Application of Supercritical fluid Extraction For Analysis of Organophosphates in Cereals

Abstract

Application of supercritical fluid extraction (SFE) utilizing pure carbon dioxide for selective isolation of organophosphates from contaminated cereals has been tested.

At the beginning of the experiments the extractability of added standards from an empty extraction vessel (thimble) and from various materials such as filter paper, sand, Celite and anhydrous sodium sulfate was tested to estimate the behavior of organophosphates. Further method development was carried out using a spiked sample of flour, which was analyzed within the proficiency testing for organophosphorus pesticides analysis (round 7) organized by Food Analysis Performance Assessment Scheme (FAPAS, MAFF-UK).

Comparison of the SFE method with a classical method currently employed for sample preparation (i.e. extraction with acetone/methanol mixture followed by gel permeation chromatographic clean up) showed advantages of the SFE technique such as simplification of the sample preparation step and thereby significant speeding up of the determination of organophosphates in cereals.     

Analysis of PCBs in Biotic Matrices by Two-Dimensional GC-ECD

Abstract

The suitability of three GC-ECD systems for the separation of a model mixture containing various congeners of PCBs together with persistent chlorinated aromatics (pesticides and their metabolites, industrial chemicals) was tested. Analyses were performed on two parallel capillaries, the stationary phase of one of them was always in routine practice very common 5% phenyl-methylpolysiloxane, the second one was either 50% phenylmethylpolysiloxane or 7% phenyl-7% cyanopropyl-methylpolysiloxane. The number of unresolved (coeluted) analytes was significantly reduced in these systems and thus unbiased quantitation of PCBs and other components used for regulation was possible. The utilization of this type of multidimensional chromatography for rapid and reliable analysis of real samples (fish oil, human fat) was documented.     

Design,preparation and characterization of Cu/GA/Fe3O4@SiO2 nanoparticles as a catalyst for the synthesis of benzodiazepines and imidazoles

The synthesis and characterization of an efficient and reusable nanocatalyst, Cu/GA/Fe₃O₄@SiO₂, obtained by ultrasonic‐assisted grafting of guanidineacetic acid on modified Fe₃O₄@SiO₂ core–shell nanocomposite spheres and subsequent immobilization of Cu(II), are described. The catalyst was characterized by means of X‐ray diffraction, scanning and transmission electron microscopies, energy‐dispersive X‐ray spectroscopy, elemental analysis, thermogravimetric analysis, Fourier transform infrared spectroscopy, vibrating sample magnetometry and inductively coupled plasma optical emission spectrometry. The prepared nanocatalyst facilitated an efficient and straightforward friendly procedure for the synthesis of benzodiazepines and imidazoles in ethanol and under solvent‐free conditions, respectively. The nanocatalyst can be easily recovered using a magnet and reused several times without any significant loss of activity. Copyright © 2016 John Wiley & Sons, Ltd.     

Use of nanoporous Na+-montmorillonite sulfonic acid (SANM) as an eco-benign, efficient and reusable solid acid catalyst for the one-pot synthesis of 14-aryl-14-H-dibenzo[a,j]xanthenes and 1,8-dioxo-dodecahydroxanthene derivatives

Nanoporous Na⁺-montmorillonite sulfonic acid was found to be an efficient and green catalyst for the synthesis of various 14-aryl-14H-dibenzo[a,j]xanthenes and 1,8-dioxo-dodecahydroxanthene derivatives by the reaction of aldehydes with 2-naphthol and 1,3-cyclohexanedione, respectively. This novel synthetic method has the advantages of high yields, short reaction times and recyclability of the catalyst, simplicity and easy workup compared to the conventional methods reported in the literature.     

Effect of Power Amplifier Nonlinearity on the Physical Layer Security of MIMO Systems

Wireless Personal Communications - This paper presents an analytical investigation on the effect of nonlinear high-power amplifiers on the physical layer security of multiple-input-multiple-output...     

Head-to-head bisbenzazole derivatives as antiproliferative agents: design,synthesis, in vitro activity,and SAR analysis

Molecular Diversity - In the present work, a series of bisbenzazole derivatives were designed and synthesized as antiproliferative agents. The antiproliferative activity of these compounds was...     

Novel palladium nanoparticles supported on β‐cyclodextrin@graphene oxide as magnetically recyclable catalyst for Suzuki–Miyaura cross‐coupling reaction with two different approaches in bio‐based solvents

A novel nanocatalyst was designed and prepared. Initially, the surface of magnetic graphene oxide (M‐GO) was modified using thionyl chloride, tris(hydroxymethyl)aminomethane and acryloyl chloride as linkers which provide reactive C═C bonds for the polymerization of vinylic monomers. Separately, β‐cyclodextrin (β‐CD) was treated with acryloyl chloride to provide a modified β‐CD. Then, in the presence methylenebisacrylamide as a cross‐linker, monomers of modified β‐CD and acrylamide were polymerized on the surface of the pre‐prepared M‐GO. Finally, palladium acetate and sodium borohydride were added to this composite to afford supported palladium nanoparticles. This fabricated nanocomposite was fully characterized using various techniques. The efficiency of this easily separable and reusable heterogeneous catalyst was successfully examined in Suzuki–Miyaura cross‐coupling reactions of aryl halides and boronic acid as well as in modified Suzuki–Miyaura cross‐coupling reactions of N‐acylsuccinimides and boronic acid in green media. The results showed that the nanocatalyst was efficient in coupling reactions for direct formation of the corresponding biphenyl as well as benzophenone derivatives in green media based on bio‐based solvents. In addition, the nanocatalyst was easily separable, using an external magnet, and could be reused several times without significant loss of activity under the optimum reaction conditions.     

The new method of fabrication of submicron structures by optical lithography with mask shifting and mask rotation

This paper presents the methods of fabricating narrow parallel submicrometric stripes in silicon dioxide and a resist layer. The experiments were conducted by two techniques: double patterning lithography and double exposure lithography. In addition to the above mentioned processes, mask translation was applied. For all conducted experiments, chrome masks and a 405 nm line of the high pressure mercury lamp of an MA-56 Mask Aligner System were used. The main aim of the performed tests was to establish the utility and the possible applications of the methods used.     

SBA-15-SO3H-assisted preparation of 4-aza-phenanthrene-3,10-dione derivatives via a one-pot,four-component reaction

Research on Chemical Intermediates - A novel four-component approach for the synthesis of 1-phenyl-1,4-dihydro-2H-9-oxa-4-aza-phenanthrene-3,10-dione derivatives has been presented via the reaction...