Sharif Digital Repository

Polystyrene is one of the best candidates as the extracting medium due to its high stability in different media and acceptable extraction capability. However, the hydrophobic nature and low wettability of polystyrene limits its application to non–polar analytes. To resolve this limitation, in this project, amine groups were chemically attached to the surface of magnetic polystyrene. The resulting hydrophilic magnetic particles were expected to be capable of extracting both polar and non–polar analytes. Non–steroidal anti–inflammatory drugs (NSAIDs) were chosen for testing the applicability of modified magnetic polystyrene according to the importance of their analysis and also their wide... 

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... 

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 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... 

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... 

Comprehensive two-dimensional gas chromatography and flame ionization detection combined with unfolded-partial least squares is proposed as a simple, fast and reliable method to assess the quality of gasoline and to detect its potential adulterants. The data for the calibration set are first baseline corrected using a two-dimensional asymmetric least squares algorithm. The number of significant partial least squares components to build the model is determined using the minimum value of root-mean square error of leave-one out cross validation, which was 4. In this regard, blends of gasoline with kerosene, white spirit and paint thinner as frequently used adulterants are used to make... 

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... 

An electro membrane extraction (EME) methodology was utilized to study the isolation of some environmentally important pollutants, such as chlorophenols, from aquatic media based upon the electrokinetic migration process. The analytes were transported by application of an electrical potential difference over a supported liquid membrane (SLM). A driving force of 10 V was applied to extract the analytes through 1-octanol, used as the SLM, into a strongly alkaline solution. The alkaline acceptor solution was subsequently analyzed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. The parameters influencing electromigration, including volumes and pH of the donor and... 

A highly sensitive and simple indirect spectrophotometric method has been developed for the determination of trace amounts of inorganic mercury (Hg2 +) in aqueous media. The method is based on the inhibitory effect of Hg2 + on the activity of horseradish peroxidase (HRP) in the oxidation of ascorbic acid by hydrogen peroxide followed by the reduction of Au3 + to Au-NPs by unreacted ascorbic acid and the measurement of the absorbance of localized surface plasmon resonance (LSPR) peak of gold nanoparticles (at 530 nm) which is directly proportional to the concentration of Hg2 +. Under the optimum conditions, the calibration curve was linear in the concentration range of 1-220 ng mL- 1. Limits... 

Dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry-selective ion monitoring (GC-MS-SIM) was applied to the determination of methyl tert-butyl ether (MTBE) in water samples. The effect of main parameters affecting the extraction efficiency was studied simultaneously. From selected parameters, volume of extraction solvent, volume of dispersive solvent, and salt concentration were optimized by means of experimental design. The statistical parameters of the derived model were R 2=0.9987 and F=17.83. The optimal conditions were 42.0μL for extraction solvent, 0.30mL for disperser solvent and 5% (w/v) for sodium chloride. The calibration linear range... 

Implementation of metal organic frameworks (MOFs) in the separation science has attracted many researchers attention. In this study, the role of metal, ligand, the reaction condition and modification on the extraction efficiency of some MOFs was investigated. Among the prevalent reported MOFs, some members of the MIL and MOF–5 families were chosen, and eleven MOF–based sorbents were prepared by changing the metal and ligand type, reaction condition, and/or functionality through post synthetic modification (PSM). MIL–101 and MIL–101–NH2 based structures were initially synthesized based on the chromium and iron salts. Also, three zinc–based structures including MOF–5, [NH2(CH3)2]2... 

Here, a three dimensional nickel–based metal organic framework (MOF) was synthesized via solvothermal and room temperature protocols. In order to study the effects of the synthesis conditions on the physical properties such as pore sizes and shapes of the prepared MOFs, their extraction capabilities were examined. Both MOFs were characterized by Fourier transform infrared spectroscopy, powder X-ray diffraction, scanning electron microscopy, Brunauer–Emmett–Teller and thermogravimetric analyses. Brilliant properties such as porous structure, high surface area and considerable thermal stability make them reasonable candidates to be employed as efficient extractive phases. The efficiency of the... 

In this study, cellulose acetate (CA) fibers were prepared using different solvent systems in electrospinning. The recorded scanning electron microscopy micrographs indicated that the morphology of the prepared fibers is closely associated with the type of electrospinning solvents. The prepared CA fibers were used as an extractive phase for on–line micro–solid phase extraction (μ-SPE) of nonsteroidal–inflammatory drugs (NSAIDs) in biological samples pursued by HPLC–UV determination. Work conducted on this research ascertained that the use of dichloromethane:acetone (3:1, v/v) solvent system in the CA dissolution for electrospinning, leads to the formation of porous ribbon–like fibers and... 

In this study, a method was described for the extraction of three antibiotic residues from cow milk samples using a graphene oxide–starch–based nanocomposite. The prepared nanocomposites were employed as an extractive phase for micro-solid phase extraction of antibiotics from cow milk samples. The extracted antibiotics, i.e. amoxicillin, ampicillin and cloxacillin, were subsequently analyzed by high-performance liquid chromatography–ultraviolet detection (HPLC–UV). Important variables associated with the extraction and desorption efficiency were optimized. High extraction efficiencies for the selected antibiotics were conveniently achieved using the starch–based nanocomposite as the... 

In this study, organic aerogels were synthesized by the sol-gel polycondensation of mixed cresol with formaldehyde in a slightly basic aqueous solution. Carbon aerogels and xerogels are generated by pyrolysis of organic aerogels. The novel sol-gel-based micro-solid-phase extraction sorbent, resorcinol-formaldehyde xerogel, was employed for preconcentration of some selected herbicides. Three herbicides of the aryloxyphenoxypropionate group, clodinafop-propargyl, haloxyfop-etotyl, and fenoxaprop-P-ethyl, were extracted from aqueous samples by micro-solid-phase extraction and subsequently determined by gas chromatography with mass spectrometry. The effect of different parameters influencing the... 

The aim of this study is to introduce an extractive phase based on gradient concept by continuous changing in chemical functional groups for non–targeted analysis. For this purpose, three different two–component coatings containing (3–aminopropyl)trimethoxysilane (APTES) as polar and either phenyltriethoxysilane (PTES), octyl–trimethoxysilane (OTMS) or methyltrimethoxysilane (MTMS) as nonpolar precursors were formed on the modified stainless steel wires using controlled rate infusion (CRI) method. The presence of polar and/or non–polar functional groups on the surface of substrate was evaluated by Fourier–transform infrared spectroscopy (FTIR) together with contact angles determined... 

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... 

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... 

We synthesized a titanium dioxide–polyaniline core–shell nanocomposite and implemented it as an efficient sorbent for the needle-trap extraction of some volatile organic compounds from urine samples. Polyaniline was synthesized, in the form of the emeraldine base, dissolved in dimethyl acetamide followed by diluting with water at pH 2.8, using the interfacial polymerization method. The TiO2 nanoparticles were encapsulated inside the conducting polymer shell, by adapting the in situ dispersing approach. The surface characteristics of the nanocomposite were investigated by Fourier transform infrared spectrometry, scanning electron microscopy, and transmission electron microscopy. After... 

In this research, an attempt was made toward synthesizing a sol–gel–based silica aerogel and its subsequent coating on a copper wire by phase separation of polystyrene. Adaption of this new approach enabled us to coat the metallic wire with powder materials. The use of this method for coating, led to the formation of a porous and thick structure of silica aerogel. The coated wire was placed in a needle and used as the sorbent for in–tube solid phase microextraction of chlorobenzenes (CBs). The superhydrophobicity of sorbent on extraction efficiency was investigated by using different ratios of tetraethylorthosilicate/methyltrimethoxysilane. The surface coated with the prepared silica aerogel...