Sharif Digital Repository

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 new and convenient format of single drop microextraction (SDME) was developed and applied for isolation of some selected aryloxyphenoxypropionate herbicides from aquatic media. In contrast to the conventional SDME procedure, in this set-up the extraction microdrop was positioned at the bottom of a conical vial in order to provide much higher stability for the organic extraction phase while a magnetic bar was used for stirring the aqueous solution. A simple magnet was used for positioning the bar on the top of the microdrop prior to stirring. The whole set-up led to the use of any volume of extraction solvent with unlimited stirring rates. Some important extraction parameters such as the... 

A magnetic polyurethane (PU) nanocomposite was synthesized by an electrospinning technique and applied for isolation and preconcentration of fluoxetine from aquatic and biological samples. The nanocomposite was electrospun using a PU polymer solution containing the dispersed magnetic nanoparticles. The magnetic properties of iron nanoparticles, along with the use of an electrospinning technique, led to the formation of a suitable sorbent toward isolation of fluoxetine. The magnetic PU nanofibers could be subsequently removed from the sample solution by applying a permanent magnet. The scanning electron microscopy (SEM) image of the magnetic PU nanofibers confirms that their diameters are in... 

The objective of the work ahead is presentation of a new carbon paste electrode (CPE) modified by TiO2 nanoparticles (TiO2NPs) and 1,2-bis-[o-aminophenyl thio] ethane (APTE) ligand as a selective cation receptor for determination of the Cd (II) ions using differential pulse anodic stripping voltammetry (DPASV). The electrode shows an excellent tendency to Cd (II) ions in presence of some interfering species. Under the optimum conditions, a linear calibration curve was obtained in the concentration range of 2.9 nM to 4.6 μM with a correlation coefficient of 0.9969 in the anodic potential of 0.54 (V vs. Ag/AgCl). The metal detection limit was 2.0 nM after 10 min preconcentration (S/N = 3). The... 

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... 

A high-temperature-resisant solid-phase microextraction (SPME) fiber was prepared based on polyetherimide (PEI) by the electrospinning method. The PEI polymeric solution was converted to nanofibers using high voltages and directly coated on a stainless steel SPME needle. The scanning electron microscopy images of PEI coating showed fibers with diameter range of 500-650 nm with a homogeneous and smooth surface morphology. The SPME nanofibers coating was optimized for PEI percentage, electrospinning voltage, and time. The extraction efficiency of the coating was investigated for headspace SPME of some environmentally important polycyclic aromatic hydrocarbons from aqueous samples followed by... 

An immersed solvent microextraction (SME) method was successfully developed for the trace enrichment of aryloxyphenoxypropionate herbicides from aquatic media. A microdrop of toluene was used as the extraction solvent. Some important extraction parameters such as type of solvent, solvent dropsize, stirring rate, ionic strength and extraction time were investigated and optimized. The microdrop volume of 1.5 μL, a sampling time of 25 min, and use of toluene were major parameters for achieving high enrichment factors. The linearity was studied by preconcentration of 4 mL of the water samples spiked with a standard solution of aryloxyphenoxypropionates at the concentration range of 0.15 to 30 ng... 

Multivariate curve resolution-alternating least squares (MCR-ALS) as a second-order calibration algorithm was proposed for the simultaneous analysis of eighteen fatty acid methyl esters (FAMEs) in a standard mixture and pomegranate seed sample using vortex-assisted extraction-dispersive liquid-liquid microextraction (VAE-DLLME), followed by gas chromatography-mass spectrometry (GC-MS). The chemometric resolution, identification and quantification of the target FAMEs in the standard mixture and real sample (i.e., the pomegranate seed) were carried out successfully in the presence of some uncalibrated interferences. The lack of fit (LOF) and reverse match factor (RMF) were used for the... 

In recent years, there has been an increasing interest in the analysis of the major active components of saffron owing to their significant role in various industries, such as food, medicine and perfume. In other words, analysis of the major active components of saffron can give complete information about its chemical composition, which can be used as a reliable index for the quality control of different saffron samples (i.e., natural and commercial). The aim of the present work was to develop a simple, low cost, efficient and comprehensive strategy for the extraction and analysis of the bioactive components of saffron. In this regard, ultrasonic-assisted solvent extraction (UASE) combined... 

In this study, a fast and sensitive flow injection μ-solid phase extraction (FI-μ-SPE) technique based on an electrospun polyaniline (PANI) nanocomposite in conjunction with gas chromatography-mass spectrometry (GC-MS) was developed. The PANI-based nanocomposite was synthesized by electrospinning of a solution containing polyvinyl alcohol (PVA)/PANI. The majority of PVA template was subsequently removed from the whole PVA/PANI nanofibers blend by exposing the electrospun nanocomposite to hot water. The homogeneity, porosity and characterization of the electrospun nanofibers were investigated by the scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR) spectroscopy. Due to... 

An inexpensive silicon rubber-based chip was constructed by fabricating a triangle-shaped microcanal with a 135 μm width and 234 μm depth by laser ablation technique. The fabricated groove was sealed by a thin glass cover while two pieces of stainless-steel tubing were connected to each side of the canal. Then, a thin polyaniline film was synthesized on the walls of the canal by chemical oxidation using a syringe pump to deliver the relevant reagents. The microfluidic system was eventually connected to a gas chromatography-mass spectrometry. To evaluate the capability of the constructed microfluidic system, it was implemented to the analysis of submilliliter volumes of environmental samples... 

A superhydrophobic polystyrene hollow fiber was electrospun around a copper spring collector. This approach led to the construction of a hollow fiber membrane, and the copper spring acted as a scaffold. The characteristic properties of the hollow fiber were studied by scanning electron microscopy. The membrane was used as a probe to transfer the extracting solvent from aquatic media to a gas chromatograph. After performing the liquid–liquid microextraction procedure on 10 mL of water sample by octanol, the whole solution was passed through the prepared polystyrene hollow fiber. Propanol, containing 2 mg/L lindane as the internal standard, was used for desorption and an aliquot of 2 μL of the... 

A magnetic nanocomposite consisting of nanoparticles–polybutylene terephthalate (MNPs–PBT) was electrospun and used as an extracting medium for an on-line μ-solid phase extraction (μ–SPE)–high performance liquid chromatography (HPLC) set–up with an ultraviolet (UV) detection system. Due to the magnetic property of the prepared nanofibers, the whole extraction procedure was implemented under an external magnetic field to enhance the extraction efficiencies. The developed method along with the synthesized nanocomposite were found to be appropriate for the determination of trace levels of selected drugs including furosemide, naproxen, diclofenac and clobetasol propionate in the urine sample.... 

Hydrogen storage/evolution behavior of nafion/NaCl/graphene quantum dot (GQD) mixed matrix as selective hydrogen capacitor (power source) was evaluated in detail through an electrochemical process at two independent potential ranges. For this purpose, a three-electrode system included Pt disk as counter electrode, Ag/AgCl as reference electrode and GQD-based mixed matrix-modified Pt disk as working electrode. For hydrogen storage, the deposition potential and time were evaluated to −1.0 V (vs. Ag/AgCl) and 120 s, respectively under high basic solution generated using NaOH (1.0 M) solution, followed by evolution of hydrogen at +0.8 V (vs. Ag/AgCl) during formation of hydrogen bubbles. The... 

Molecularly imprinted polymer (MIP) was synthesized through the coprecipitation method on the graphene oxide anchored pencil lead as a substrate for the first time and applied as an efficient sorbent for pseudo stir bar sorptive extraction of nabumetone. The extracted analyte was determined by a novel spectrophotometric method based on the aggregation of silicate sol-gel stabilized silver nanoparticles in the presence of the analyte. The synthesized polymer was characterized using Fourier transform infrared spectroscopy and field emission scanning electron microscopy. Optimization of important parameters affecting the extraction efficiency was done using central composite design whereas the... 

This work presents a novel melatonin sensor based on unfunctionalized macroporous graphene networks decorated with gold nanoparticles for the differential pulse voltammetric detection of melatonin in pharmaceutical products. Highly porous graphene structures were prepared by metallic template-assisted chemical vapor deposition, and their active surface area and electrocatalytic activity were improved by electrochemical deposition of gold nanoparticles (50-250 nm) on their struts. The graphene-gold electrodes present a highly sensitive performance toward electro-oxidation of melatonin with a wide linear range of 0.05-50 μM, a low detection limit of 0.0082 μM (3σ/m), and a significant... 

Fluopyram, flupyradifurone, and indaziflam are novel systemic pesticides developed by Bayer. Based on available data, these pesticides appears to have a favorable safety profile in the case of pesticide residue problems. Herein, we report an effective analytical method for the determination of novel pesticides were developed using ultra-high performance liquid chromatography with tandem mass spectrometry coupled with a quick, easy, cheap, effective, rugged, and safe procedure. These target compounds were extracted with acetonitrile and cleaned up with PSA, and were separated successfully between 10.2 and 18.3 min using a C18 chromatographic column connected to an electrospray ionization... 

In salting-out liquid-liquid extraction (SALLE) technique, water-miscible organic solvents are used for extraction of polar analytes from saline solutions. In this study, for the first time, a coupled 1-mL syringes system was utilized to perform a miniaturized SALLE method. Sulfanilamide antibiotic was extracted and determined via the developed method followed by high performance liquid chromatography-ultraviolet detection (HPLC-UV). The extraction process was carried out by rapid shooting of acetonitrile as extraction solvent (syringe B) into saline aqueous sample solution (syringe A), and then the shooting was repeated several times at a rate of 1 cycle s-1. Thereby, an extremely large... 

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... 

Comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS) combined to multivariate curve resolution-alternating least-squares (MCR-ALS) is proposed for the resolution and quantification of very complex mixtures of compounds such as polycyclic aromatic hydrocarbons (PAHs) in heavy fuel oil (HFO). Different GC × GC-TOFMS data slices acquired during the analysis of HFO samples and PAH standards were simultaneously analyzed using the MCR-ALS method to resolve the pure component elution profiles in the two chromatographic dimensions as well as their pure mass spectra. Outstandingly, retention time shifts within and between GC × GC runs were not affecting...