Sharif Digital Repository

A multi-residue method using gas chromatography coupled with flame ionisation detector has been developed for simultaneous determination of 10 pesticides in milk. The methodology involved a sample clean-up procedure using ‘quick, easy, cheap, effective, rugged and safe’ followed by a preconcentration step based on dispersive liquid–liquid microextraction. In this regard, acetonitrile was added to the milk sample with specific pH and ionic strength, and the mixture was rigorously shaken. The extracts were centrifuged; then, the organic phase (acetonitrile) was transferred to a test tube and was mixed with deionised water. The mixture was sonicated and chloroform was added as an acceptor phase... 

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... 

Introduction: This report describes the synthesis of 2-Amino-2-deoxy(S- benzoylthioacetyl)-D-glucose (S-Bz-TA-DG), radiolabeled with [ 99mTc(CO)3(OH2)3]+ complex with a procedure including deprotection of the benzoyl group, characterization by HPLC using a C18 reverse phase column and preliminary biodistribution study in normal mice. Methods: [99mTc(CO) 3(H2O)3]+ complex was used to label TA-DG with 99mTc. This complex was prepared using up to 46 mCi of Na99mTcO4 in 1mL saline. The radiochemical purity (>95%) was determined by TLC in normal saline solution as the mobile phase. Radio-HPLC analysis of [99mTc]-(TA-DG) at pH=9.5-10, revealed that labeling with 99mTc resulted in the formation of... 

In this work a novel unbreakable sol-gel-based in-tube device for on-line solid phase microextraction (SPME) was developed. The inner surface of a copper tube, intended to be used as a high performance liquid chromatography (HPLC) loop, was electrodeposited by metallic Cu followed by the self assembled monolayers (SAM) of 3-(mercaptopropyl) trimethoxysilane (3MPTMOS). Then, poly (ethyleneglycol) (PEG) was chemically bonded to the -OH sites of the SAM already covering the inner surface of the copper loop using sol-gel technology. The homogeneity and the porous surface structure of the SAM and sol-gel coatings were examined using the scanning electron microscopy (SEM) and adsorption/desorption... 

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... 

Multivariate curve resolution-particle swarm optimization (MCR-PSO) algorithm is proposed to exploit pure chromatographic and spectroscopic information from multi-component hyphenated chromatographic signals. This new MCR method is based on rotation of mathematically unique PCA solutions into the chemically meaningful MCR solutions. To obtain a proper rotation matrix, an objective function based on non-fulfillment of constraints is defined and is optimized using particle swarm optimization (PSO) algorithm. Initial values of rotation matrix are calculated using local rank analysis and heuristic evolving latent projection (HELP) method. The ability of MCR-PSO in resolving the chromatographic... 

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... 

Liquid-liquid-liquid microextraction (LLLME) in combination with HPLC and UV detection has been used as a sensitive method for the determination of ephedrine in urine samples. Extraction process was performed in a homemade total glass vial without using a Teflon ring, usually employed. Ephedrine was first extracted from 3.5 mL of urine sample (pH 12) into a microfilm of toluene/benzene (50:50). The analyte was subsequently back extracted into an acidic microdrop solution (pH 2) suspended in the organic phase. The extract was then injected into the HPLC system directly. An enrichment factor of 137 along with a good sample clean-up was obtained under the optimized conditions. The calibration... 

The simultaneous oxidation performance of benzene, toluene, ethylbenzene, and xylene (BTEX) by nanoscale calcium peroxide particles (nCaO2) activated with ferric ions (Fe(III)) and the mechanism of the enhancement of BTEX degradation by L-cysteine (L-cys) were investigated. The batch experimental results showed that the nCaO2/Fe(III)/L-cys process was effective in the destruction of BTEX in both ultrapure water and actual groundwater. A proper amount of L-cys could enhance BTEX degradation due to the promotion of Fe(II)/Fe(III) redox cycles by the participation of L-cys, but an excessive presence of L-cys would cause inhibition. Adding 1.0 mM L-cys to the nCaO2/Fe(III) system, the... 

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... 

Ultrafine particles of paracetamol were produced by Rapid Expansion of Supercritical Solution (RESS). The experiments were conducted to investigate the effects of extraction temperature (313353K), extraction pressure (1018MPa), preexpansion temperature (363403K), and postexpansion temperature (273323 K) on particles size and morphology of paracetamol particles. The characterization of the particles was determined by Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Liquid Chromatography/Mass Spectrometry (LC-MS) analysis. The average particle size of the original paracetamol was 20.8m, while the average particle size of paracetamol after nanonization via the... 

Experimental design of directly suspended droplet liquid-liquid-liquid microextraction has been used to determine residue of 2,4-D, in environmental water samples. A free suspended droplet of 5.5 μL of receiving phase is delivered to the top-center position of 1-Octanol, which is an immiscible organic solvent, floating on the top of a 2.5 mL aqueous sample while being agitated by a stirring bar to create a mild vortex at the center of the vial. Central composite rotatable design has been used for studying the effect of the parameters, the factors interacting with each other and finding the optimum condition. The chromatographic separation was accomplished on a shim-Pak C18 column using a... 

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... 

This paper describes the development and implementation of MCRC software, chemometric software for Multivariate Curve Resolution of two-way Chromatographic data. MCRC software is developed for chemometric analysis of chromatographic data; however, it may also be used for other types of multivariate data. It consists of five groups of techniques for preprocessing, chemical rank determination, local rank analysis, multivariate resolution and peak integration. This software has the ability of the analysis of complex multi-component chromatographic signals of gas chromatography-mass spectrometry (GC-MS) and high performance liquid chromatography-diode array detection (HPLC-DAD). The software... 

Introduction - Recently, there have been growing attention on the modification and optimisation of new extraction and quantification methods, caused by the lack of environmentally friendly methodologies for the extraction of phytochemicals from complex matrices. In the case of pharmaceutical compounds, not only the extraction procedure but also the analysis method should be efficient, precise, fast and easy.Objectives - The essential pharmaceutical characteristics and trace concentration of withanolides led us to modify and optimise the previously reported extraction and quantification procedure for withaferin A (WA) as a candidate for withanolides.Matrial and methods - The WA from the... 

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...