Sharif Digital Repository

Multisensor arrays employing various sensing principles are a rapidly developing field of research as they allow simple and inexpensive quantification of various parameters in complex samples. Quantitative analysis with such systems is based on multivariate regression techniques, and deriving of traditional analytical figures of merit (e.g., sensitivity, selectivity, limit of detection, and limit of quantitation) for such systems is not obvious and straightforward. Nevertheless, it is absolutely needed for further development of the multisensor research field and for introducing these instruments into the general context of analytical chemistry. Here, we report on the protocol for... 

A horizontally oriented liquid-liquid-liquid microextraction (HOLLLME) setup was developed and applied for the isolation of two major estrogens from aquatic media. In contrast to the conventional procedure, in this setup the extracting microdrop was suspended from a horizontally positioned needle in order to provide much higher stability to the extracting phase. The developed HOLLLME approach was applied to isolate two major selected estrogens from aquatic media followed by high performance liquid chromatography-ultraviolet (HPLC-UV) determination. Estrogens were, initially, extracted from water samples into hexane and subsequently, the back extraction stage was performed with 6 μL of sodium... 

A novel solid-phase microextraction(SPME) fiber was prepared using sol-gel technology with ethoxylated nonylphenol as a fiber coating material. The fiber was employed to develop a headspace SPME-GC-MS method suitable for quantification of 13 polycyclic aromatic hydrocarbons (PAHs) in water samples. Surface characteristics of the fibers were inspected by energy dispersive X-ray (EDX) spectroscopy as well as by scanning electron microscopy (SEM). The SEM measurements showed the presence of highly porous nano-sized particles in the coating. Important parameters affecting the extraction efficiency such as extraction temperature and time, desorption conditions as well as ionic strength have been... 

A novel approach for highly sensitive detection of captopril was developed based on the fluorescence resonance energy transfer (FRET) between gold nanoparticles (Au NPs) and fluorescein isothiocyanate (FITC), in which FITC acts as the donor and Au NPs as the acceptor. The fluorescence intensity of fluorescein isothiocyanate (FITC) was strictly quenched as a result of noncovalently adsorbed on Au NPs. Upon the addition of captopril, the fluorescence intensity of FITC turn-on due to the competition between captopril and FITC towards the surface of Au NPs. Under the optimum conditions, the fluorescence intensity of the released FITC displays a linear relationship in the range of 20 μg L-1 to... 

This work describes a novel Fe3O4@SiO2@polypyrrole magnetic nanocomposite and its application in the preconcentration of Cd(ii) and Ni(ii) ions. The parameters affecting the preconcentration procedure were optimised by a Box-Behnken design using response surface methodology. Three variables (extraction time, magnetic sorbent amount, and pH) were selected as the main factors affecting the sorption step, while four variables (type, volume and concentration of the eluent, and elution time) were selected as the main factors in the optimisation study of the elution step. Following the sorption and elution of analytes, the ions were quantified by FAAS. The limits of detection were 0.3 and 1.2 ng... 

Levodopa [L-3, 4-dihydroxyphenylalanine, or L-DOPA] is an important neurotransmitter used for the treatment of neural disorders such as Parkinson's disease. Abnormal L-Dopa concentrations in biological fluids can be used for the evaluation of such diseases. In this work, a rapid and sensitive method for L-DOPA detection has been reported which is based on in situ formation of polylevodopa nanoparticles. Under alkaline conditions, L-DOPA is spontaneously oxidized to its quinone derivative and shows fluorescence properties. The fluorescence signal of the oxidation product has been monitored and used for the determination of L-DOPA in the presence of dopamine, uric acid, ascorbic acid and other... 

This paper describes the construction of a silver-based LSPR biosensor for endotoxin detection. We used GLAD method to procure reproducible silver nanocolumns. In this work, the silver nanostructures were considerably stabilized by a SAM of MPA, and the limit of detection of biosensor was measured to be 340 pg/ml for endotoxin E. coli. Considering endotoxin B. abortus as the second type of endotoxin contamination in our target samples (HBs-ag produced in Institute Pasteur, Iran), we investigated selectivity of the biosensor in various experiments. We showed that this biosensor can selectively detect both types of endotoxins compared to other biological species. Overall, this study proposes... 

Sol composition and ripening conditions are two important parameters in silica fiber production through the conventional sol-gel process. In the current study, silica nanofibers were successfully obtained via the electrospinning technique, and sol-gel formation occurred during this process. Based on previous reports, with the aim of increasing the selectivity, we used the molecular imprinted methodology to produce a selective medium via sol-gel electrospinning. In this process, sol-gel was formed during electrospinning and then, the backbone polymer was removed by heating. To obtain a thin layer of silica nanofibers, the influencing parameters such as backbone polymer types, imprinting time... 

For the rapid detection of hyperglycemia in human blood, we adopted a facile and two-step electrochemical procedure to prepare nickel/reduced graphene oxide (rGO) hybrid electrodes in the framework of a three-dimensional (3D) nanostructure. High-density and vertically-aligned nickel submicrorods with an average diameter of 155 ± 15 nm and a length of 7 ± 1 μm (an aspect ratio of about 40-50) were prepared by template-mediated electrochemical deposition techniques. Networks of rGO nanosheets between the rod-shaped arrays were formed by the cathodic electrophoretic deposition method. The synergistic effect of nickel morphology (planar and high-density rod-shaped arrays) and graphene oxide... 

Concentration procedures have always been implemented when trace analysis of compounds in real matrices is contemplated. A variety of concentration strategies have been reported aiming at decreasing the limits of detection (LODs). The optical concentration of the substance in solution is one of the novel concepts for the enhancement of the analytical sensitivity. In this study, the optical concentration has been measured by the trapping of gold nanoparticles ((Formula presented.) nm) dispersed in water at low-concentrations at the focal volume of the laser beam. The influence of factors such as the time of gold nanoparticle trapping, the size of the nanoparticles, the intensity of the laser... 

A novel modified electrode is reported for the electrochemical investigation of the oxidation mechanism and also voltammetric determination of raloxifene (RLX). The surface of the electrode was modified with a thin layer of reduced graphene oxide-carbon nanotube nano-composite (rGO-CNT) was prepared, and successfully employed for the electrochemical studies of RLX. The morphology of the sensor surface was characterized by using a scanning electron microscopy. RLX Oxidation response significantly increased at the GCE covered with rGO-CNT, regarding the bare and CNT or rGO functionalized GCE. Experimental parameters affecting the RLX response were optimized and mechanism of the RLX oxidation... 

Developing chemical sensors with pronounced sensitivity towards lanthanides is a very important task related to the analytical control of industrial processes in nuclear industry. Various diamides of organic acids were shown to be very effective for such sensing applications when employed as ligands in plasticized polymeric membranes of potentiometric sensors. The chemical structures of some of these ligands (diamides of diglycolic acid) are very similar to those suggested in 80’s as Ca(II) ionophores that were later commercialized. We have hypothesized that commercial ionophores ETH 129 (N,N,N′,N′-tetra[cyclohexyl] diglycolic acid diamide) and ETH 5234... 

The electrochemical behavior of lamotrigine (LMT) at the pyrolytic graphite electrode (PGE) is investigated in detail by the means of cyclic voltammetry. During the electrochemical reduction of LMT, an irreversible cathodic peak appeared. Cyclic voltammetric studies indicated that the reduction process has an irreversible and adsorption-like behavior. The observed reduction peak is attributed to a two-electron process referring to the reduction of azo group. The electrode showed an excellent electrochemical activity toward the electro-reduction of LMT, leading to a significant improvement in sensitivity as compared to the glassy carbon electrode. The results of electrochemical impedance... 

A headspace adsorptive microextraction technique was developed using a novel polyaniline-nylon-6 (PANI-N6) nanofiber sheet, fabricated by electrospinning. The homogeneity and the porosity of the prepared PANI-N6 sheet were studied using the scanning electron microscopy (SEM) and nanofibers diameters were found to be around 200nm. The novel nanofiber sheet was examined as an extracting medium to isolate some selected chlorobenzenes (CBs), as model compounds, from aquatic media. The extracted analytes were desorbed using μL-amounts of solvent and eventually an aliquot of extractant was injected into gas chromatography-mass spectrometry (GC-MS). Various parameters affecting the extraction and... 

An imprinted interpenetrating polymer network (IPN) was synthesized and used as a medium for isolation of carbamazepine from urine samples. The polymer network consisted of a homogeneous polystyrene–sol gel hybrid constructed by in–situ radical polymerization method. In this process, within the sol–gel reaction duration, styrene monomer could penetrate into the reaction mixture and after the polymerization initiation, a monolithic IPN structure was prepared. The scanning electron microscopy (SEM) image and energy dispersive spectroscopy (EDX) are indications of the polystyrene dispersion at nano- to micro-meter level in the sol gel matrix. Eventually, the synthesized IPN was used as a... 

A cryogel–based semi–interpenetrating polymer network (Cryo–SIPN) was prepared in which conductive polymers such as polyaniline (PANI) and polypyrrole (PPy) were formed within the super porous network of acrylic acid cryogel. For completion of cryo-polymerization, all the constituent solutions were severely mixed and placed into the plastic straws and kept at -20°C and then the synthesized cyrogels were cut into the 1-cm length and freeze dried after washing with water. The Cryo–SIPN polymeric composite was applied in micro solid phase extraction (µSPE) of some selected antibiotic residues from various samples. The µSPE method combined with a high performance liquid... 

Pyrrole was electro-polymerized on the surface of the glassy carbon electrode (GCE) coated with a thin film of carbon nanomaterials, including carbon nanotubes (CNTs), carbon nanoparticles (CNPs), nanodiamond-graphite (NDG) or graphite nanopowder (GNP). Morphology, thickness, stability and loading of the polypyrrole (PPY) film were significantly affected by the structure and morphology of the sub-layer of carbon nanomaterials. Electrochemical oxidation of atorvastatin (ATOR) was investigated. Under the optimized conditions, a significant increase in the peak current (compared to other modified electrodes and bare GCE) and a negative shift in the peak potential (compared to bare GCE) were... 

A rapid, convenient and reliable method for microextraction in packed syringe (MEPS) of the loop diuretic furosemide (FUR) in urine along with high-performance liquid chromatography (HPLC) was developed. A nanocomposite based on silver nanoparticles/polyaniline (Ag-NPs/PANI) was synthesized and used as the MEPS packing material. This nanocomposite was prepared conveniently using interfacial polymerization without the need for any templates or functional dopants. The feasibility of the synthesized nanocomposites was examined by isolation of FUR from diluted urine samples. After extraction, the analyte was desorbed by 200 μL of methanol. It was then dried and the residue was dissolved in 30 μL... 

An on-line extraction/determination set up was designed for micro solid-phase extraction of clodinafop propargyl from water, soil and wheat samples using electrospun polyamide nanofiber mats. The prepared mats were packed in a stainless steel tube which conveniently acted as a high-performance liquid chromatography injection loop. Influential parameters affecting the extraction efficiency were optimized using a distilled water sample fortified with 25 μg L-1 of clodinafop propargyl. An enrichment factor of 440 was achieved for clodinafop propargyl indicating the ability of the whole procedure. Under the optimum conditions, the linearity for the analyte was in the range of 6-700 μg L-1, while... 

Pichia pastoris is used extensively as a production platform for many recombinant proteins. The dissolved oxygen (DO) is one of the most important factors influencing protein production. The influence of the DO on productivity has not been studied independent from the feed rate. In this work, various DO levels were investigated independent from the feed rate. The model system was recombinant P. pastoris under the control of methanol-induced alcohol oxidase promoter, which expressed HRP as the target protein. No significant effect was observed in terms of titer and specific productivity, which is a confirmation of the fact that the DO in a one-compartment system cannot boost productivity for...