Sharif Digital Repository

Lung cancer (LC) is the leading cause of cancer mortality so, the analysis of exhaled human breath has great significance for early non-invasive diagnosis. Poor selectivity and strong humidity are two bottlenecks for the application of gas sensors to exhaled breath analysis. The development of novel extractive phases for the analysis of exhaled breath by chromatography is therefore a lucrative object. Polyhedral oligomeric silsesquioxanes (POSS) are among the 3D porous materials whose unique properties make them promising coatings for solid-phase microextraction (SPME). Selective enrichment of polar or nonpolar targets depends on the pore size and functional groups on the POSSs. Herein, we... 

Ionic liquids are a significant type of organic salts with attractive and superior physicochemical features for employing in a number of chemical processes. Ionic liquids include one large and asymmetric cationic or anionic functional group. The properties of cationic functional group are almost similar and it is main motivation of this study. In the present investigation, we extended various semi-empirical correlations to predict some temperature-based properties of ionic liquids mixture (IL-mixture). These properties are density, viscosity, surface tension and bubble point pressure. In the case of IL-mixture density, modified Rackett equation and Taylor equation with three scenarios,... 

A stable porous zinc-based metal organic framework (MOF) containing nitrogen-rich bis-tetrazolate ligand was synthesized to study the role of similar structures concerning both extractive phase and the desired solutes to achieve greater sorption efficiency. With implementing a dispersive micro-solid phase extraction (d-µ-SPE) methodology, the sorption capability and influencing structural parameters i.e., porosity, surface area and interactions types were investigated for the synthesized zinc-bis-tetrazolate (ZnBT) MOF and compared with some synthesized sorbents such as MIL-101, MIL-101-NH2, cadmium naphthalene dicarboxylic acid dimethyl formamide [Cd(NDC)(DMF)], polyaniline and LiChrolut®... 

Biomass, originates from plant- or animal-based materials with a huge potential to be reused. Here we report a simple, rapid and inexpensive method for preparation of modified biochars derived from the banana peel followed by their applications in pipette-tip micro solid-phase extraction (PT-µSPE). Due to the contribution of various effective parameters on modification of banana peel biochars (BPBs), Taguchi design was used to optimize activation temperature, activation repetition, treatment material and impregnation ratio. Efficiency of the prepared BPBs were studied by extraction of twelve various pesticides, as model analytes with an extended range of log P values (1.4–5.7), followed by... 

Low accuracy, requirement of expensive instruments, derivatization and multi-step sample preparation, inconsistencies during the fabrication process, time-consuming procedures and utilization of eco-unfriendly chemicals are some limitations of various developed methods for detection of 4-methylimidazol (4-MeI). Herein, a rapid and miniaturized fluorescent probe based on the ultrasound‒assisted formation of carbon dots (CDs) in a metallic deep eutectic solvent (MDES) was developed and conveniently implemented to detect 4-MeI in commercial dark soft drinks. In-situ synthesis of CDs-chelated metals in the presence of the target analyte facilitates a kinetically fluorescence emission with no... 

In the present work, with the focus on an environmentally–friendly approach, some gels were prepared by synthesizing amine–modified lignin, extracted from sugarcane bagasse, and further esterification and subsequent freeze–drying. These lignin–based gels were implemented as extractive phases in an online micro–solid phase extraction (μSPE) setup in conjunction with high performance liquid chromatography (HPLC) with UV detector. The developed method was used for analytical determination of valsartan and losartan in urine samples. To study the effect of the functionalization process, the efficiency of the unmodified lignin and the functionalized lignin were compared both in the absence and the... 

A cryogel–based semi–interpenetrating polymer network (Cryo–SIPN) was prepared in which conductive polymers such as polyaniline (PANI) and polypyrrole (PPy) were formed within the super porous network of acrylic acid cryogel. For completion of cryo-polymerization, all the constituent solutions were severely mixed and placed into the plastic straws and kept at -20°C and then the synthesized cyrogels were cut into the 1-cm length and freeze dried after washing with water. The Cryo–SIPN polymeric composite was applied in micro solid phase extraction (µSPE) of some selected antibiotic residues from various samples. The µSPE method combined with a high performance liquid... 

A gradient derived base layer extractive phase was synthesized and applied for the determination of volatile organic compounds (VOCs) in saliva samples using the headspace cooled in–tube microextraction (HS–CITME) method. The base layers from three different sols of phenyltriethoxysilane (PTES), octyltrimethoxysilane (OTMS) and methyltrimethoxysilane (MTMS) as nonpolar precursors were individually dip coated on the stainless steel wires (SSW). Then, the hydrolyzed polar precursor aminopropyltriethoxysilane (APTES) reacted with the silanol groups already formed on the surface of SSWs via controlled rate infusion (CRI) method. The presence of polar and non–polar functional groups on the... 

Herein, some (modified) paper–based substrates were prepared and utilized as extractive phases in a microfluidic device and their extraction performances examined for analytes with different polarities. Reagents including hexadecyltrimethoxysilane (HDTMS), phenyltrimethoxysilane (PTES), (3-aminopropyl) triethoxysilane (APTES) and 3–(2,3–epoxypropoxy) propyltrimethoxysilane (EPPTMOS) were implemented for the modification process. Due to the induction of different silane functional groups, it was anticipated to have various interactions for the tested analytes. Eventually, the prepared paper sheets were used as extractive phases for solid–phase extraction within a microfluidic system. The... 

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... 

A superhydrophobic extractive phase was prepared and packed in a needle trap microextraction device for extraction of volatile organic compounds, followed by their determination by gas chromatography. The superhydrophobic phase was prepared by surface modification of melamine formaldehyde (MF) sponge embedded by reduced graphene oxide (rGO). The overall properties of the modified MF along with its high sorption capacity and low cost fabrication were indicative of its feasibility to be highly suitable for extraction of organic pollutants. The determined water contact angle (>150o) from the surface of melamine formaldehyde–reduced graphene oxide (MF–rGO) revealed its high affinity toward... 

In this survey, a reliable and applicable Y–Y shaped micro–channel in a microfluidic device was designed and manufactured. A number of micro–scaled hedges were precisely fabricated inside the micro–channel to facilitate the immobilization of synthesized core–shell Fe3O4@SiO2 magnetic nanoparticles (MNPs), functionalized by triethoxyphenylsilane (TEPS) by sol-gel technique. Both sample and reagents were introduced into the microfluidic device by a syringe pump to perform the extraction and desorption steps. The functionalized MNPs were characterized by transmission electron microscopy, X-ray diffraction spectroscopy and Fourier transform infrared spectroscopy. By adopting the strategy of... 

A turn-on fluorometric assay is described for determination of the activity of enzyme telomerase. For this purpose, graphene quantum dots (GQDs) were first modified with the telomeric sequence (5′-amino-AATCCGTCGAGCAGAGTT-3′) via a condensation reaction. Injection of graphene oxide causes instant quenching of the blue fluorescence of the GQDs. Addition of cell extract containing telomerase, triggers the extension of telomer via addition of specific sequence (TTAGGG)n to its 3′ end. Fluorescence, best measured at excitation/emission wavelengths of 390/446 nm, is subsequently restored due to folding of the extended telomeric sequence into G-quadruplex structure. The method was applied to the... 

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 this study, firstly, a double-reservoir and switchable prototype of a micro-chip along with the respective holders were fabricated. A cyclic desorption process using microliter volume of organic solvent was adopted to prevent any outdoor contamination. As extractive phases, two identical sheets of electrospun polyamide/polypyrrole/titania nanofibers were synthesized using core–shell electro-spinning technique and utilized for determination of memantine in plasma samples. Field emission scanning electron microscopy images showed a high degree of porosity and homogeneity throughout the sheet structure. Also, energy dispersive X-ray analysis confirmed the presence of titania, while the... 

Sample preparation for non-target analysis is challenging due to the difficulty in the extraction of polar and non-polar analytes simultaneously. Most commercial solid sorbents lack the proper comprehensiveness for extraction of analytes with different physiochemical properties. A possible key is the combination of hydrophobic polymer and hydrophilic surface functional groups in solid based extraction methods in order to generate the susceptibility for retaining both polar and non-polar analytes. To pursue this goal, in this study, four polar groups including [sbnd]NH 2 , [sbnd]NO 2 , [sbnd]COOH, and [sbnd]COCH 3 were chemically bound to Amberlite XAD-4 substrate in order to prepare a... 

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 survey, firstly, a silicon wafer-based microchip, possessing a 50-cm microchannel with the dimensions of 120 and 60 μm, was manufactured by chemical etching technique. Subsequently, the inner surface of the microchannel was coated with a primary layer of gold nanoparticles synthesized by galvanic displacement. Then a self-assembled monolayer of 3-mercaptopropyltriethoxysilane was immobilized on the first layer. Eventually, a polydimethylsiloxane film with a thickness of 16 ± 1 μm was formed on the walls of the microchannel by means of sol-gel method. Field emission scanning electron microscopy and atomic force microscopy were extensively employed to investigate the status of both... 

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...