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  • Open access
  • 67 Reads
Reductive Properties of (4R,5R)-2,2-Dimethyl-1,3-Dioxolane-4,5-Bis(Diphenylmethylstannane)
Chiral organotin halides and hydrides have been widely investigated as chiral inductors for asymmetric synthesis. They have been used in a variety of reactions such as ketone reduction, alpha bromo esters reduction, radical cyclization of aldehydes, among others. Several chiral organotin hydrides are reported in literature, but to the best of our knowledge none of them have two tin hydrides moieties. So that, we were interested in the synthesis of (4R,5R)-2,2-dimethyl-1,3-dioxolane-4,5-bis(diphenylmethylstannane). The synthesis of this tin hydride was achieved in six steps starting from dimethyl-(L)-tartrate. The first attempt was to apply the new chiral organotin hydride in the reduction of prochiral ketones. We faced with several disadvantages in this reaction because stoichiometric amounts of the tin hydrides were needed to reduce ketones, and despite of this, the tin hydride was unable to reduce them completely. We decided to focus on the reduction of alpha bromo esters, inspired in the work of Metzger and co-workers. Alpha bromo esters can be reduced by using an organotin halide and NaCNBH3 as a source of hydride. In this condition, the organotin halide is used in catalytic amount. We permormed the reactions with 1, 5 and 10 mol% the organotin halide and the last conditions allowed the reaction to complete.
  • Open access
  • 73 Reads
Microwave Preparation of Uniform CeO2/Organo-Clay Nanoparticles and its Composition with Resin Epoxy
Organoclay is an organic-inorganic composite that is consists of layers of two tetrahedral silica sheets and one octahedral alumina sheet pillared by organic reagents to improve the physical and chemical properties. We report the synthesis of CeO2/organo-clay nanocomposite with a uniform distribution of particles in morphology by a programmed method of microwave heating reaction. Cerium nitrate hexahydrate as an initial metal source was added to the dispersed organoclay in aqueous solution and then transferred into a domestic microwave oven with a power of 900 W for 20 min. the synthesized nanocomposite was characterized by using Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion of x-ray spectrometry (EDX) techniques. XRD pattern clearly revealed the formation of the CeO2/ organoclay nanocomposite having pillared planes. Scanning electron microscopy (SEM) images of the resulting product indicated a uniform morphology of nano-sized particles with an average size of 33 nm. The composition of the resulting product into a matrix of resin epoxy in different weight ratios was studied.
  • Open access
  • 94 Reads
Validated Liquid Chromatography/Tandem Mass Spectrometry Method for Determination and Pharmacokinetic Study of Metolazone in Rat Plasma
A simple, highly sensitive and rapid LC-MS/MS method has been developed and validated for the quantification of metolazone in rat plasma using irbesartan as internal standard (IS). After simple protein precipitation extraction by acetonitrile, the analyte and IS were extracted from 50 μL plasma sample on an Agilent Poroshell 120, EC- C18 (50 mm × 4.6 mm, i.d., 2.7 μm) column using 5μL injection volume with a total run time of 2 min. Acidified methanol/water mixture was used as a mobile phase. The parent/product ion transitions for metolazone (m/z 366.1/258.9) and IS (m/z 429.2/207.0) were monitored on a triple quadrupole mass spectrometer, operating in the multiple reaction monitoring and positive ion mode. The method was found to be linear in the range of 0.05 – 200 metolazone. The method was validated with respect to selectivity, linearity, accuracy, precision, recovery and stability according to accepted regulatory guidelines. The described method was successfully applied to preclinical pharmacokinetic studies of analytes after an oral administration of metolazone (0.5 mg/kg) in rats.
  • Open access
  • 87 Reads
A Simplified Microwave-Assisted Synthesis of NiMoO4 Nanoparticles by Using Organic Driving Agent and Study of Photocatalytic Activity
Organic reagents can be used as a driving agent to synthesize a wide spectrum of nanomaterials.  In this work, nickel molybdate (NiMoO4) nanoparticles with a pure monoclinic crystalline phase were synthesized by using a facile one step microwave heating technique in solid state within a few minutes. Ammonium hepta molybdate tetrahydrate and nickel nitrate hexahydrate as initial materials were mixed to each other without any solvent and put into a domestic microwave oven with one step scheduled run. We introduced an alternative route of power input into chemical reactions in solid state by using microwave radiation.  In fact, the obtained results can draw an outlook of the effectiveness and feasibility of this technique for the synthesis of various nanoparticles. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion of x-ray spectrometry (EDX) were used to characterize the prepared product.  The study of photocatalytic behaviour of the resulting product indicated a high capability on the removal of Methylene Blue (MB) from aqueous solution.
  • Open access
  • 67 Reads
An Amperometric Glucose Sensor Based on Nickel Nanoparticle/Chitosan and Multiwall Carbon Nanotube on Modified Graphite Electrode
Many studies about providing suitable coating on the electrodes have been investigated. Electron transfer chemical and electrocatalysis properties are very important for them. Exact determination of glucose concentration is necessary for treatment of diabet and food industry.A novel Ni (Nickel)/CS(chitosan)/CNT(carbon nanotube) network nanocomposite was constructed on graphite electrode for glucose detection. Firstly, multi-walled carbon nanotubes were purified and characterized by Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM).Chitosan include excellent biocompatibility, biodegradability, nontoxicity, high mechanical strength, good adhesion and cheapness properties, therefore it has been used as an immobilization matrix. Although it has poor electrical conductivity, but it usually has been combined with carbon nanotubes, redox mediator and metal nanoparticles. Carbon nanotubes have been used in various sensors due to their unique properties such as high electronical and mechanical stability. Nickel hydroxide severely adsorbs some organic substances such as chitosan and has high electrocatalytical properties. Therefore, it has been used for preparation of modified electrodes. In this work, a film of Ni/CS/CNTs network was prepared for oxidation of glucose. The modified electrode with the Ni/CS/CNTs showed excellent electrocatalytical response to the oxidation, which was studied by cyclic voltammetry (CV). The synthesized biosensor exhibited rapid response, low detection limit, broad linear range, good reproducibility and stability.
  • Open access
  • 80 Reads
Optimization Process for Increasing the Yield of Crude Alkaloid from Litsea polyantha Juss. bark
Litsea polyantha Juss. (Lauraceae) also known as Litsea monopetala Roxb. is a small to medium sized evergreen tree distributed chiefly in tropical and subtropical Asia, Australia and the Pacific Islands. The bark of Litsea polyantha Juss. has a long history of medicinal use among the traditional healers of Oraon and Munda community of Jharkhand (India). In this work, optimization process for increasing the yield of crude alkaloid from Litsea polyantha Juss. bark was performed by taking pH and temperature as the factors influencing the yield. With the help of yield optimization by 22 factorial design the percentage yield of crude alkaloid was increased from 3.8% w/w to 17.3% w/w.
  • Open access
  • 240 Reads
Flavonoids and Phenolic Compounds from Litsea polyantha Juss. bark
Flavonoids and phenolic compounds from plants have been reported to have multiple biological effects. In the present communication, bioactive compounds from Litsea polyantha Juss. bark were studied. The total phenolic content was determined by using the Folin-Ciocalteu reagent and aluminum chloride colorimetric method was used for determination of total flavonoids. The content of phenolics in 100 gm (dry weight) extract of Litsea polyantha Juss. was 511.472 ± 22.304 mg gallic acid equivalent (GAE), while total flavonoid content was 230.785 ± 5.439 mg/g quercetin equivalent in MELP. Results obtained showed that the plant materials studied are a good source of phenolic and flavonoids compounds.
  • Open access
  • 65 Reads
Synthesis of Porphyrin- Graphene Oxide Nanocomposite for an Optical Chemical Sensor Application
In this project a new method by using graphene oxide nanosheets–porphyrin composites was presented as sorbents for the removal of toxic mercury ions from aqueous solutions. The compound has the ability to adsorb the organic and inorganic compounds. Herein, few layered graphene oxide nanosheets were synthesized from graphite using the modified Hummers and Offeman's method. 5, 10, 15, 20-tetrakis (4-hydroxyphenyl) porphyrin (THPP) was prepared using a modification of Adler–Longo method. Through the immobilization of THPP onto graphene oxide nanosheets, the desired composite was synthesized and identified by field emission scanning electron microscopy (FE-SEM), UV-Vis and Fourier transform infrared (FT-IR) spectroscopic techniques. The various experimental parameters such as pH and concentration of the aqueous solution of Hg (II), content of the THPP and the grapheme oxide have been optimized.  It was shown that the uptake efficiency of Hg (II) significantly increased after immobilization of porphyrin on the graphene oxide nanosheets.
  • Open access
  • 123 Reads
Synthesis, Characterization and Photocatalytic Activity of Porphyrin–Polyoxometalate Hybrid Material
In the present work, the preparation of an organic-inorganic hybrid material in which tetrakis phenylporphyrin is immobilized on the surface of polyoxometalate (H3PMo12O40) is reported. This porphyrin-polyoxometalate hybrid material was characterized by FT-IR and UV-Vis spectroscopic methods. The photocatalytic activity of this hybrid material was investigated in the photodegradation of methylene blue.
  • Open access
  • 89 Reads
Synthesis and Characterizationof Core-ShellFe3O4@Collagen Nanoparticle, and Application as Catalyst Ingreen Synthesis of Benzimidazoles and Benzithiazoles
Nanoparticles are nanostructures with at least one dimensionbeing less than 100 nm.In this research, nano magnetic Fe3O4@collagen was prepared and characterized by Fourier transforms infrared spectroscopy (FT-IR) spectra, Scanning electron microscopy (SEM) images, energy dispersive X-ray spectroscopy (EDX) spectra, X-ray diffraction (XRD) measurements.Fe3O4@collagen is a new and greennano catalysis and using in synthesis of benzimidazoles and benzithiazoles.This method offers several advantages including high yields, short reaction times, easy work up procedure, reusability of catalyst and environmentally benign reaction conditions.
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