Sharif Digital Repository

A highly efficient and simple synthesis of unsymmetrical thioureas is reported based on the reaction of readily synthesized dithiocarbamates with amines, without using any catalyst under solvent-free conditions. The short reaction time, high yields, and solvent-free conditions are advantages of this method. We did not observe the formation of any symmetric disubstituted thiourea, under these reaction conditions. © 2008 Elsevier Ltd. All rights reserved  

An efficient method for the preparation of 2,3,5-trisubstituted thiophenes in a one-pot synthesis from thiomorpholides via the thio-Claisen rearrangement was developed. © 2003 Elsevier Ltd. All rights reserved  

Fructose is utilized as a common sweetener in many food industries. Today, a large amount of HFCS (high fructose corn syrup, an equilibrium mixture of glucose and fructose) is produced by glucose isomerase, immobilized enzymes from corn starch. There are a lot of date palms in Iran. Date is a favorable source of carbohydrates, and a suitable source for HFDS (high fructose date syrup) production. In this investigation, date syrup properties were first determined and the operational conditions for glucose isomerase application were optimized respectively. Ion exchange chromatography has been utilized for carbohydrate separation. Fructose obtained from chromatographic column reached 90 %... 

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 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 quantitative structure-retention relationships model has been developed to study the retention behavior of 87 aliphatic and aromatic compounds in Reversed-Phase Liquid Chromatography (RPLC) on five bonded-phase columns differing in silanol group acidity. Six numerical descriptors of Molecular Mass (M), partial charge of the most negative atom (NPCH), partial charge of the most positive hydrogen (PCHH), van der Waals volume (VOLUME), Dipole Moment (DIMO), and Highest Occupied Molecular Orbital (HOMO) have been calculated for each compound. A separate Multiple Linear Regression (MLR) model has been developed using the six descriptors for each column. Partial Least Square (PLS) combined with... 

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... 

Bio-inspired Human Serum Albumin (HSA) imprinted polydopamine nano-layer was produced through oxidative polymerization of dopamine on the pore surface of HSA modified porous silica particles. The coating thickness was controlled by the reaction time and thereby varied within 0-12. nm. The samples were characterized by elemental analysis, FT-IR, DSC, SEM, TEM, TGA, physisorption and thermoporometry. The characterization confirmed the success of evolution and deposition of polydopamine layer on the silica pore surface. Batch rebinding experiment showed that the molecularly imprinted polymer (MIP) with 8.7. nm coating thickness, in comparison with the thinner and thicker coatings, displays the... 

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... 

Gas chromatography-mass spectrometry (GC-MS) combined with Chemometric resolution techniques were proposed as a method for the analysis of volatile components of Iranian damask rose oil. The essential oil of damask rose was extracted using hydrodistillation method and analyzed with GC-MS in optimized conditions. A total of 70 components were identified using similarity searches between mass spectra and MS database. This number was extended to 95 components with concentrations higher than 0.01% accounting for 94.75% of the total relative content using Chemometric techniques. For the first time in this work, an approach based upon subspace comparison is used for determination of the chemical... 

Multivariate curve resolution (MCR) and multivariate clustering methods along with other chemometric methods are proposed to improve the analysis of gas chromatography-mass spectrometry (GC-MS) fingerprints of secondary metabolites in citrus fruits peels. In this way, chromatographic problems such as baseline/background contribution, low S/N peaks, asymmetric peaks, retention time shifts, and co-elution (overlapped and embedded peaks) occurred during GC-MS analysis of chromatographic fingerprints are solved using the proposed strategy. In this study, first, informative GC-MS fingerprints of citrus secondary metabolites are generated and then, whole data sets are segmented to some... 

In the present work, a new micro-solid phase extraction (μ-SPE) sorbent as an extracting medium based on core-shell nanofibers was synthesized by electrospinning. The core-shell nanofibers of polyvinylpyrrolidone-Polybutylene terephthalate/polypyrrole (PVP-PBT/PPy) were electrospun and subsequently, modified hollow nanofibers were prepared by removing the central PVP moiety. Moreover, conventional PBT/PPy was also prepared for the comparison purposes. The homogeneity and the porous surface structure of the core-shell nanofibers were confirmed by scanning electron microscopy (SEM). The applicability of the fabricated nanofibers-coating was examined by immersed μ-SPE of some selected triazine... 

A method based on direct immersion solid-phase microextraction (DI-SPME) coupled with high performance liquid chromatography combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection (HPLC-PIF-FD) was developed to extract three pyrethroid insecticides, i.e. cyfluthrin, cypermethrin, and flumethrin from water samples. A sol-gel based coating fiber using 3-(trimethoxysilyl propyl) amine as precursor was prepared and used for the extraction of the pyrethroids from groundwater samples. A post-column photochemical reactor was designed and constructed for the derivatization of these environmentally important pollutants to increase their fluorescence... 

The one-pot synthesis of a novel class of substituted quinoline derivatives with good yields is achieved via the Cu-catalyzed intramolecular C─H activation reaction between isocyanides, aniline, and acetylene dicarboxylate in MeCN at room temperature. The existence of one-pot conditions, availability of a starting material-catalyst, the absence of column chromatography, and a high yield of products are among the advantages of this method. The structures are confirmed spectroscopically (1H NMR and 13C NMR, IR, and EI-MS) and through elemental analyses  

A facile sonochemical route for the synthesis of benzo[1,3]thiazine derivatives via a one pot, multicomponent, intramolecular C–H activation reaction from isocyanides, aniline and benzoyl (acetyl) isothiocyanate adduct catalyzed by copper (I) iodide in acetone at 30 °C have been reported. The advantages of the described method include using simple and readily available starting materials and performing under mild copper-catalytic reaction conditions and also obtaining pure product with high yield without applying column chromatography. Furthermore, using the sonochemical methodology as an efficient method led to reduce the reaction times. © 2018 Elsevier B.V  

A facile sonochemical route for the synthesis of benzo[1,3]thiazine derivatives via a one pot, multicomponent, intramolecular C–H activation reaction from isocyanides, aniline and benzoyl (acetyl) isothiocyanate adduct catalyzed by copper (I) iodide in acetone at 30 °C have been reported. The advantages of the described method include using simple and readily available starting materials and performing under mild copper-catalytic reaction conditions and also obtaining pure product with high yield without applying column chromatography. Furthermore, using the sonochemical methodology as an efficient method led to reduce the reaction times. © 2018 Elsevier B.V