Sharif Digital Repository

A fast high-performance liquid chromatography-diode array detection (HPLC-DAD) approach combined to solid phase extraction (SPE) as a pre-concentration step is developed for simultaneous determination of five selected pharmaceuticals (carbamazepine, naproxen, diclofenac, gemfibrozil and mefenamic acid) in water samples. The effective factors on the efficiency of SPE procedure are optimized using faced-centered central composite design (FCCD). In addition, multi-response optimization by using Derringer's desirability function is used to find the optimum experimental conditions for extraction of analytes from well and river waters. Due to the complexity of water matrices and the presence of... 

For the first time, a new platform based on electrochemical growth of Au nanoparticles on aligned multi-walled carbon nanotubes (A-MWCNT) was developed for sensitive lable-free DNA detection of the TP53 gene mutation, one of the most popular genes in cancer research. Electrochemical impedance spectroscopy (EIS) was used to monitor the sequence-specific DNA hybridization events related to TP53 gene. Compared to the bare Ta or MWCNT/Ta electrodes, the synergistic interactions of vertically aligned MWCNT array and gold nanoparticles at modified electrode could improve the density of the probe DNA attachment and resulting the sensitivity of the DNA sensor greatly. Using EIS, over the extended... 

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 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... 

Titanium(IV) tetraisopropoxide was employed as a metal oxide sol-gel precursor to prepare ceramic composite nanofibers by the electrospinning system. To facilitate this process and obtain the desired nanofibers with higher aspect ratios and surface area, poly(vinylpyrrolidone) was added to the sol of titania. Four ceramic nanofibers sheets based on titania were prepared while each sheet contained different transition metals such as Fe-Mn, Fe-Ni, Fe-Co, and Fe-Mn-Co-Ni. The scanning electron microscope images showed good homogeneity for all the prepared ceramic composites with a diameter range of 100-250 nm. The sorption efficiency was investigated by a micro-solid-phase extraction setup in... 

A solution of polyamide (PA) containing polyethylene glycol (PEG) as a side low-molecular-weight polymer was electrospun. After synthesizing the PA-PEG nanofibers, the constituent was subsequently removed (modified PA) and confirmed by Fourier transform infrared spectroscopy. The scanning electron microscopy images showed an average diameter of 640 and 148 nm for PA and PA-PEG coatings, respectively, while the latter coating structure was more homogeneous and porous. The extraction efficiencies of PA, PA-PEG, and the modified PA fiber coatings were assayed by headspace solid-phase microextraction of a number of chlorophenols from real water samples followed by their determination by gas... 

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... 

Intracellular production of recombinant proteins in prokaryotes necessitates subsequent disruption of cells for protein recovery. Since the cell disruption and subsequent purification steps largely contribute to the total production cost, scalable tools for protein release into the extracellular space is of utmost importance. Although there are several ways for enhancing protein release, changing culture conditions is rather a simple and scalable approach compared to, for example, molecular cell design. This contribution aimed at quantitatively studying process technological means to boost protein release of a periplasmatic recombinant protein (alkaline phosphatase) from E. coli.... 

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... 

The present work deals with a novel approach for grafting a sol-gel based sorbent, using diazonium salts for preparation of an unbreakable capillary microextraction (CME) device in on-line combination with high performance liquid chromatography (HPLC). The use of diazonium salts modifier allowed all types of metallic and non-metallic substrates to be used without any limitation. Substrates including copper, brass, stainless steel and polytetrafluoroethylene (PTFE) were chosen to be functionalized by chemical or electrochemical reduction of 4-amino phenyl acetic acid. Then, 3-(trimethoxysilyl)propylamine (3TMSPA) was selected as the precursor and the only reagent for preparation of the... 

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 Fe3O4-poly(aniline-naphthylamine)-based nanocomposite was synthesized by chemical oxidative polymerization process as a magnetic sorbent for micro solid phase extraction. The scanning electron microscopy images of the synthesized nanocomposite revealed that the copolymer posses a porous structure with diameters less than 50nm. The extraction efficiency of this sorbent was examined by isolation of rhodamine B, a mutagenic and carcinogenic dye, from aquatic media in dispersion mode. Among different synthesized polymers, Fe3O4/poly(aniline-naphthylamine) nanocomposite showed a prominent efficiency. Parameters including the desorption solvent, amount of sorbent, desorption time, sample... 

A novel high-throughput device based on 96-micro-solid phase extraction (96-μ-SPE) system was constructed for multiresidue determination of nine pesticides in aquatic samples. The extraction procedure was performed on a commercially available 96-well plate system. The extraction module consisted of 96 pieces of 1cm×3cm of cylindrically shaped stainless steel meshes. The prepared meshes were fixed in a home-made polytetrafluoroethylene-based constructed ninety-six holes block for possible simultaneous immersion of meshes into the center of individual wells. Dodecyl methacrylate and ethylene glycol dimethacrylate was copolymerized as a monolithic polymer and placed in the cylindrically shaped... 

This paper presents a new method for spectrophotometirc detection of sulfide applying fungal peroxidase immobilized on sodium alginate. The sensing scheme was based on decrease of the absorbance of the orange compound, purpurogallin produced from pyrogallol and H2O2 as substrates, due to the inhibition of peroxidase by sulfide. Absorbance of purpurogallin was detected at 420nm by using a spectrophotometer. The proposed method could successfully detect the sulfide in the concentration range of 0.6-7.0μM with a detection limit of 0.4μM. The kinetic parameters of Michaelis-Menten with and without sulfide were also calculated. Possible inhibition mechanism of peroxidase by sulfide was deduced... 

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... 

A new sensor for simultaneous determination of peroxyacetic acid and hydrogen peroxide using silver nanoparticles (Ag-NPs) as a chromogenic reagent is introduced. The silver nanoparticles have the catalytic ability for the decomposition of peroxyacetic acid and hydrogen peroxide; then the decomposition of them induces the degradation of silver nanoparticles. Hence, a remarkable change in the localized surface plasmon resonance absorbance strength could be observed. Spectra-kinetic approach and artificial neural network was applied for the simultaneous determination of peroxyacetic acid and hydrogen peroxide. Linear calibration graphs were obtained in the concentration range of (8.20×10-5 to... 

The electrooxidation of clozapine (CLZ) was studied on the surface of a glassy carbon electrode (GCE) modified with a thin film of multiwalled carbon nanotubes (MWCNTs)/new coccine (NC) doped polypyrrole (PPY) by using linear sweep voltammetry (LSV). The pH of the supporting electrolyte (D), drop size of the cast MWCNTs suspension (E) and accumulation time of CLZ on the surface of modified electrode (F) was considered as effective experimental factors and the oxidation peak current of CLZ was selected as the response. By using factorial-based response-surface methodology, the optimum values of factors were obtained as 5.44, 10 μL and 300 s for D, E and F respectively. Under the optimized... 

A method based on solid-phase microextraction (SPME) followed by on-fiber derivatization and gas chromatography-mass spectrometry detection (GC-MS) for determination of phenol in air was developed. Three different types of SPME fibers, polar and non-polar poly(dimethylsiloxane) (PDMS) and polyethylene glycol (PEG) were synthesized using sol-gel technology and their feasibility to the sampling of phenol were investigated. Different derivatization reagents for post on-fiber derivatization of phenol were studied. Important parameters influencing the extraction and derivatization process such as type of fiber coating, type and volume of derivatizing reagent, derivatization time and temperature,... 

A simple, rapid and sensitive method based on microextraction in packed syringe (MEPS), in combination with gas chromatography-mass spectrometry (GC-MS) was developed. Polyaniline (PANI) nanowires network was synthesized and used as sorbent of MEPS for the multiresidue determination of selected analytes from triazine, organochlrorine and organophosphorous pesticides in aqueous samples. The PANI nanowires network was prepared using soft template technique and its characterization was studied by scanning electron microscopy (SEM). The presence of micelles in this methodology showed to be an important parameter in shaping the growing polymer. Hexadecyltrimethylammonium bromide (HTAB) was used...