Sharif Digital Repository

Essential oils (EOs) are valuable natural products that are popular nowadays in the world due to their effects on the health conditions of human beings and their role in preventing and curing diseases. In addition, EOs have a broad range of applications in foods, perfumes, cosmetics and human nutrition. Among different techniques for analysis of EOs, gas chromatography-mass spectrometry (GC-MS) is the most important one in recent years. However, there are some fundamental problems in GC-MS analysis including baseline drift, spectral background, noise, low S/N (signal to noise) ratio, changes in the peak shapes and co-elution. Multivariate curve resolution (MCR) approaches cope with ongoing... 

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... 

Vacuum residue cracking has been successfully conducted under supercritical water condition in presence of various metal oxide nanocalysts, namely NiO, CuO, ZnO, Co2O3, and Cr2O3 synthesized at supercritical water. The cracking experiments were carried out at 450 °C. Three species of cracking: maltene, asphaltene, and coke were then weighed and their corresponding speciation was defined. Gas chromatography-mass spectrometry (GC–MS), nuclear magnetic resonance spectroscopy (NMR), thermogravimetric analysis (TGA), and elemental analysis (CHNS) tests were utilized to prove the performance of upgrading reactions. It was revealed that NiO showed the best performance among other catalyst, in which... 

A head-space solid-phase microextraction (HS-SPME) method coupled to GC-MS was developed to extract fentanyl from human plasma. The protein binding was reduced by acidification and, eventually, the sample was deproteinized with trichloroacetic acid. The parameters influencing adsorption (extraction time, temperature, pH and salt addition) and desorption (desorption time and temperature) of the analyte on the fibre were investigated and validated for method development. The developed method proved to be rapid, simple, easy and inexpensive and offers high sensitivity and reproducibility. Linear range was obtained from 0.1 ng/ml to 2 μg/ml. The limit of detection was 0.03 ng/ml while an... 

Scandium is a rare earth element that is not very abundant on Earth, however in recent years due to the employment of scandium in various high-tech fields the interest in the analytical chemistry of this metal is growing. Currently, the methods for scandium quantification are mainly based on inductively coupled plasma atomic emission and mass-spectrometry and to the best of our knowledge no potentiometric sensors for scandium detection were reported so far. This study is devoted to the development of simple and cost-effective ion-selective sensors for quantification of Sc3+ in aqueous media. Employing the variety of lipophilic ligands suggested in liquid extraction for separation of... 

Metabolomics is the science of studying small molecules (metabolites) in biological systems with the aim of getting insight into cells, biofluids and organisms. Chemometric methods are powerful tools to address data problems generated in metabolomic studies and to extract valuable information. This review focuses mainly on a range of chemometric methods used for processing of metabolomics data generated from gas chromatography-mass spectrometry (GC-MS) and comprehensive two-dimensional gas chromatography-mass spectrometry (GC × GC-MS). Herein, essential skills used for preprocessing of raw data, multivariate resolution, pattern recognition, variable selection and identification of... 

CaO derived from calcined eggshell was doped with Na–K by wet impregnation method and the effect of different Na/K molar ratios was investigated on biodiesel production from canola oil. The catalysts were characterized by X-ray Powder Diffraction (XRD), Brunauer–Emmett–Teller (BET), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray (EDX), and Thermogravimetric (TGA) analyses. FAME yields were determined by Gas Chromatography-Mass Spectrometry (GC-MS). The Na–K/CaO catalyst with Na/K molar ratio of 1 showed the highest FAME yield of 97.6% at optimum reaction conditions. Structural investigation of materials revealed that FAME yield was proportional to the number of basic sites on... 

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 analysis of complex natural matrices by gas chromatography-mass spectrometry (GC-MS), many disturbing factors such as baseline drift, spectral background, homoscedastic and heteroscedastic noise, peak shape deformation (non-Gaussian peaks), low S/N ratio and co-elution (overlapped and/or embedded peaks) lead the researchers to handle them to serve time, money and experimental efforts. This study aimed to improve the GC-MS analysis of complex natural matrices utilizing multivariate curve resolution (MCR) methods. In addition, to assess the peak purity of the two-dimensional data, a method called variable size moving window-evolving factor analysis (VSMW-EFA) is introduced and examined. The... 

In the present research, ultrasonic-assisted emulsification-microextraction (USAEME) coupled with gas chromatography-mass spectrometry (GC-MS) has been proposed for analysis of thirteen environmental protection agency (EPA) polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Tetrachloroethylene was selected as extraction solvent. The main parameters of USAEME affecting the efficiency of the method were modeled and optimized using a central composite design (CCD). Under the optimum conditions (9 μL for extraction solvent, 1.15% (w/v) NaCl (salt concentration) and 10min for ultrasonication time), preconcentration factor (PF) of the PAHs was in the range of 500-950. In order to have a... 

In order to improve the catalytic activity and durability of proton-exchange-membrane-fuel-cells (PEMFCs), Nafion-free Pt-based catalyst using the superacid-doped polymer coated multiwall carbon nanotubes (MWCNTs) was investigated. The modification and nano polymerization of MWCNTs were developed by polyvinylpyrrolidone (PVP). The following observations were made in the presence of polymer: better dispersion of MWCNTs, higher thermal stability of MWCNT/PVP than that of pristine MWCNT up to 450 °C as tested by thermal gravimetric analysis (TGA), homogeneous distribution of Pt without agglomeration as observed by transmission electron microscope (TEM), and not too much difference in Pt loading... 

The objective of the present work is development of joint approximate diagonalization of eigenmatrices (JADE) as a member of independent component analysis (ICA) family, for the analysis of gas chromatography-mass spectrometry (GC–MS) and comprehensive two-dimensional gas chromatography-mass spectrometry (GC × GC–MS) data to address incomplete separation problem occurred during the analysis of complex sample matrices. In this regard, simulated GC–MS and GC × GC–MS data sets with different number of components, different degree of overlap and noise were evaluated. In the case of simultaneous analysis of multiple samples, column-wise augmentation for GC–MS and column-wise super-augmentation... 

Enhancing stability against photocorrosion and improving photocurrent response are the main challenges toward the development of cupric oxide (CuO) based photocathodes for solar-driven hydrogen production. In this paper, stable and efficient CuO-photocathodes have been developed using in situ materials engineering and through gold-palladium (Au-Pd) nanoparticles deposition on the CuO surface. The CuO photocathode exhibits a photocurrent generation of ∼3 mA/cm2 at 0 V v/s RHE. Time-of-flight secondary ion mass spectrometry (TOF-SIMS) analysis and X-ray spectroscopy (XPS) confirm the formation of oxygen-rich (O-rich) CuO film which demonstrates a highly stable photocathode with retained... 

In this research, a new approach for extraction and determination of polycyclic aromatic hydrocarbons from sea and rain water samples was developed by implementing a superhydrophobic substrate and consuming the least amount of solvent. This version of solvent–supported microextraction enabled us to perform the procedure in the immersion mode with the slightest troubles arising from water leakage into the gas chromatography. The superhydrophobic property leads to the fixation of extracting solvent on the substrate surface during water sampling. To prepare a superhydrophobic substrate, a piece of melamine foam was coated by tannic acid and silica nanoparticles using methyltrimethoxysilane and... 

A novel amino-functionalized polymer was synthesized using 3-(trimethoxysilyl) propyl amine (TMSPA) as precursor and hydroxy-terminated polydimethylsiloxane (OH-PDMS) by sol-gel technology and coated on fused-silica fiber. The synthesis was designed in a way to impart polar moiety into the coating network. The scanning electron microscopy (SEM) images of this new coating showed the homogeneity and the porous surface structure of the film. The efficiency of new coating was investigated for headspace solid-phase microextraction (SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different...