Magnetic molecularly imprinted polymer nanoparticles for dispersive micro solid-phase extraction and determination of buprenorphine in human urine samples by HPLC-FL

A simple, sensitive and accessible while reliable method was developed and validated for quantitation of buprenorphine (Bup) as a highly lipophilic drug in human urine samples. The proposed method is based on a rapid and easy dispersive micro solid-phase extraction procedure using magnetic molecularly imprinted polymer nanoparticles (MMIPNPs), magnetite (Fe₃O₄) cores surrounded by polyamidoamine and Bup as template, followed by high-performance liquid chromatographic analysis with fluorescence detector (HPLC-FL). The prepared MMIPNP adsorbent was characterized by different techniques. Transmission electron microscopy images show that the Fe₃O₄ core nanoparticles are well enwrapped by MIP layers. In determination process, Bup could be quantitatively extracted using MMIPNPs and then can be easily desorbed by mixture of sodium hydroxide (0.1 mol/L) and methanol (1:9, v/v) solution before injection to HPLC. The relative recoveries of Bup were found to be 97.4–100.3%, and the linear dynamic range was within the ranges of 1–1000 ng/mL with R² of 0.9998. Remarkably high quality of 0.21 and 0.71 ng/mL was obtained as the limit of detection and limit of quantification, respectively. The developed method was successfully applied for determination of Bup in infected human urine samples.     

Reaction Between 5-Isopropylidene-2,2-dimethyl-1,3-dioxane-4,6-dione and <Emphasis Type="Italic">tert</Emphasis>-Butyl Isocyanide in the Presence of Primary or Secondary Amines

Summary. 5-Isopropylidene-2,2-dimethyl-1,3-dioxane-4,6-dione (the condensation product of Meldrums acid and acetone) reacts smoothly with tert-butyl isocyanide in the presence of primary or secondary amines to produce N-tert-butyl-2,2-dimethylbutyramide derivatives and/or 1-tert-butyl-4,4-dimethyl-2,5-dioxopyrrolidine-3-carboxamides in good yields.     

Redetermination de la structure cristalline du tetrafluoroantimonate III de sodium NaSbF4 - interaction liaison fluor-paire electronique libre

The crystal structure of NaSbF₄ has been redetermined by X-ray diffraction. The coordination about antimony is AX₆E with a 2.2.2.1 geometry. The units are linked by fluorine bridges and form a double layer perpendicular to the a axis. Infrared and Raman spectra were recorded and are discussed in terms of the distorted octahedral arrangement of fluorines about each antimony.     

Efficient synthesis of novel tricyclic fused pyranothiazolopyrimidine derivatives via isocyanide-based three-component reactions

An efficient and facile one-pot synthesis is described for the preparation of novel tricyclic fused pyranothiazolopyrimidines containing both biologically active thiazolopyrimidine and pyranopyrimidine templates via three-component reaction involving an isocyanide with a dialkylacetylenedicarboxylate (DAAD) and 2,3-dihydro-5H-[1,3]thiazolo[3,2-a]pyrimidine-5,7(6H)-dione, in high yields.     

Synthesis of 1‐(2,6‐Dimethylphenyl)‐N‐hydroxy‐4,4‐dialkyl‐2,5‐dioxo‐N‐aryl‐3‐pyrrolidine‐carboxamides from Reaction of 2,6‐Dimethylphenyl Isocyanide,Alkylidene Meldrum's Acids,and Arylhydroxylamines

Alkylidene Meldrum's acids and 2,6‐dimethylphenyl isocyanide react smoothly in the presence of arylhydroxylamines at room temperature to produce 2,5‐dioxo‐pyrrolidines in fairly high yield.     

Polypyrrole/Fe3O4/CNT as a recyclable and highly efficient catalyst for one‐pot three‐component synthesis of pyran derivatives

Polypyrrole (PPY)/Fe₃O₄/CNT has been synthesized and characterized by FT‐IR, TEM and SEM techniques and its catalytic activity has been evaluated in the synthesis of several series of pyran derivatives. Tetrahydrobenzo[b]pyranes, 4H‐pyran‐3‐carboxylates, 4H,5H‐pyrano[3,2‐c]chromenes and dihydropyrano[2,3‐c]pyrazoles have been successfully prepared from one‐pot three‐component condensation of aldehyde, malononitrile and active methylene‐containing compounds (dimedone /ethyl acetoacetate/4‐hydroxycoumarin/3‐methyl‐2‐pyrazoline‐5‐one) using PPY/Fe₃O₄/CNT as a new and reusable heterogeneous catalyst. The present method offer several advantages such as; high yields of products, short reaction times, easy work‐up procedure and easy separation of the catalyst from the reaction mixture due to its magnetic character. Furthermore, chemoselective synthesis of bis‐benzo[b]pyran from terephthalaldehyde can be achieved by this method.     

The reduction of 4‐nitrophenol and 2‐nitroaniline by palladium catalyst based on a KCC‐1/IL in aqueous solution

KCC‐1/IL/Pd NPs can used as an excellent support for the synthesis of highly sparse homogeneous catalyst. KCC‐1 has high surface area that was functionalized with ionic liquid phase acting as the strong performers so that the Pd catalyst was well‐dispersed without aggregation on the framework of the KCC‐1/IL. This nano catalyst was specified by TGA, XRD, TEM, SEM, FT‐IR, and ICP. For reduction of 2‐nitroaniline and 4‐nitrophenol used from the KCC‐1/IL/Pd NPs as a green catalyst that showed excellent catalytic activities. Compared with the traditional substrate, KCC‐1 substantially increases protection and the accessibility of the nanoparticle sites due to its three dimensional hierarchical structure.     

Graphite disk Lanthanum(III)-selective electrode based on Kryptofix-22DD

ABSTRACT

A novel ion-selective electrochemical sensor based on kryptofix-22DD (1,10-didecyl-1,10-diaza-18-crown-6) as an ionophore was constructed for determination of lanthanum(III) cation in solutions. The D-Optimal Mixture Design(D-OMD) was used as an experimental design strategy for optimal formulation of the membrane ingredients, and the actual values of the ingredients were compared with their predicted values. The amounts of the ionophore, plasticizer, PVC, and also the graphite powder which influence the performance of the fabricated electrode were analyzed using D-OMD. A non-linear relationship was observed between the slope of the electrochemical response of the electrode and these variables and the interaction between the variables as well. The experimental results showed that the amount of the ionophore has the most positive effect on the electrochemical response of the electrode. The constructed electrode exhibits a Nernstian slope (20.60 ± 0.21 mv.decade^?1) in a wide linear concentration range from 1.0 × 10^?7 to 1.0 × 10^?1 M with respect to La³⁺ cation at pH range of 4.0 to 6.0, and its detection limit was found to be:0.8 × 10^?7M. The selectivity of the proposed electrode towards some of the metal cations present in lanthanum(III) cation solutions was tested, and the experimental results showed a good selectivity towards this metal cation.