Pd Nanocatalyst Adorned on Magnetic Chitosan@N-Heterocyclic Carbene: Eco-Compatible Suzuki Cross-Coupling Reaction.

A novel magnetic-functionalized-multi-walled carbon nanotubes@chitosan N-heterocyclic carbene-palladium (M-f-MWCNTs@chitosan-NHC-Pd) nanocatalyst is developed in two steps. The first step entails the fabrication of a three-component cross-linking of chitosan utilizing the Debus-Radziszewski imidazole approach. The second step comprised the covalent grafting of prepared cross-linked chitosan to the outer walls of magnetically functionalized MWCNTs (M-f-MWCNTs) followed by introducing PdCl2 to generate the m-f-MWCNTs@cross-linked chitosan with a novel NHC ligand. The repeated units of the amino group in the chitosan polymer chain provide the synthesis of several imidazole units which also increase the number of Pd linkers thus leading to higher catalyst efficiency. The evaluation of catalytic activity was examined in the expeditious synthesis of biaryl compounds using the Suzuki cross-coupling reaction of various aryl halides and aryl boronic acids; ensuing results show the general applicability of nanocatalyst with superior conversion reaction yields, high turnover frequencies (TOFs) and turnover numbers (TON). Meanwhile, nanocatalyst showed admirable potential in reusability tests, being recycled for five runs without losing significant activities under optimum reaction conditions. The successfully synthesis of catalyst and its characterization was confirmed using the Fourier transform infrared spectrometer (FT-IR), spectrometer transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photo-electron spectroscopy (XPS) and thermogravimetric analysis (TGA).

Isolation and identification of two alkaloid structures with radical scavenging activity from Actinokineospora sp. UTMC 968, a new promising source of alkaloid compounds.

For decades, natural products from Actinomycetes have been recognized as one of the inestimable sources of therapeutic compounds. Presently, due to some challenges in the identification of novel compounds including the validation of novel natural products and their compatibility with the high throughput screening bioassays, evaluating new activity from known commercial ones would be an important designation. On the other hand, finding new sources of bioactive compounds from Actinomycetes can be promising in attaining pharmaceutical compounds with fewer purification steps and cost-effective production of the bioproducts. Here we describe the isolation and identification of two alkaloid compounds from a soil actinobacterium Actinokineospora sp. UTMC 968 including N-acetyltyramine (1) and N-acetyltryptamine (2) with revealing a new bioactivity for these molecules. The producer is a rare actinobacterium belonging to family Pseudonocardiaceae as the first alkaloid compounds producer genus in its family. The structures of alkaloid 1 and 2 were assigned on the basis of 1D and 2D NMR spectroscopy and MS analyses. Compound 1 and 2 are used commercially for their pharmaceutical activity but their radical scavenging activity has not previously been reported. The results of 1,1-diphenyl-2-picrylhydrazyl radical scavenging assay represented a remarkable DPPH radical scavenging capability with an IC50 value of 64.7 ± 0.5 and 131.3 ± 1.8 µg/mL for compound 1 and 2, respectively.

Highly selective and sensitive recognition of multi-ions in aqueous solution based on polymer-grafted nanoparticle as visual colorimetric sensor.

A novel, selective and sensitive colorimetric sensor for naked-eye detection and adsorption of multi-ions in aqueous solution was synthesized using hybridization of organic-inorganic phase. The polymer-grafted nanoparticles (PGNPs) was synthesized via atom transfer radical polymerization (ATRP) of monomers on modified TiO2 NPs and applied under optimized conditions for naked-eye detection: sensor mass: 15 mg; response time: 30 s with limits of detection (LODs) as small as 10, 1, 0.5, and 1 ppb Hg (II), Cd (II), Cu (II), and UO2 (II) at pH = 8, 9, 6, and 7, respectively. The efficient selectivity of the naked eye sensor to multi-ions in the presence of various ions was affirmed wherein the color of the chemosensor in the presence of Hg (II), Cd (II), Cu (II), and UO2 (II) shifted from gray to violet, orange, green and yellow, respectively. The salient advantages of this method comprise expeditious, selectable, high reproducibility, with reasonable adsorption capacity (133 mg g-1) and inexpensive nature for rapid detection of heavy metal ions contamination in aqueous solution in an inexpensive manner. The adsorption mechanism was studied via adsorption kinetics and adsorption isotherm models and the accuracy of the chemosensor has been confirmed and supported by XRD, FT-IR, TGA, 1H-NMR, SEM, TEM, EDX mapping, DLS, BET, and EDS analysis.

PEGylated Pemetrexed and PolyNIPAM Decorated Gold Nanoparticles: A Biocompatible and Highly Stable CT Contrast Agent for Cancer Imaging.

This study describes a multifunctional nanoparticle platform for targeted CT imaging and therapy of cancers. Pemetrexed (conjugated with polyethylene glycol, MW 2000 Da) and polyNIPAM (PEGylated) were designed for targeted delivery to folate receptors and thermally ablated tumors, respectively. These moieties were coated on gold nanoparticles (7 and 30 nm), and the prepared compounds were characterized using 1H NMR, FT-IR, CHNS, DLS, TEM, TGA, and UV-vis. The resulting agents exhibited 2-4 times higher X-ray attenuation compared to Visipaque and demonstrated specific accumulation in tumor tissue (4T1 xenograft model) 90 min after injection in mice. The nanoparticles displayed anticancer activity against 4T1 and MDA-MB-231 breast cancer cells (IC50: 182.87 and 206.18 µg/mL) and good biocompatibility. Importantly, the platform showed excellent stability over a year and at pH 2-12 and temperature range of -78 to 40 °C, and a water-dichloromethane extraction method was optimized for efficient purification, facilitating large-scale production.

Applications of Cu(0) encapsulated nanocatalysts as superior catalytic systems in Cu-catalyzed organic transformations.

Recently, Cu nanoparticles (NPs) encapsulated into various materials as supports (e.g., zeolite, silica) have attracted much devotion due to their unique catalytic properties such as high catalytic activity, intensive reactivity and selectivity through highly protective properties. Nowadays, the superior catalytic activity of Cu-NPs, encapsulated onto zeolite, silica and different porous systems, is extensively investigated and now well-established. As a matter of fact, Cu-NPs are protected from deactivation by this kind of encapsulation. Thus, their exclusion proceeds smoothly, and their recyclability is significantly increased. Cu-NPs have been used as potential heterogeneous catalysts in different chemical transformations. In this review, we try to show the preparation and applications of Cu(0) encapsulated nanocatalysts in zeolite and silica as superior catalytic systems in Cu-catalyzed organic transformations. In addition, the catalytic activity of these encapsulated Cu-NPs in different important organic transformations (such as hydrogenation, oxidation and carbon-carbon bond formations) are compared with those of a variety of organic, inorganic and hybrid porous bearing a traded metal ion. Moreover, the results from the TGA/DTA analysis and optical properties of Cu-complexes are demonstrated. The inherited characteristic merits of the encapsulated Cu-NPs onto zeolite and silica, such as their low leaching, catalytic activity, reusability economic feasibility and originality are critically considered.

Efficient Optical and UV-Vis Chemosensor Based on Chromo Probes-Polymeric Nanocomposite Hybrid for Selective Recognition of Fluoride Ions.

A novel colorimetric sensor based on the TiO2/poly(acrylamide-co-methylene bis acrylamide-co-2-(3-(4-nitro-phenyl)thioureido)ethyl methacrylate) nanocomposite was synthesized via a surface modification strategy; methacryloxypropyltrimethoxysilane was used to provide reactive vinyl groups on the surface of TiO2 nanoparticles for the successful surface polymerization of Am (acrylamide), MBA (methylenbisacrylamide), and NPhM (2-(3-(4-nitrophenyl)thioureido)ethyl methacrylate) components. The successful preparation of nanocomposites was confirmed using Fourier transform infrared, 1H NMR, 13C NMR, scanning electron microscopy, transmission electron microscopy, thermogravimetry analysis, and X-ray diffraction methods, and the sensing ability of the probe toward fluoride ions was investigated using naked-eye detection and UV-vis measurement. The interaction of the prepared polymeric nanocomposite with fluoride ions elicited a significant visible change in color from pale yellow to orange and was further affirmed by a clean interconversion of the two absorption bands at 330 and 485 nm. The selective binding ability of the polymeric nanocomposite towards fluoride over other anions, such as I-, Cl-, Br-, AcO-, H2PO4 -, and H2SO4 - was further explored; the prepared chemosensor could detect fluoride ions in acetonitrile with a detection limit of 3 µM.

Novel magnetic ion-imprinted polymer: an efficient polymeric nanocomposite for selective separation and determination of Pb ions in aqueous media.

A novel ion-imprinted polymer (IIP) toward Pb(II) recognition was synthesized on the surface of magnetic multi-walled carbon nanotubes (magnetic MWCNTs). In order to prepare magnetic functionalized-MWCNT/IIP (magnetic f-MWCNT/IIP), copolymerization of methylenebisacrylamide (MBAm) and acrylamide (AM) in the presence of dithizone-Pb(II) complex was carried out on the surface of the magnetic f-MWCNTs. Selectivity of the new synthesized sorbent toward Pb(II) and the influence of a variety of foreign ions on the recognition, preconcentration, and removal of Pb(II) were evaluated using adsorption experiments in aqueous solution. The synthesized sorbent exhibited a good affinity with high adsorption capacity (Q = 80.81 mg/g) and an excellent selectivity toward Pb(II) in comparison with other common cations including alkaline, alkaline earth, and transition metals such as Na+, K+, Mg2+, Ca2+, Cd2+, and Ni2+. The parameters such as adsorption and desorption time, adsorption capacity, effect of the sorbent mass, eluent type, concentration and volume, and also pH of the solutions were investigated. The result demonstrated that the proposed sorbent provided a fast removal and higher maximum binding capacity compared to other reported synthesized sorbents. The characteristics of the magnetic f-MWCNT/IIP were analyzed using Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD), energy-dispersive spectroscopy (EDS), vibrating sample magnetometer (VSM), and elemental analysis (EA). Graphical abstract ᅟ.

Thermo-responsive molecularly imprinted polymer containing magnetic nanoparticles: Synthesis, characterization and adsorption properties for curcumin.

A novel intelligent thermoresponsive-magnetic molecularly imprinted polymer (TMMIP) nanocomposite based on N-isopropylacrylamide (NIPAM) & Fe3O4 was designed for the controlled & sustained release of Curcumin (CUR) with the ability to response external stimulus. The TMMIP nanocomposite was prepared using acryl functionalized ß-cyclodextrin (ß-CD) and NIPAM as functional monomers and CUR as target molecule. The recognition cavities which caused by host-guest interactions had direct influence to enhanced drug loading and sustained release of CUR. According to in-vitro release experiment in two different temperatures (below & above LCST of NIPAM) the prolonged & controlled release of CUR were observed. The release rate could be controlled by changing the temperature because of the phase transition behavior of NIPAM monomer. Also, the proposed biosensor displayed effective role in separation science, reasonable adsorption capacity (77mgg-1), fast recognition (10min equilibration), selective extraction toward CUR in the presence of structural analogues and easily separation using external magnetic field. Moreover, the synthesized TMMIP was confirmed by various characterization.

Novel molecularly imprinted polymer based on ß-cyclodextrin@graphene oxide: Synthesis and application for selective diphenylamine determination.

A sensitive and selective molecularly imprinted polymer (MIP) for the determination of diphenylamine (DPA) was developed based on host-guest interactions of a cyclodextrin-based polymer which possesses an inherent affinity for the target. The proposed GO@MIP has been prepared using the graphene oxide (GO) sheets as surface of polymerization, DPA as target molecule, ß-cyclodextrin (ß-CD) and acrylamide (AM) as functional monomers, azobisisobutyronitrile (AIBN) as initiator and N, N methylene bisacrylamide (MBAm) as crosslinker which denoted as GO@MIP nanocomposite. The MIP sites were formed by the inclusion complex through interaction of DPA and ß-CD, followed by extraction of target. The resulting GO@MIP nanocomposite possess a fast adsorption kinetics, highly improved imprinting effect, high adsorption capacity, and it can be applied to fast extraction of DPA. The resultant GO@MIP nanocomposite was characterized using the Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA) scanning electron microscope (SEM) and energy-dispersive spectroscopy (EDS) analysis. On the other hand, the non-imprinted polymer (GO@NIP nanocomposite) has been synthesized and was used in the adsorption experiments. The MIP exhibited good affinity with a maximum adsorption capacity of 95.98mgg-1 and excellent selectivity toward DPA than other structural analogues such as 2-amino benzophenone and dithizone.

Effect of Coriandrum sativum hydroalcoholic extract and its essential oil on acetic acid- induced acute colitis in rats.

OBJECTIVE: The aim of this study was to determine the protective effects of Coriandrum sativum on acetic acid-inducedcolitis in rats. C. sativum (Coriander) has long been used in Iranian traditional medicine and its use as an anti-inflammatory agent is still common in some herbal formulations. MATERIALS AND METHODS: Colitis was induced by intra-rectal administration of 2ml acetic acid 4% in fasted male Wistar rats. Treatment was carried out using three increasing doses of extract (250, 500, 1000 mg/kg) and essential oil (0.25, 0.5, 1 ml/kg) of coriander started 2 h before colitis induction and continued for a five-day period. Colon biopsies were taken for weighting, macroscopic scoring of injured tissue, histopathological examination and measuring myeloperoxidase (MPO) activity. RESULTS: Colon weight was decreased in the groups treated with extract (500 and 1000 mg/kg) and essential oil (0.5 ml/kg) compared to the control group. Regarding MPO levels, ulcer severity and area as well as the total colitis index, same results indicating meaningful alleviation of colitis was achieved after treatment with oral extract and essential oil. CONCLUSION: Since the present experiment was made by oral fractions of coriander thus the resulting effects could be due to both the absorption of the active ingredients and/or the effect of non-absorbable materials on colitis after reaching the colon. In this regard, we propose more toxicological and clinical experiments to warranty its beneficial application in human inflammatory bowel diseases.

Synthesis, characterization and application of poly(acrylamide-co-methylenbisacrylamide) nanocomposite as a colorimetric chemosensor for visual detection of trace levels of Hg and Pb ions.

In this study, a new colorimetric chemosensor based on TiO2/poly(acrylamide-co-methylenbisacrylamide) nanocomposites was designed for determination of mercury and lead ions at trace levels in environmental samples. The removal and preconcentration of lead and mercury ions on the sorbent was achieved due to sharing an electron pair of N and O groups of polymer chains with the mentioned heavy metal ions. The hydrogel sensor was designed by surface modification of a synthesized TiO2 nanoparticles using methacryloxypropyltrimethoxysilan (MAPTMS), which provided a reactive C=C bond that polymerized the acrylamide and methylenbisacrylamide. The sorbent was characterized using X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscope (SEM), EDS analysis and Fourier transform in frared (FT-IR) spectrometer. This nanostructured composite with polymer shell was developed as a sensitive and selective sorbent for adsorption of mercury and lead ions from aqueous solution at optimized condition. This method involves two-steps: (1) preconcentration of mercury and lead ions by the synthesized sorbent and (2) its selective monitoring of the target ions by complexation with dithizone (DZ). The color of the sorbent in the absence and presence of mercury and lead ions shifts from white to violet and red, respectively. The detection limit of the synthesized nanochemosensor for mercury and lead ions was 1 and 10 µg L(-1), respectively. The method was successfully applied for trace detection of mercury and lead ions in tap, river, and sea water samples.