Electrospun EU/HPMC nanofibers decorated by ZIF-8 nanoparticle as the advanced electrochemical biosensor modifier for sensitive and selective detection of c-MET cancer biomarker in human plasma sample.

This research presents a selective and sensitive electrochemical biosensor for the detection of the mesenchymal-epithelial transition factor (c-MET). The biosensing is based on a modification of the SPCE (screen-printed carbon electrode) with the electrospun nanofiber containing eudragit (EU), hydroxypropyl methylcellulose (HPMC), and Zeolite imidazolate frameworks (ZIF-8) nanoparticles. EU/HPMC/ZIF-8 nanofibers have presented a high capability of electron transfer, and more active surface area than bare SPCE due to synergistic effects between EU, HPMC, and ZIF-8. On the other hand, EU/HPMC nanofibers provided high porosity, flexible structures, high specific surface area, and good mechanical strength. The presence of ZIF-8 nanoparticles improved the immobilization of anti-c-MET on the modified SPCE and also resulted in increasing the conductivity. By c-MET incubation on the modified SPCE, c-MET was connected to anti-c-MET, and consequently the electrochemical signal of [Fe(CN)6]3-/4- as the anion redox probe was reduced. In order to investigate the structural and morphological characteristics and elemental composition of electrospun nanofibers, various characterization methods including FE-SEM, XRD, FTIR, and EDS were used. Under optimum conditions with a working potential range -0.3-0.6 V (vs. Ag/AgCl), linear range (LR), correlation coefficient (R2), sensitivity, and limit of detection (LOD) were acquired at 100 fg/mL-100 ng/mL, 0.9985, 53.28 µA/cm2.dec, and 1.28 fg/mL, respectively. Moreover, the mentioned biosensor was investigated in a human plasma sample to determine c-MET and showed ideal results including reproducibility, stability, and good selectivity against other proteins.

Detection of receptor tyrosine kinase-orphan receptor-2 using an electrochemical immunosensor modified with electrospun nanofibers comprising polyvinylpyrrolidone, soy, and gold nanoparticles.

An electrochemical immunosensing platform was developed for the detection of receptor tyrosine kinase-orphan receptor-2 (ROR2) at a glassy carbon electrode (GCE) modified with the electrospun nanofiber containing polyvinylpyrrolidone (PVP), soy, and Au nanoparticles (AuNPs). The PVP/soy/AuNP nanofiber exhibited good electrochemical behavior due to synergistic effects between PVP, soy, and AuNPs. The PVP/soy in the modified film provided good mechanical strength, high porosity, flexible structures, and high specific surface area. On the other hand, the presence of AuNPs effectively improved conductivity, as well as the immobilization of anti-ROR2 on the modified GCE, leading to enhanced sensitivity. Various characterization approaches such as FE-SEM, FTIR, and EDS were used for investigating the morphological and structural features, and the elemental composition. The designed immunosensor performance was investigated using electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and differential pulse voltammetry (DPV). Under optimum conditions with a working potential range from -0.2 to 0.6 V (vs. SCE), sensitivity, linear range (LR), limit of detection (LOD), and correlation coefficient (R2) were acquired at 122.26 µA/cm2 dec, 0.01-1000 pg/mL, 3.39 fg/mL, and 0.9974, respectively. Furthermore, the determination of ROR2 in human plasma samples using the designed immunosensing platform was examined and exhibited satisfactory results including good selectivity against other proteins, reproducibility, and cyclic stability.

Label-free electrochemical immunosensor for detection of insulin-like growth factor-1 (IGF-1) using a specific monoclonal receptor on electrospun Zein-based nanofibers/rGO-modified electrode.

A novel electrochemical immunosensor was developed for ultrasensitive determination of the hormone insulin-like growth factor 1 (IGF-1) based on immobilization of a specific monoclonal antibody on the electrospun nanofibers of Polyacrylonitrile (PAN)/Zein-reduced graphene oxide (rGO) nanoparticle. The nanofibers deposited on glassy carbon electrode (GCE) showed good electrochemical behaviors with synergistic effects between PAN, Zein, and rGO. PAN/Zein nanofibers were used due to flexibility, high porosity, good mechanical strength, high specific surface area, and flexible structures, while rGO nanoparticles were used to improve the detection sensitivity and anti-IGF-1 immobilizing. Different characterization techniques were applied consisting of FE-SEM, FT-IR, and EDS for the investigation of morphological features and nanofiber size. The redox reactions of [Fe(CN)6]4-/3- on the modified electrode surface were probed for studying the immobilization and determination processes, using differential pulse voltammetry (DPV) and cyclic voltammetry (CV). Under optimal conditions, LOD (limit of detection) and LOQ (limit of quantification) were obtained as 55.72 fg/mL and 185.73 fg/mL respectively, and sensitivity was acquired 136.29 µA/cm2.dec. Moreover, a wide linear range was obtained ranging from 1 pg/mL to 10 ng/mL for IGF-1. Furthermore, the proposed method was applied for the analysis of IGF-1 in several human plasma samples with acceptable results, and it also exhibited high selectivity, stability, and reproducibility.

Introduction of a Zn-based metal-organic framework @ biomass porous activated carbon as a high-sensitive coating for a stainless steel SPME fiber: application to the simultaneous analysis of nonsteroidal anti-inflammatory drugs.

The present study introduces a high-efficiency nanocomposite material featuring a zinc-based metal-organic framework and a novel porous activated carbon derived from bread waste. The prepared nanocomposite, namely Zn-MOF-5@BHPAC, has been synthesized by a low-temperature hydrothermal process and coated onto the surface of a stainless steel wire with epoxy glue. The fabricated fiber has been employed as an SPME fiber applied in the extraction and pre-concentration of some nonsteroidal anti-inflammatory drugs (NSAIDs) before their high-performance liquid chromatography-ultraviolet (HPLC-UV) studies. The characterization studies were performed utilizing field emission scanning electron microscopy, elemental mapping, energy-dispersive X-ray spectroscopy, elemental analyzer, Fourier-transform infrared spectroscopy, and Brunauer-Emmett-Teller surface area analysis. Under the optimal conditions, the method demonstrated low detection limits (LODs, 0.06-0.15 µg L-1), wide linear ranges (LRs, 0.20-380 µg L-1) with good linearity (R2 > 0.991), good precisions (RSDs < 6.95%), and acceptable relative recoveries (RR > 85%). Using the green and affordable biomass of bread as a novel carbon-rich source is an innovative idea provided in this study. In addition, the hybridization of the obtained carbon-based material with the MOF compound to create a new high-capacity sorbent is another strength of the proposed method. Long service lifetime, economic efficiency, environmental friendliness, and high extraction capability were some of the other advantages of the suggested procedure. Therefore, the method can utilize successfully for the simultaneous determination of NSAIDs (as model analytes) in different matrixes.

Voltammetric determination of pethidine in biofluids at a carbon cloth electrode modified by carbon selenide nanofilm.

Developing a sensitive portable sensor for the screening of illicit drugs is always challenging. Due to the importance of pethidine (PTD) tracking in addiction diagnosis, many demands have recently increased for a selective and real-time sensor. Herein, a simple electrochemical sensor has been developed based on conductive carbon cloth (CC) modified with carbon selenide nanofilms (CSe2NF) to provide a CSe2NF/CC electrode as a novel PTD sensing tool. Profiting from the ingenious design of doping strategy during the synthesis process, Se was doped in the carbonaceous skeleton of the CC. Thus, the active surface area of the CSe2NF (4.61 cm2) increased respect to the unmodified CC (0.094 cm2) to embed a suitable sensing interface in the fast PTD assay. By optimizing some effective experimental parameters such as pH, supporting electrolyte, Se powder amount, scan rate and accumulation time, the sensor catalyzed efficiently the oxidation reaction of PTD at 0.97 V. Based on peak current variations, the PTD was measured over a broad concentration range from 29 nM up to 181.8 µM with a limit of detection (LOD) as low as 19.3 nM compared to the other reported PTD sensors. The developed flexible sensor recognized the spiked PTD concentrations in some biofluids, including human blood, urine and saliva. The results of PTD analysis in the non-spiked and spiked blood, urine and saliva samples as the real samples by the developed sensor were validated by HPLC analysis as the reference method using t-test statistical method at confidence level of 5%. This sensing strategy based on the binder-free electrode could be promising for designing some sizable wearable sensors at a low cost. The high sensitivity of the sensor, which is a bonus for the rapid and on-site measurement of PTD, may open up a route for noninvasive routine analysis in clinical samples.

Salt-Mediated Organic Solvent Precipitation for Enhanced Recovery of Peptides Generated by Pepsin Digestion.

Conventional solvent-based precipitation makes it challenging to obtain a high recovery of low mass peptides. However, we previously demonstrated that the inclusion of salt ions, specifically ZnSO4, together with high concentrations of acetone, maximizes the recovery of peptides generated from trypsin digestion. We herein generalized this protocol to the rapid (5 min) precipitation of pepsin-digested peptides recovered from acidic matrices. The precipitation protocol extended to other organic solvents (acetonitrile), with high recovery from dilute peptide samples permitting preconcentration and purification. Mass spectrometry profiling of pepsin-generated peptides demonstrated that the protocol captured peptides as small as 800 u, although with a preferential bias towards recovering larger and more hydrophobic peptides. The precipitation protocol was applied to rapidly quench, concentrate, and purify pepsin-digested samples ahead of MS. Complex mixtures of yeast and plasma proteome extracts were successfully precipitated following digestion, with over 95% of MS-identified peptides observed in the pellet fraction. The full precipitation workflow-including the digestion step-can be completed in under 10 min, with direct MS analysis of the recovered peptide pellets showing exceptional protein sequence coverage.

Preparation of a new coating of graphene oxide/nickel complex on a nickelized metal surface for direct immersion solid phase microextraction of some polycyclic aromatic hydrocarbons.

BACKGROUND: Solid-phase microextraction (SPME) is a versatile sampling and sample preparation technology that possess a significant application in the extraction and pre-concentration of a broad range of micro-pollutants from different kind of matrices. Selection and preparation of an appropriate fiber substrate and coating materials have always been the main challenges of the SPME procedure. This paper introduces a high-efficiency metal-based SPME fiber with a new chemical coating of nickel/graphene oxide/nickel tetraazamacrocyclic complex (Ni/GO/NiTAM). RESULT: The Ni/GO/NiTAM sorbent was electroless deposited onto the surface of an aluchrom (Alu) wire, and then the prepared fiber was employed for the extraction and pre-concentration of some PAHs before their HPLC-UV analysis. The prepared fiber characterization data were assessed using FE-SEM, EDX, XRD, FT-IR, and BET techniques. The method validation parameters, including the linearity range (LRs: 0.10 to 200.0 µg L-1), the limit of detection (LODs: 0.03‒0.30 µg L-1), and the limit of quantification (LOQs: 0.10-1.00 µg L-1), under optimal conditions. The relative standard deviations (RSDs) of intra-day, inter-day, and single fiber repeatability (for the samples spiked at 25 µg L‒1) were in the range of 0.32-2.94, 1.20-4.09, and 1.42‒4.39%, respectively. In addition, the technique recoveries (RR %) and enrichment factors (EF) were in the range of 83.10‒107.80% and 83-164, respectively. CONCLUSION: The fiber fabrication was simple, and the applied materials were also economical and easily accessible. Alu metal has high physicochemical and mechanical stability and thus can be a good alternative for the substrate of the fragile commercial SPME fibers. High rigidity and durability, long service life, and high extraction capability are some of the other advantages of the offered fiber.

Recent advances in developing optical and electrochemical sensors for analysis of methamphetamine: A review.

Recognition of misused stimulant drugs has always been a hot topic from a medical and judicial perspective. Methamphetamine (MAMP) is an addictive and illegal drug that profoundly affects the central nervous system. Like other illicit drugs, the detection of MAMP in biological and street samples is vital for several organizations such as forensic medicine, anti-drug headquarters and diagnostic clinics. By emerging nanotechnology and exploiting nanomaterials in sensing applications, a great deal of attention has been given to the design of analytical sensors in MAMP tracing. For the first time, this study has briefly reviewed all the optical and electrochemical sensors in MAMP detection from earlier so far. How various receptors with engineering nanomaterials allow developing novel approaches to measure MAMP have been studied. Fundamental concepts related to optical and electrochemical recognition assays in which nanomaterials have been used and relevant MAMP sensing applications have been comprehensively covered. Challenges, opportunities and future outlooks of this field have also been discussed at the end.

Chemical binding of horseradish peroxidase enzyme with poly beta-cyclodextrin and its application as molecularly imprinted polymer for the monitoring of H2 O2 in human plasma samples.

In this study, a selective and sensitive molecular imprinting-based electrochemical sensors, for horseradish peroxidase (HRP) entrapment was fabricated using electro polymerization of ß-Cyclodextrin (ß-CD) on the surface of glassy carbon electrode. Poly beta-cyclodextrin P(ß-CD) provide efficient surface area for self-immobilization of HRP as well as improve imprinting efficiency. The proposed imprinted biosensor successfully utilized for detection of HRP with excellent analytical results which linear range is 0.1 mg/mL to 10 ng/mL with LOD of 2.23 ng/mL. Furthermore, electrocatalytical activity of the prepared biosensor toward the reduction of hydrogen peroxide was investigated in the ranges of 1 to 15 µM with a detection limit of 0.4 µM by using chronoamperometry technique. The developed biosensor was used for the detection of hydrogen peroxide in unprocessed human plasma sample.

Trace analysis of organophosphorus pesticide residues in fruit juices and vegetables by an electrochemically fabricated solid-phase microextraction fiber coated with a layer-by-layer graphenized graphite/graphene oxide/polyaniline nanocomposite.

Herein, a solid-phase microextraction pencil lead fiber coated with a layer-by-layer graphenized graphite/graphene oxide/polyaniline nanocomposite (GG/GO/PANI) was fabricated by an in situ electrochemical technique for the trace analysis of organophosphorus pesticide residues in packed grape and apple juice and also fresh tomato samples. The effects of various parameters, including the type of desorption solvent, adsorption time, desorption time, pH, salt addition, and stirring rate, on the extraction efficiency of the studied pesticides were investigated and accordingly, these parameters were optimized. The proposed fiber demonstrated desirable linear ranges (0.01-300 µg L-1) with good correlation coefficients (R2 ≥ 0.996) as well as low limits of detection (0.003-0.03 µg L-1) for the studied pesticides. The relative standard deviations (n = 5) for the extraction of 50 µg L-1 of each analyte were less than 7 and 11.5% for inter and intra-day precisions, respectively. This fast, facile, and repeatable electrochemical fabrication method produced a porous and homogeneous coating. The proposed fiber demonstrated good extraction efficiency, high stability, and long life-time despite being low cost. The successful application of the proposed fiber for the trace determination of pesticides in complex food matrices was proven by the satisfactory relative recoveries of 80.7-116.5%.

A novel bioassay for the monitoring of hydrogen peroxide in human plasma samples based on binding of horseradish peroxidase-conjugated prostate specific antigen to poly (toluidine blue) as imprinted polymer receptor.

A low cost, sensitive and selective electrochemical imprinted biosensor for horseradish peroxidase-conjugated prostate-specific antigen (PSA) was designed and prepared based on the combination of Toluidine blue (TB) and self-assembly surface molecular imprinting technique. Poly toluidine blue [P(TB)] provided high surface area for dense loading of HRP-PSA antibody on GCE surface. P(TB), as supporting material, could effectively enhance imprinting efficiency and the electrode conductivity and facilitate electron transfer. The imprinted biosensor was characterized through Field emission scanning electron microscopy (FE-SEM), Energy-dispersive X-ray spectroscopy (EDX) and electrochemical methods. The proposed biosensor indicates very highly electrocatalytical activity for the reduction of hydrogen peroxide (H2O2). Also, engineered biosensor was used for determination of H2O2 by different electrochemical techniques including differential pulse voltammetry, square wave voltammetry and chronoamperometry. Under the optimized conditions, the proposed bio-imprinted polymer exhibit excellent electrocatalytical activity toward the reduction of H2O2 with wide linear range of 0.001 to 40 mM and a low limit of quantification (LLOQ) of 1 µM.

An in situ electrochemical fabrication of layer by layer graphenized graphite polyaniline as a stable solid-phase microextraction fiber coating for trace environmental analysis.

A layer by layer graphenized graphite/polyaniline coating was fabricated on commercial pencil lead substrate by an in situ facile, fast and efficient electrochemical procedure. The electrodeposited polyaniline film on surface-confined graphene structure can integrate the advantages of the both layers and was used for solid-phase microextraction. Effective experimental parameters in electrochemical production of graphene nanosheets and electropolymerization of aniline were optimized. The prepared fiber was used for extraction and determination of four polycyclic aromatic hydrocarbons: phenanthrene, anthracene, fluoranthene and pyrene in aqueous samples by high performance liquid chromatography. The fiber coating was characterized by Fourier transform infrared spectroscopy, X-ray diffraction and scanning electron microscopy. Under the optimized conditions, the coating provided good linear ranges (0.10-25 µg/L for phenanthrene, 0.05-12.5 µg/L for anthracene, 0.825-99 µg/L for fluoranthene and 0.625-75 µg/L for pyrene (R2  = 0.999)) and limits of detection, 0.016 to 0.275 µg/L. The produced coating has several attractive features such as high stability, low cost and long operation time.

Application of sunflower stalk-carbon nitride nanosheets as a green sorbent in the solid-phase extraction of polycyclic aromatic hydrocarbons followed by high-performance liquid chromatography.

A green biocomposite of sunflower stalks and graphitic carbon nitride nanosheets has been applied as a solid-phase extraction adsorbent for sample preparation of five polycyclic aromatic hydrocarbons in different solutions using high-performance liquid chromatography with ultraviolet detection. Before the modification, sunflower stalks exhibited relatively low adsorption to the polycyclic aromatic hydrocarbons extraction. The modified sunflower stalks showed increased adsorption to the analytes extraction due to the increase in surface and existence of a π-π interaction between the analytes and graphitic carbon nitride nanosheets on the surface. Under the optimal conditions, the limits of detection and quantification for five polycyclic aromatic hydrocarbons compounds could reach 0.4-32 and 1.2-95 ng/L, respectively. The method accuracy was evaluated using recovery measurements in spiked real samples and good recoveries from 71 to 115% with relative standard deviations of <10% have been achieved. The developed method was successfully applied for polycyclic aromatic hydrocarbons determination in various samples-well water, tap water, soil, vegetable, and barbequed meat (kebab)-with analytes contents ranging from 0.065 to 13.3 µg/L. The prepared green composite as a new sorbent has some advantages including ease of preparation, low cost, and good reusability.

Introduction of coiled solid phase microextraction fiber coated by mesoporous silica/cetyltrimethylammonium bromide for ultra-trace environmental analysis.

In this study, a tiny coiled cupper wire as a novel solid phase microextraction (SPME) fiber was coated with mesoporous silica/cetyltrimethylammonium bromide (MCM-41/CTAB) as an adsorbent by electrochemically assisted self-assembly method and used for the preconcentration of polycyclic aromatic hydrocarbons (PAHs) as model analytes prior to chromatographic determination. Deposition of MCM-41/CTAB on the coiled SPME (C-SPME) fiber resulted in easily controlled and reproducible SPME coatings. Non-calcined MCM-41/CTAB on C-SPME plays a key role in the adsorption of PAHs. Under the optimized experimental conditions, low detection limits (36-1220pgL-1), and wide linear dynamic ranges (R2>0.98) were achieved in the range of 0.25-25,000, 0.12-15,000, 0.56-32,000, 4.1-100,000ngL-1 for phenanthrene, anthracene, fluoranthene and pyrene respectively. The reusability of proposed fiber as well as relative standard deviations for repetitive determination of the target analytes was evaluated. The proposed method was successfully applied for determination of PAHs in several real samples.

Introduction of a coiled solid-phase microextraction fiber based on a coating of animal bone waste for chromatographic analysis.

We attempt to introduce animal bone waste as a coating material with an organic-inorganic structure for the fabrication of a coiled solid-phase microextraction fiber for the first time. The coiled fiber was simply prepared with the use of copper wire and coated with bone waste suspension through the dip-coating method. The bone waste coating was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and X-ray diffraction analysis. It was applied as new type of solid-phase microextraction fiber for preconcentration of polycyclic aromatic hydrocarbons before determination by high-performance liquid chromatography with UV detection. A wide linear range 0.01-99.0 µg/L and limits of detection in the range 3.0-11.1 ng/L were obtained at optimized conditions. The bone waste coated coiled solid-phase microextraction fiber has promise in sample preparation techniques because it is cost effective, available, stable in aqueous and organic solutions, environmentally friendly, and easy to fabricate and operate.

Preparation of graphene oxide doped eggshell membrane bioplatform modified Prussian blue nanoparticles as a sensitive hydrogen peroxide sensor.

This study describes the preparation and characterization of graphene oxide doped eggshell membrane (GO-ESM) as a novel electrochemical bioplatform for electroanalytical purposes. The GO-ESM bioplatform was prepared by incorporation of GO nano-sheets into the ESM via a facile sonication procedure. Field emission scanning electron microscopy and X-ray diffraction powder techniques were used to characterize the developed bioplatform. The electrochemistry of GO-ESM was investigated by decorating it on the surface of carbon ceramic electrode (CCE) by an O-ring. The GO-ESM platform was modified with Prussian blue (PB) via a facile dip-coating method. Then the resulted modified electrode (PB|GO-ESM|CCE) was used as a novel hydrogen peroxide electrochemical sensor. The fabricated electrode responds efficiently to H2O2 over the concentration range 125nM-195µM with a detection limit of 31nM (S/N=3) and sensitivity 8.8µAµM(-1)cm(-2). The PB|GO-ESM|CCE has been successfully applied to determination of H2O2 content in spiked milk samples. Due to good stability, environmental friendly, cheapness, nontoxic, well behaved electrochemical properties, and biocompatibility, the fabricated bioplatform has the promising future for practical applications.

Desirability function approach for the optimization of an in-syringe ultrasound-assisted emulsification-microextraction method for the simultaneous determination of amlodipine and nifedipine in plasma samples.

In the present study, an in-syringe ultrasound-assisted emulsification-microextraction using a low-density organic solvent was developed for simultaneous extraction and pre-concentration of amlodipine besylate and nifedipine from plasma samples. The extracts were analyzed by high-performance liquid chromatography with UV detection. Central composite design combined with desirability function was applied to find out the optimal experimental conditions providing the highest global extraction efficiency. The optimal conditions identified were volume of the extracting solvent 45 µL, ionic strength 18.95% w/v, sonication time 2.58 min, and centrifugation time 3 min. Under the optimal conditions, the proposed method was evaluated, and applied to the analysis of amlodipine besylate and nifedipine in plasma samples. The validation results of the method indicated a wide linear range (2-1200 ng/mL) with a good linearity (r(2) >0.9991) and low detection limits (0.17 ng/mL for amlodipine besylate and 0.15 ng/mL for nifedipine) with RSD less than 5.2% for both components, both in intra- and inter-day precision studies. The applicability of the proposed in-syringe ultrasound-assisted emulsification-microextraction coupled to high-performance liquid chromatography with UV detection method was demonstrated by analyzing the drugs in spiked plasma samples.

D-penicillamine capped cadmium telluride quantum dots as a novel fluorometric sensor of copper(II).

D-penicillamine-capped cadmium telluride quantum dots (DPA-capped CdTe QDs) were synthesized as the new fluorescent semiconductor nanocrystal in aqueous solution. Fourier transmission infrared spectroscopy, X-ray diffraction, transmission electron microscopy, ultraviolet-visible and photoluminescence spectroscopy were used for characterization of the QDs. Based on the quenching effect of Cu(2+) ions on the fluorescence intensity of DPA-capped CdTe QDs, a new fluorometric sensor for copper(II) detection was developed that showed good linearity over the concentration range 5 × 10(-9)-3 × 10(-6) M with the detection limit 0.4 × 10(-9) M. Owing to the strong affinity of the DPA to copper(II), the sensor showed appropriate selectivity for copper(II) compared with conventional QDs. The DPA-capped CdTe QDs was successfully applied for determination of Cu(2+) concentration in river, well and tap waters with satisfactory results.

Graphene quantum dots as a new substrate for immobilization and direct electrochemistry of glucose oxidase: application to sensitive glucose determination.

Graphene quantum dots (GQD) were introduced as a novel and suitable substrate for enzyme immobilization. Glucose oxidase (GOx) was immobilized on GQD modified carbon ceramic electrode (CCE) and well-defined quasi-reversible redox peaks were observed. The UV-vis photoluminescence spectroscopy, transition electron microscopy, field emission scanning electron microscopy, electrochemical impedance spectroscopy, and cyclic voltammetry techniques were used for characterizing the electrochemical biosensor. The electron transfer coefficient (α) and the heterogeneous electron transfer rate constant (k(s)) for redox reaction of GOx were found to be 0.48 and 1.12 s(-1), respectively. The developed biosensor responds efficiently to glucose presence over the concentration range 5-1270 µM with the detection limit 1.73 µM (S/N=3) and sensitivity 0.085 µA µM(-1) cm(-2). The high value of surface coverage GOx-GQD|CCE (1.8×10(-9) mol/cm(2)) and the small value of Michaelis-Menten constant (0.76 mM) confirmed an excellent loading of the enzyme and a high affinity of biosensor to glucose. High performance of the biosensor is attributed to the large surface-to-volume ratio, excellent biocompatibility of GQD, porosity of GQD|CCE, and the abundance of hydrophilic edges as well as hydrophobic plane in GQD which enhances the enzyme absorption on the electrode surface.

Multi-response optimization of magnetic solid phase extraction based on carbon coated Fe3O4 nanoparticles using desirability function approach for the determination of the organophosphorus pesticides in aquatic samples by HPLC-UV.

The present study investigates the application of carbon coated Fe(3)O(4) (Fe(3)O(4)/C) magnetic nanoparticles as an adsorbent for magnetic solid phase extraction (MSPE) of trace amounts of organophosphorus pesticides (OPPs) from environmental water samples and their determination using high performance liquid chromatography with ultraviolet detection (HPLC-UV). The Fe(3)O(4)/C magnetic nanoparticles were synthesized by a simple hydrothermal reaction and the resultant material was characterized by X-ray powder diffraction, field emission scanning electron microscopy and Fourier transform infrared. Central composite design combined with desirability function (DF) was applied to find the experimental conditions providing the highest global extraction efficiency. These conditions were found in correspondence with a solution pH of 9.16, 97.4 mg Fe(3)O(4)/C and 10 mmol L(-1) NaCl added to samples. Under the optimal conditions, the proposed method was evaluated, and applied to the analysis of OPPs in water samples. The results demonstrated that our proposed method had wide dynamic linear range (0.05-400 ng mL(-1)) with a good linearity (R(2)>0.9949) and low detection limits (4.3-47.4 pg mL(-1)). High enrichment factors were achieved ranging from 330-1200. The established MSPE-HPLC-UV method has been successfully applied for the determination of the OPPs in spiked water samples (well, tap, river and mineral). Satisfactory recovery results showed that the matrices under consideration do not significantly affect the extraction process.