence metal-organic framework of cerium (Ce-MOF) were successfully synthesized on the surface of multiwalled carbon nanotubes using 1,3,5-benzenetricarboxylic acid ligand via a facile solvothermal assisted route and magnetized. The accuracy of the proposed synthesis was confirmed using the FT-IR, FE-SEM, XRD, and VSM methods. The obtained product as presented the fluorescence emission in 331 nm by excitation of 293 nm in excitation/emission slit widths of 10.0 nm. The operation of suggested method is based on quenching the fluorescence signal in accordance with increasing the 6-MP concentration. The proposed assay effectively detected the trace amount of 6-MP in the linear range of 1.0 × 10-6 to 7 × 10-5 M. The limit of detection and limit of quantification were obtained as 8.6 × 10-7 and 2.86 × 10-6 M, respectively. The analyte molecule was determined in real samples with satisfactory recoveries between 98.75 and 105.33.

Ultrasensitive and highly selective "turn-on" fluorescent sensor for the detection and measurement of melatonin in juice samples.

Melatonin (MLT), a hormone related to the regulation of brain functions, is directly related to sleep quality and is considered to be a possible adjuvant therapy for patients needing hospitalization for coronavirus disease 2019 pneumonia, and accurate measurement of MLT is crucial. Herein, a new, highly sensitive, and easy operation fluorescent probe was provided based on Zr metal-organic framework encapsulation into the molecularly imprinted polymer (MOF@MIP). By combining unique properties of MIP and fluorescent MOF, selectivity and operation of the applied method were significantly improved. Different characterization methods, such as XRD, FT-IR, and FE-SEM, were used to confirm the synthesis reliability. MOF@MIP was successfully used for the precise identification and ultrasensitive detection for trace amounts of MLT. The detection mechanism for the analytical system is based on the ''turn-on'' fluorescence (FL) signal in 404 nm. The findings proved that it is possible to detect trace amounts of MLT in real samples including grape, cherry, and sour cherry juice. The linear range and the limit of detection (LOD) for trace amounts of MLT were obtained as 1-100 ng/mL and 0.18 ng/mL, respectively.

New fabrication of CuFe2O4/PAMAM nanocomposites by an efficient removal performance for organic dyes: Kinetic study.

Today, removing pollutants from water sources is essential because of the population increase and the growing need for safe drinking water. Dyes are one of the most critical pollutants from industrial effluents such as paper and textile industries that profoundly affect the environment. There are several ways to remove environmental contaminants. Magnetic nanoparticles have a high ability to adsorb dyes. Of course, increasing the interaction between magnetic nanomaterials and pollutants is also essential, which can be done using porous materials such as dendrimers. In this work, the synthesis of CuFe2O4 magnetite nanoparticles within the polyamidoamine dendrimers structure was used as an efficient sorbent to remove both alizarin reds (ARS) and brilliant green (BG) dyes. Moreover, various parameters for dyes removal were studied. The optimum removal conditions were obtained for ARS within 30 min at a sorbent dose of 2 mg per 5 mL for the initial dye concentration of 7.0 ppm in pH 6 at 25 °C, and for BG within 45 min at a sorbent dose of 5 mg per 5 mL for the initial dye concentration of 17.0 ppm in pH 8 at 25 °C. At the optimum values of the above parameters, both dyes' removal efficiency was more than 97%. Also, the obtained results showed that the adsorption isotherm follows the Langmuir model and Temkin model for ARS and BG, respectively. This method was successfully used for the removal of both dyes in water samples.

A hierarchical 3D camellia-like molybdenum tungsten disulfide architectures for the determination of morphine and tramadol.

A practical technique was applied to fabricate MoWS2 nanocomposite through a one-pot hydrothermal method for use as the electrocatalyst. The characterization of MoWS2 nanocomposite was investigated by several techniques to identify the size, crystal structure, and elemental composition. MoWS2 nanocomposite exhibited a unique and well-defined hierarchical structure with neatly and densely piled nanopetals acting as the active sites in the electrocatalytic reactions. A carbon screen-printed electrode (CSPE) modified with interesting MoWS2 nanopetals (MoWS2/CSPE) was constructed. Subsequently, the electrochemical oxidation of morphine on fabricated MoWS2/CSPE was studied. Experimental results confirm that under optimized conditions, the maximum oxidation current of morphine occurs at 275 mV in the case of MoWS2/CSPE that is around 100 mV more negative than that observed in the case of the unmodified CSPE and about 2.6 times increase was observed for the oxidation peak current. The analytical approach was obtained by differential pulse voltammetry in accordance with the relationship between the oxidation peak current and the morphine concentration. The oxidation peak currents for morphine were found to vary linearly with its concentrations in the range of 4.8 × 10-8-5.05 × 10-4 M with the detection limit of 1.44 × 10-8 M. Two completely separated signals occured at the potentials of 275 mV and 920 mV for oxidation of morphine and tramadol at the surface of MoWS2/CSPE which are sufficient for determination of morphine in the presence of tramadol. The presence of morphine was also detected in real samples using the introduced approach. Graphical abstract Schematic representation of fabrication of the MoWS2 nanocomposite through a one-pot hydrothermal method for use as the electrocatalyst. A carbon screen-printed electrode was modified with MoWS2 nanocomposite. Subsequently, the electrochemical oxidation of morphine on the fabricated electrode was studied.

Fluorescence detection of laccases activity by the photoinduced electron transfer (PET) process.

Laccases play a vital role in some physiological processes, for example in morphogenesis, carbon cycle, and defense against parasitism. So, designing a high-sensitivity accurate method is essential for researchers. In this study, a simple fluorescence method based on the function of carbon nitride (g-C3N4) by dopamine is synthesized. For the design of this sensor, carbon nitride (g-C3N4) is initially synthesis by using a simple method, which is carried out by heating melamine at 550 °C for 3 h and modifying it with dopamine by a linker such as glutaraldehyde. However, the g-C3N4-Dopa produced by this method, with an excitation wavelength of 330 nm, has a fluorescence emission at 466 nm. When laccase and g-C3N4-Dopa were mixed, dopamine with redox property was oxidized to dopaquinone; this causes the phenomenon of photoinduced electron transfer (PET) process between g-C3N4 and the dopaquinone. Hence, fluorescence quenching occurs due to this phenomenon. As a result of these discussions, a sensor for the laccase activity was designed based on the fluorescence quenching degree, supporting a linear range of 0.0-400.0 U L-1 with the detection limit of 2.0 U L-1. Using this sensor, the activity of the laccase enzyme in the human serum samples is measured. Dopamine-functionalized carbon nitride was prepared and utilized for the highly sensitive detection of laccases activity.

Facile synthesis and characterization of magnetic nanocomposite ZnO/CoFe2O4 hetero-structure for rapid photocatalytic degradation of imidacloprid.

This work has attempted to investigate the potential of ZnO/CoFe2O4 magnetic nanocomposite to mineralize imidacloprid completely to have sustainable pollutant free and safe water supply. The co-precipitation method was performed to prepare the composites; was performed to characterize composites, scanning electron microscope (SEM), transmission electron microscopy (TEM), energy dispersive x-ray crystallography (EDX), x-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, and vibrating sample magnetometer (VSM). It was attempted to explore and enhance parameters influencing the process and the percentage of imidacloprid degradation, including photocatalyst amount, pesticide concentration, pH, radiation time, and temperature. UV-Vis spectrophotometer was used for the degradation percent of organochlorine pesticides. Parameters affecting the process, including photocatalyst amount, pesticide concentration, pH, radiation time, and temperature effect on the percentage of imidacloprid degradation were Investigated and optimized. 0.05 g of photocatalyst, with a concentration of 5 ppm for 45 min under light exposure was obtained at pH 10 at room temperature.

Simultaneous voltammetric determination of glutathione, doxorubicin and tyrosine based on the electrocatalytic effect of a nickel(II) complex and of Pt:Co nanoparticles as a conductive mediator.

Glutathione (GSH) is an important tripeptide that plays an important role in preventing damage to reactive oxygen species. An electrochemical assay was fabricated for this purpose by modification of a carbon paste electrode (CPE) with bis(1,10-phenanthroline)(1,10-phenanthroline-5,6-dione)nickel(II) hexafluorophosphate (BPPDNi) as new electro-catalyst and Pt:Co nanoparticle (Pt:CO-NPs) as highly conductive mediator. The analyses were performed at a scan rate of 10 mV/s and at a pH value of 7.4. The BPPDNi/Pt:CO-NPs/CPE showed a high sensitivity and good selectivity for electro-catalytic determination of glutathione (GSH) in nano-molar concentration range. In addition, the BPPDNi/Pt:CO-NPs/CPE was used for the determination of glutathione in the presence of doxorubicin (DOX) and tyrosine (Tyr) with three separated oxidation signals ~160 mV, ~385 mV and ~790 mV vs. Ag/AgCl/KClsat, respectively. The peak currents of the square wave voltammetric analyses were linearly dependent on glutathione, doxorubicin and tyrosine concentrations in the respective ranges of 0.001-450, 0.5-300 and 1.0-650 µM, with detection limits of 0.5 nM, 0.1 µM and 0.6 µM, respectively. Graphical abstract The first analytical sensor for simultaneous determination of glutathione, doxorubicin and tyrosine.

A catechol biosensor based on immobilizing laccase to Fe3O4@Au core-shell nanoparticles.

This work is directed towards the synthesis of the magnetic nanoparticle in a core and a gold shell with immobilized of laccase on its surface (Fe3O4@Au@ Lac). The prepared Fe3O4@Au@ Lac core/shell nanoparticles are characterized by means TEM, SEM, DLS, zeta potential, UV-Vis, and TGA. Meanwhile, as an example of the applications, Biosensor activity was investigated by using the oxidation of catechol and recording the UV-Vis absorption in the 402 nm wavelength. The biosensor also demonstrated optimum activity at pH 5.0, reaction time at 40 min, and 35 mg the amount of biosensor. Linear response in the catechol concentration range of 5.0-70.0 µM. The limit of detection and the apparent Michaels-Menten constant (Km) of the biosensor were 2 µM and 15 µM respectively.

A novel electrochemical sensor based on silver/halloysite nanotube/molybdenum disulfide nanocomposite for efficient nitrite sensing.

In the present study, the silver/halloysite nanotube/molybdenum disulfide (Ag/HNT/MoS2) nanocomposite was successfully synthesized. For this purpose, the lumen of HNTs was firstly modified by silver to generate Ag nanorods via chemical process and then the MoS2 layers deposited on the Ag/HNT nanocomposite by hydrothermal method. The characterization of Ag/HNT/MoS2 nanocomposite were investigated by field emission scanning electron microscopy (FE-SEM), Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS), energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD) analyses. The nanocomposite modified carbon paste electrode (CPE) was applied for the electrocatalytic detection of nitrite in aqueous solutions. It was demonstrated that the treatment of HNTs with Ag and MoS2 materials enhanced the catalytic performance of modified CPE. At optimal experimental conditions, the designed sensor displayed remarkable sensing ability toward nitrite oxidation, offering a good linearity from 2 to 425 µM. The limit of detection (LOD) of the proposed strategy was estimated to be 0.7 µM based S/N = 3. The good reproducibility, acceptable stability, fast response time and anti-interference performance of the proposed assay suggests that the modified CPE has great potential working as a nitrite electrochemical sensor for environmental applications.

Application of dispersive liquid-liquid-solidified floating organic drop microextraction and ETAAS for the preconcentration and determination of indium.

A new, simple and efficient method, including dispersive liquid-liquid-solidified floating organic drop microextraction and then electrothermal atomic absorption spectrometry, has been developed for the preconcentration and determination of ultratrace amounts of indium. The method was applied to preconcentrate the indium-1-(2-pyridylazo)-2-naphthol complex in 25 µL 1-undecanol. The various factors affecting the extraction efficiency, such as pH, type and volume of extraction solvent, type and volume of disperser solvent, sample volume, ionic strength, and ligand concentration, were investigated and optimized. Under the optimum conditions, an enrichment factor of 62.5, precision of ±4.75%, a detection limit of 55.6 ng L-1, and for the calibration graph a linear range of 96.0-3360 ng L-1 were obtained. The method was used for the extraction and determination of indium in water and standard samples with satisfactory results. Graphical Abstract Preconcentration of indium ions via liquid-liquid-solidified floating organic drop microextraction method and determination by ETAAS.

Preparation and Application of Nanostructure Ion-Imprinted Polymer for Selective Solid-Phase Extraction of Pb Ions in Water, Hair, and Food Samples.

In this research, nanostructure Pb(II) ion-imprinted polymer (IIP) was prepared by formation of 1,5-diphenylthiocarbazon (dithizone) complex. Polymerization was performed via bulk polymerization, with methacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross-linking monomer in the presence of ammonium persulfate as the initiator. To characterize the synthesized IIP, FTIR spectroscopy and field emission scanning electron microscopy were used. This polymer was used for selective preconcentration of ultra-trace amounts of Pb ions through the SPE method. The Pb ion concentration was determined by electrothermal atomic absorption spectrometry. In the optimization process, the effects of various factors, such as pH of the sample solution, type and concentration of eluent, equilibrium sorption and desorption times, and sample volume, were investigated. Under optimized conditions, the maximum sorbent capacity was 38.46 mg/g and the enrichment factor was 200. Linearity was within the range 1.0-320.0 ng/L, with good r(2) values. The LOD was 0.55 ng/L, and the intraday and interday RSD values (n = 7, 20 ng/L Pb ions) were 2.8 and 3.5%, respectively. This selective and sensitive proposed method was applied successfully to the determination of Pb in water, hair, and food samples, with high recoveries.

A novel voltammetric sensor for sensitive detection of mercury(II) ions using glassy carbon electrode modified with graphene-based ion imprinted polymer.

In this paper, a novel strategy was proposed to prepare ion-imprinted polymer (IIP) on the surface of reduced graphene oxide (RGO). Polymerization was performed using methacrylic acid (MAA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, 2,2'-((9E,10E)-1,4-dihydroxyanthracene-9,10-diylidene) bis(hydrazine-1-carbothioamide) (DDBHCT) as the chelating agent and ammonium persulfate (APS) as initiator, via surface imprinted technique. The RGO-IIP was characterized by means of Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The electrochemical procedure was based on the accumulation of Hg(II) ions at the surface of a modified glassy carbon electrode (GCE) with RGO-IIP. The prepared RGO-IIP sensor has higher voltammetric response compared to the non-imprinted polymer (NIP), traditional IIP and RGO. The RGO-IIP modified electrode exhibited a linear relationship toward Hg(II) concentrations ranging from 0.07 to 80 µg L(-1). The limit of detection (LOD) was found to be 0.02 µg L(-1) (S/N=3), below the guideline value from the World Health Organization (WHO). The applicability of the proposed electrochemical sensor to determination of mercury(II) ions in different water samples was reported.

Synthesis and application of novel ion-imprinted polymer coated magnetic multi-walled carbon nanotubes for selective solid phase extraction of lead(II) ions.

In this study, novel magnetic ion-imprinted polymer (MIIP) nanoparticles were utilized for the sensitive and selective detection of Pb(II) ions by graphite furnace atomic absorption spectrometry (GFAAS). The Pb(II)-imprinted polymer was synthesized by using 4-vinylpyridine (4VP) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, 2,3,5,6-tetra(2-pyridyl) pyrazine (TPPZ) as the chelating agent and magnetic multi-walled carbon nanotubes (MMWCNTs) as the carrier. The synthesized MIIP materials were characterized by field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and vibrating sample magnetometer (VSM). Various analytical parameters such as extraction and desorption time, eluent type and concentration, pH and sample volume were systematically examined. The selectivity of MIIP sorbent for Pb(II) ions in the presence of some cations was also evaluated. The limit of detection (LOD, 3S(b)) and the relative standard deviation (RSD, n=8, c=25 ng L(-1)) were found to be 2.4 ng L(-1) and 5.6%, respectively. The maximum sorption capacity of the MIIP for Pb(II) was found to be 48.1 mg g(-1). Finally, the proposed analytical procedure was successfully applied to monitoring lead in human hair and water samples with satisfactory results for the spiked samples.

Simultaneous column preconcentration of ultra trace amounts of heavy metals with nano-adsorbent in some environmental and biological samples.

In the present investigation, multi-walled carbon nanotubes impregnated by 1,4,10,13-tetraoxa-7,16-diazacyclooctadecane were prepared and applied as adsorbent for the simultaneous separation of Bi(III), Cu(II), Cd(II) and Pb(II) ions prior to their determination by electrothermal atomic absorption spectrometry. The following analytical figures of merit were determined for bismuth, copper, cadmium and lead, respectively: enrichment factors of 168, 134, 111 and 146, assay precisions of ±4.6%, ±4.8%, ±5.3% and ±5.0% and detection limits of 11.3, 3.7, 0.5 and 0.3 ng L(-1). The method was successfully applied for the determination of heavy metals in environmental, biological and certified reference materials.