bluuebunny/crossref_metadata_2025 huggingface dataset:
A lab‐on‐a‐chip device for analysis of amlodipine in biological fluids using peroxyoxalate chemiluminescence system
Authors: Al Lawati Haider A. J. , Al‐Nadabi Mira M. , Varma Gouri B. , Suliman Fakhr Eldin O. , Al‐Abri Hasnaa
Published: April 2014

A highly sensitive, rapid and economical method for the determination of amlodipine (AM) in biological fluids was developed using a peroxyoxalate chemiluminescence (CL) system in a lab‐on‐a‐chip device. Peroxyoxalate‐CL is an indirect type of CL that allows the detection of native fluorophores or compounds derivatized with fluorescent labels. Here, fluorescamine was reacted with AM, and the derivatization product was used in a bis‐(2,4,6‐trichlorophenyl)oxalate‐CL system. Fluorescamine reacts selectively with aliphatic primary amine at neutral or basic pH. As most of the calcium channel blocker and many cardiovascular drugs do not contain primary amine, the developed method is highly selective. The parameters that influenced the CL signal intensity were studied carefully. These included the chip geometry, pH, concentration of reagents used and flow rates. Moreover, we confirmed our previous observation about the effects of imidazole, which is commonly used in the bis‐(2,4,6‐trichlorophenyl)oxalate‐CL system as a catalyst, and found that the signal was significantly improved when imidazole was absent. Under optimized conditions, a calibration curve was obtained with a linear range (10–100 µg/L). The limit of detection was 3 µg/L, while the limit of quantification was 10 µg/L. Finally the method was applied for the determination of AM in biological fluids successfully. Copyright © 2014 John Wiley & Sons, Ltd.
A validated LC‐MS/MS assay for the quantitative determination of curdione in rabbit plasma and its application to a pharmacokinetic study after administration of zedoary turmeric oil and bioavailability of the oil
Authors: Peng Ying , Zhang Mei , Li Weiwei , Liu Bingjie , Wu Haiqing , Jiang Fai , Zhao Lulu , Zhu Huafeng
Published: April 2014

A selective and sensitive liquid chromatography tandem mass spectrometry method was developed for the first time for the identification and quantification of curdione in rabbit plasma after vaginal drug administration and intravenous administration of zedoary turmeric oil (ZTO) solution (10 mg/kg). The analysis was performed on a triple‐quadrupole tandem mass spectrometer with multiple reaction monitoring mode via electrospray ionization source in positive ionization mode. After mixing with internal standard diazepam, plasma samples were extracted with ethyl ether–acetic ether (1:1, v/v). Chromatographic separation was carried out on a C18 column with gradient elution using a mixture of water and acetonitrile (both containing 0.1% formic acid) as mobile phases. Linearity ranged over 1.06–106 and 10.6–530 ng/mL (r ≥ 0.995) with the lower limit of quantfication 1.06 ng/mL. The intra‐ and inter‐day precision relative standard deviation values were <12% and the accuracy relative error was from −10.6 to −6.1% at all quality control sample levels. The method was applied to a study of the pharmacokinetics of curdione after vaginal drug administration and intravenous administration of ZTO. Copyright © 2014 John Wiley & Sons, Ltd.
Development and validation of a UHPLC‐qTOF‐MS method for quantification of fuziline in rat plasma and its application in a pharmacokinetic study
Authors: Li Yun‐xia , Gong Xiao‐hong , Li Yan , Zhang Ruo‐qi , Xiong Liang , Xie Xiao‐fang , Peng Cheng
Published: April 2014

A specific and sensitive UHPLC‐qTOF‐MS method was developed and validated for quantification of fuziline in rat plasma after oral administration of three dosages. The analyte was separated on an Acquity UPLC BEH C18 column with a total running time of 3 min using a mobile phase of 0.1% formic acid aqueous solution and methanol (80:20, v/v) at a flow‐rate of 0.25 mL/min. The calibration curves for fuziline showed good linearity in the concentrations ranging from 1 to 200 ng/mL with correlation coefficients >0.997. The precision, accuracy, recovery and stability were deemed acceptable. The method was applied to a pharmacokinetics study of fuziline in rats. The mean half‐life was 5.93, 6.13 and 5.12 h for 1, 2 and 4 mg/kg oral administration of fuziline, respectively. The peak concentration and area under the concentration–time curve increased linearly with the doses. The sum of these results indicated that, in the range of the doses examined, the pharmacokinetics of fuziline in rat was based on first‐order kinetics. Copyright © 2014 John Wiley & Sons, Ltd.
Aspiration thrombectomy in patients undergoing primary angioplasty: Totality of data to 2013
Authors: Kumbhani Dharam J. , Bavry Anthony A. , Desai Milind Y. , Bangalore Sripal , Byrne Robert A. , Jneid Hani , Bhatt Deepak L.
Published: April 2014

Objectives

We sought to update our meta‐analysis on clinical outcomes with aspiration thrombectomy prior to primary percutaneous coronary intervention (PPCI) compared with conventional PPCI alone due to the availability of additional trial data.

Background

The clinical efficacy of adjunctive aspiration thrombectomy in ST‐elevation myocardial infarction (STEMI) patients undergoing PPCI remains controversial. A recent large‐scale randomized trial showed no benefit in terms of mortality at 30 days.

Methods

Clinical trials that randomized STEMI patients to aspiration thrombectomy prior to PPCI compared with conventional PPCI alone were included.

Results

A total of 11,321 patients from 20 randomized controlled trials were included. The composite major adverse cardiac event (MACE) endpoint was lower in the aspiration thrombectomy arm compared with conventional PPCI alone (risk ratio [RR] = 0.81, 95% CI 0.70–0.94; P = 0.006). Although all‐cause mortality was similar between the adjunctive aspiration thrombectomy arm and PPCI arms (RR = 0.83, 95% CI 0.67–1.01; P = 0.06), late mortality (6–12 months) was significantly reduced (RR = 0.64; 95% CI 0.44–0.92; P = 0.016). Reinfarction (RR = 0.64, 95% CI 0.44–0.92; P = 0.017) and stent thrombosis (RR = 0.54; 95% CI 0.32–0.91; P = 0.021) were similarly lower. Differences in target vessel revascularization were of borderline significance (RR = 0.83, 95% CI 0.68–1.01; P = 0.06).

Conclusions

Our meta‐analysis including all randomized controlled trials on aspiration thrombectomy to date demonstrates a significant reduction in adverse clinical outcomes including stent thrombosis compared with conventional PCI alone. © 2014 Wiley Periodicals, Inc.
A novel technique for transcatheter patent ductus arteriosus closure in extremely preterm infants using commercially available technology
Authors: Zahn Evan M. , Nevin Phillip , Simmons Charles , Garg Ruchira
Published: April 2014

Objectives

To describe a new technique for transcatheter patent ductus arteriosus (PDA) closure in extremely preterm infants using commercially available technology.

Background

PDA in premature neonates continues to be a significant clinical problem contributing importantly to both morbidity and mortality. Surgical ligation and medical therapy both have their drawbacks.

Material and Methods

Hospital records and catheterization reports of all premature neonates (< 32 weeks gestation) who underwent transcatheter PDA closure between March 2013 and February 2014 were reviewed. Particular attention was paid to procedural details, complications, and short and mid‐term outcomes.

Results

Six premature infants born at gestational ages ranging between 26 and 31 weeks (median, 26 weeks) underwent attempted transcatheter PDA closure using the Amplatzer Vascular Plug II (AVP II). Median age and weight was 21.5 days (16–80 days) and 1,180 g (870–2,240 g), respectively. Fluoroscopy and echocardiography were used to guide device. Contrast angiography was not used in any patient. Complete closure was achieved in all patients with no major procedural complications. Median fluoroscopy and procedural times were 9.4 (0–19.5) and 51.5 (33–87) min, respectively. All patients were alive at the time of this report. There were no instances of device migration, left pulmonary artery (LPA), or aortic coarctation.

Conclusions

This preliminary study demonstrates that transcatheter PDA closure can be successfully performed in extremely preterm neonates using currently available technology with a high success rate and a low incidence of complications. This report also describes a novel transvenous approach using a combination of echocardiography and judicious use of fluoroscopy to avoid arterial access in this fragile patient population. © 2014 Wiley Periodicals, Inc.
Acute small bowel volvulus in a 2‐month‐old infant
Authors: Wouters Roderick , Raber Menno , van Baren Robertine
Published: April 2014

Key Clinical Message

Abdominal cystic lymphangiomas are rare and occur secondary to congenital malformation of the lymphatics, mostly in the mesenterium. Acute or chronic volvulus of the small bowel may occur by traction of the lymphangioma. Therapy includes resection of the lymphangioma and of the small bowel involved.
Formic Acid Electrooxidation on Noble‐Metal Electrodes: Role and Mechanistic Implications of pH, Surface Structure, and Anion Adsorption
Authors: Brimaud Sylvain , Solla‐Gullón José , Weber Isabella , Feliu Juan M. , Behm R. Jürgen
Published: April 2014

The influence of the electrolyte pH on formic acid (HCOOH) electrooxidation is investigated on both polycrystalline Pt and Au electrodes and on single‐crystalline Au electrodes in perchloric and sulfuric acid‐based electrolytes. On Au electrodes, the potentiodynamic oxidation currents are found to depend, in a nonlinear way, on the electrolyte pH in a bell‐shaped relation, with a maximum of the catalytic activity at the pKa of HCOOH. On polycrystalline Pt electrodes, this feature is not observed; the catalytic activity increases steadily with increasing pH up to a pH value of approximately 5, which is followed by a plateau until pH 10, in contrast with recent observations [J. Joo, T. Uchida, A. Cuesta, M. T. M. Koper, M. Osawa, J. Amer. Chem. Soc.­ 2013, 135, 9991–9994]. In addition, for Au surfaces, the reaction is only weakly influenced by the electrode surface structure, whereas for Pt, structural effects are known to be considerable. Anion effects, in contrast, are much stronger for the reaction on Au electrodes compared to Pt electrodes. Also, it is shown that Pt‐group‐metal‐free Au electrodes do not oxidize molecular hydrogen under reaction conditions. The results are discussed in relation to findings in previous mechanistic studies. Most importantly, the activity on both electrodes is closely correlated with the concentration of HCOO−, and for Au correlates with both HCOO− and HCOOH concentrations. Based on these results, a number of mechanistic proposals put forward in earlier studies must be discarded, and examples for mechanisms compatible with these results are discussed.
Desolvation and Dehydrogenation of Solvated Magnesium Salts of Dodecahydrododecaborate: Relationship between Structure and Thermal Decomposition
Authors: Chen Xuenian , Liu Yi‐Hsin , Alexander Anne‐Marie , Gallucci Judith C. , Hwang Son‐Jong , Lingam Hima Kumar , Huang Zhenguo , Wang Cong , Li Huizhen , Zhao Qianyi , Ozkan Umit S. , Shore Sheldon G. , Zhao Ji‐Cheng
Published: April 2014

Attempts to synthesize solvent‐free MgB12H12 by heating various solvated forms (H2O, NH3, and CH3OH) of the salt failed because of the competition between desolvation and dehydrogenation. This competition has been studied by thermogravimetric analysis (TGA) and temperature‐programmed desorption (TPD). Products were characterized by IR, solution‐ and solid‐state NMR spectroscopy, elemental analysis, and single‐crystal or powder X‐ray diffraction analysis. For hydrated salts, thermal decomposition proceeded in three stages, loss of water to form first hexahydrated then trihydrated, and finally loss of water and hydrogen to form polyhydroxylated complexes. For partially ammoniated salts, two stages of thermal decomposition were observed as ammonia and hydrogen were released with weight loss first of 14 % and then 5.5 %. Thermal decomposition of methanolated salts proceeded through a single step with a total weight loss of 32 % with the release of methanol, methane, and hydrogen. All the gaseous products of thermal decomposition were characterized by using mass spectrometry. Residual solid materials were characterized by solid‐state 11B magic‐angle spinning (MAS) NMR spectroscopy and X‐ray powder diffraction analysis by which the molecular structures of hexahydrated and trihydrated complexes were solved. Both hydrogen and dihydrogen bonds were observed in structures of [Mg(H2O)6B12H12]⋅6 H2O and [Mg(CH3OH)6B12H12]⋅6 CH3OH, which were determined by single‐crystal X‐ray diffraction analysis. The structural factors influencing thermal decomposition behavior are identified and discussed. The dependence of dehydrogenation on the formation of dihydrogen bonds may be an important consideration in the design of solid‐state hydrogen storage materials.
Recognition of Free Tryptophan in Water by Synthetic Pseudopeptides: Fluorescence and Thermodynamic Studies
Authors: Martí‐Centelles Vicente , Izquierdo M. Angeles , Burguete M. Isabel , Galindo Francisco , Luis Santiago V.
Published: April 2014

Pseudopeptidic receptors containing an acridine unit have been prepared and their fluorescence response to a series of amino acids was measured in water. Free amino acids, not protected either at the C or the N terminus, were used for this purpose. The prepared receptors display a selective response to tryptophan (Trp) versus the other assayed amino acids under acidic conditions. The macrocyclic nature of the receptor is important as the fluorescence quenching is higher for the macrocyclic compound than for the related open‐chain receptor. Notably, under the experimental acidic conditions used, both the receptor and guest are fully protonated and positively charged; thus, the experimental results suggest the formation of supramolecular species that contain two positively charged organic molecular components in proximity stabilized through aromatic–aromatic interactions and a complex set of cation‐anion‐cation interactions. The selectivity towards Trp seems to be based on the existence of a strong association between the indole ring of the monocharged amino acid and the acridinium fragment of the triprotonated form of the receptor, which is established to be assisted by the interaction of the cationic moieties with hydrogen sulfate anions.
A “Catch‐and‐Release” Protocol for Alkyne‐Tagged Molecules Based on a Resin‐Bound Cobalt Complex for Peptide Enrichment in Aqueous Media
Authors: Miyazaki Ayako , Asanuma Miwako , Dodo Kosuke , Egami Hiromichi , Sodeoka Mikiko
Published: April 2014

The development of new and mild protocols for the specific enrichment of biomolecules is of significant interest from the perspective of chemical biology. A cobalt–phosphine complex immobilised on a solid‐phase resin has been found to selectively bind to a propargyl carbamate tag, that is, “catch”, under dilute aqueous conditions (pH 7) at 4 °C. Upon acidic treatment of the resulting resin‐bound alkyne–cobalt complex, the Nicholas reaction was induced to “release” the alkyne‐tagged molecule from the resin as a free amine. Model studies revealed that selective enrichment of the alkyne‐tagged molecule could be achieved with high efficiency at 4 °C. The proof‐of‐concept was applied to an alkyne‐tagged amino acid and dipeptide. Studies using an alkyne‐tagged dipeptide proved that this protocol is compatible with various amino acids bearing a range of functionalities in the side‐chain. In addition, selective enrichment and detection of an amine derived from the “catch and release” of an alkyne‐tagged dipeptide in the presence of various peptides has been accomplished under highly dilute conditions, as determined by mass spectrometry.
Modeling of the Stress Behavior of Confined Particle Beds
Authors: Mütze Thomas
Published: April 2014

Das Beanspruchungsverhalten von Gutbetten beschreibt den Zusammenhang zwischen der Kraft, die auf ein Gutbett wirkt, und der Energie, die dem Gutbett insgesamt zugeführt wird. Es ist eng mit der Verdichtung des Gutbetts verknüpft, wobei hier eine rein elastische und eine rein plastische Verformung zu unterscheiden ist. Die elastische Verformung kann durch die Elastizität E des Gutbetts als materialspezifische und vom E‐Modul des Feststoffs unabhängige Kenngröße charakterisiert werden. Die Modellierung des Beanspruchungsverhaltens baut auf dem plastischen Verformungsverhalten auf.
Binding to Large Enzyme Pockets: Small‐Molecule Inhibitors of Trypanothione Reductase
Authors: Persch Elke , Bryson Steve , Todoroff Nickolay K. , Eberle Christian , Thelemann Jonas , Dirdjaja Natalie , Kaiser Marcel , Weber Maria , Derbani Hassan , Brun Reto , Schneider Gisbert , Pai Emil F. , Krauth‐Siegel R. Luise , Diederich François
Published: April 2014

The causative agents of the parasitic disease human African trypanosomiasis belong to the family of trypanosomatids. These parasitic protozoa exhibit a unique thiol redox metabolism that is based on the flavoenzyme trypanothione reductase (TR). TR was identified as a potential drug target and features a large active site that allows a multitude of possible ligand orientations, which renders rational structure‐based inhibitor design highly challenging. Herein we describe the synthesis, binding properties, and kinetic analysis of a new series of small‐molecule inhibitors of TR. The conjunction of biological activities, mutation studies, and virtual ligand docking simulations led to the prediction of a binding mode that was confirmed by crystal structure analysis. The crystal structures revealed that the ligands bind to the hydrophobic wall of the so‐called “mepacrine binding site”. The binding conformation and potency of the inhibitors varied for TR from Trypanosoma brucei and T. cruzi.
An integrated spectral imaging system for producing color images of static and moving objects
Authors: Tominaga Shoji , Nishioka Daisuke , Horiuchi Takahiko
Published: April 2014

An integrated spectral imaging system constructed by synchronizing a programmable light source, a high‐speed monochrome camera, and a display device is proposed to produce tristimulus images of static and moving objects effectively in real time onto the display. This system is called the CIE‐XYZ display. Active spectral illuminants, containing both the device characteristics of camera and display, are projected onto object surfaces as time sequence. The images are captured synchronously by the camera and quickly transmitted to the display device in the RGB signal form so that the accurate tristimulus images are displayed. First, we describe the principle of the CIE‐XYZ tristimulus display. The theoretically optimal illuminants contain negative parts in the spectral curves. Second, we design practical illuminants with all positive spectral curves. The color images in our system are composed of the time sequence of RGB component images. Then, the synthesized color images on the display contain color artifacts when objects move fast. An image processing algorithm for correcting the motion color artifact is proposed based on optical flow estimation using a graphics processing unit. The comprehensive performance of the proposed system and algorithms is examined using both static and moving objects. © 2014 Wiley Periodicals, Inc. Col Res Appl, 40, 329–340, 2015
Long‐Lasting Oscillations in the Electro‐Oxidation of Formic Acid on PtSn Intermetallic Surfaces
Authors: Perini Nickson , Batista Bruno C. , Angelo Antonio C. D. , Epstein Irving R. , Varela Hamilton
Published: April 2014

Even when in contact with virtually infinite reservoirs, natural and manmade oscillators typically drift in phase space on a time‐scale considerably slower than that of the intrinsic oscillator. A ubiquitous example is the inexorable aging process experienced by all living systems. Typical electrocatalytic reactions under oscillatory conditions oscillate for only a few dozen stable cycles due to slow surface poisoning that ultimately results in destruction of the limit cycle. We report the observation of unprecedented long‐lasting temporal oscillations in the electro‐oxidation of formic acid on an ordered intermetallic PtSn phase. The introduction of Sn substantially increases the catalytic activity and retards the irreversible surface oxidation, which results in the stabilization of more than 2200 oscillatory cycles in about 40 h; a 30–40‐fold stabilization with respect to the behavior of pure Pt surfaces. The dynamics were modeled and numerical simulations point to the surface processes underlying the high stability.
Metal Nanoparticles with Liquid‐Crystalline Ligands: Controlling Nanoparticle Superlattice Structure and Properties
Authors: Lewandowski Wiktor , Wójcik Michał , Górecka Ewa
Published: April 2014

Nanoparticle ordered aggregates are promising candidates for future application in a variety of sensing, optical and electronic technologies, mainly based on collective interactions between individual nano‐building blocks. Physicochemical properties of such assemblies depend on nanoparticle spacing, therefore a lot of effort throughout the last years was put on development of assembly methods allowing control over aggregates structure. In this minireview we describe efficient self‐assembly process based on the utilization of liquid‐crystalline ligands grafted onto nanoparticle surface. We show strategies used to synthesize liquid‐crystalline nanoparticles as well as discuss parameters influencing structural and thermal characteristic of aggregates. It is also demonstrated that the liquid‐crystalline approach offers access to dynamic self‐assembly and metamaterials with anisotropic plasmonic properties, which makes this strategy unique among others.
Synthesis and Stability of N,N′‐Dialkyl‐1,13‐dimethoxyquinacridinium (DMQA+): A [4]Helicene with Multiple Redox States
Authors: Sørensen Thomas Just , Nielsen Merete F. , Laursen Bo W.
Published: April 2014

N,N′‐Dialkyl‐1,13‐dimethoxyquinacridinium (DMQA+) is a configurationally locked [4]helicene, a stable carbenium ion and a potent near‐infrared emitter. The versatile synthesis and resolution into M and P enantiomers has made DMQA+ and its congener helicenium derivatives attractive chiral dyes and building blocks. In the present study, electrochemical and spectroscopic studies showed that several redox states of DMQA+ are accessible and stable. The cation stability towards nucleophiles is determined and it is shown that the addition of OH− proceeds with a surprisingly low rate of reaction. The synthetic methodologies leading to DMQA+ are described, and the chemistry occurring from the different redox states of DMQA is identified. This [4]helicene is shown to be a unique molecular framework that is stable as a neutral radical and very stable as a carbenium ion.
Predicting Psychotherapy Dropouts: A Multilevel Approach
Authors: Kegel Alexander F. , Flückiger Christoph
Published: April 2014

The role of therapeutic processes in predicting premature termination of psychotherapy has been a particular focus of recent research. The purpose of this study was to contrast outpatients who completed therapy and those who dropped out with respect to their self‐reported in‐session experiences of self‐esteem, mastery, clarification and the therapeutic alliance. The 296 patients with mixed disorders were treated with an integrative form of cognitive–behavioural therapy without pre‐determined time limit (M = 20.2 sessions). Multilevel analyses indicated that patients who did not completetreatment reported, on average, lower levels of self‐esteem, mastery and clarification and lower ratings of their therapeutic alliance in treatment in contrast to patients who completed therapy. Patient‐reported change in self‐esteem experiences over the course of treatment turned out to be the strongest predictor of dropout from psychotherapy or successful completion. When dropout occurred before the average treatment length was reached, patients reported fewer clarifying experiences as early as the first session and their ratings of the therapeutic alliance were characterized by an absence of positive development. Both of these aspects seem to be involved in patients' decisions to leave treatment early. The findings underscore the importance of the therapeutic process in understanding the mechanisms behind treatment dropout. Copyright © 2014 John Wiley & Sons, Ltd.

Key Practitioner Message

Analyses data from 296 patients at a private outpatient clinic in a routine practice setting (CBT).

Completer/dropout definition: presence or absence of measurement battery at post-assessment.

Focuses on change in therapy processes by investigating post‐session reports.

Finds that positive changes in self‐esteem experiences is the most robust predictor of dropout, followed by ratings of clarification experiences and the global alliance.

In line with recent dropout research, these process indicators might help to detect therapeutic situations that are connected with psychotherapy dropouts.
Flow‐oriented detection of low‐rate denial of service attacks
Authors: Wu Zhijun , Hu Ran , Yue Meng
Published: April 2014

In this paper, an approach of detecting low‐rate denial of service attack is proposed on the basis of principal component analysis algorithm. The proposed approach analyzes low‐rate denial of service attack flows and handles complicated network flows by using principal component analysis algorithm to establish the network traffic matrix model, which is established on the basis of a large number of data acquisitions. Simulation results show that the proposed approach can predigest the high dimension vector, which is composed of networks flows, guarantee the detection precision, and reduce the computation consuming. Copyright © 2014 John Wiley & Sons, Ltd.
The Synthesis of Dimeric ReI–Phenylenediimine Conjugates: Spectroscopic and Electrochemical Studies
Authors: Hasheminasab Abed , Engle James T. , Bass Jacob , Herrick Richard S. , Ziegler Christopher J.
Published: April 2014

A series of dimeric ReI(CO)3 compounds have been prepared by means of a one‐pot reaction of [Re(CO)5X] (X = Cl, Br), pyridine‐2‐carboxyaldehyde, and o‐, m‐, or p‐phenylenediamine. For the m‐ and p‐substituted phenylenediamine reactions, phenyl‐bridged bis(pyridine‐2‐carbaldimine) compounds of the formula [Re(CO)3X]2(μ‐PPC) [3–7; X = Cl, Br; μ‐PPC = m‐ or p‐phenylene bis(pyridine‐2‐carbaldimine)] were produced, with m‐phenylenediamine forming a mixture of isomers. For reactions with o‐phenylenediamine, multiple products formed (compounds 8–11), which ranged from the desired o‐phenylene bis(pyridine‐2‐carbaldimine) adduct to 2‐pyridylbenzimidazole and bridging dipyridinylquinoxaline complexes. An example of each complex was structurally elucidated by single‐crystal X‐ray methods. The dimeric m‐ and p‐phenylene‐bridged Re(CO)3X compounds, including a sulfonate derivative designed to improve solubility, were investigated for possible photophysical applications through the use of UV/Vis spectroscopy and cyclic voltammetry; the study revealed coupling between the rhenium centers.
C–H Activation at a Bidentate Ligand Coordinated to Palladium(II) – an Electrophilic Attack Supported by an External Base
Authors: Cayir Merve , Ghoochany Leila Taghizadeh , Walli Adam , Busch Mark , Sun Yu , Meyer Franc , Bräse Stefan , Thiel Werner R.
Published: April 2014

2‐(2‐Phenylaminopyrimidin‐4‐yl)pyridines undergo C–H activation at the phenyl ring in the ortho position to the amine nitrogen atom when reacted with (PhCN)2PdCl2 and finally form N,N,C‐coordinated palladium(II) complexes in high yields. Five differently substituted complexes were synthesized and characterized by spectroscopy and X‐ray structure analysis. The reaction mechanism for the formation of these complexes was elucidated by kinetic experiments, which allowed the calculation of the activation parameters of the complex formation.
Acrylamide – Still a matter of concern for fried potato food?*
Authors: Matthäus Bertrand , Haase Norbert U.
Published: April 2014

Acrylamide is a well‐known chemical compound that came into the discussion as food‐borne contaminant in 2002 when the Swedish National Food Administration (NFA) together with the University of Stockholm announced the finding of acrylamide in food for the first time. A lot of research has been done all over the world to elucidate the reaction pathway for the formation of acrylamide during processing, to find mitigation strategies to reduce acrylamide in food and to evaluate the toxicity of acrylamide to humans after consumption of acrylamide containing food. Today, it is known that acrylamide is formed under the conditions of the Maillard reaction with low moisture content and temperature >120°C by the amino acid asparagine in presence of certain α‐dicarbonyl compounds from the Maillard reaction. From this knowledge several set screws became evident for the development of successful mitigation strategies such as choice of appropriate raw material low in precursors, pre‐treatment of the raw material before frying or reducing the frying temperature. Until today no significant correlation between the consumption of acrylamide with food and the occurrence of cancer has been found. The present paper reviews the recent research on these topics with special focus on fried potato food.

Practical applications: Formation of acrylamide in fried food is still of concern, and even 12 years after the first communication of acrylamide in processed food a lot of papers are published. The questions of formation, mitigation, toxicity, and exposure are partly answered but on the other side important parts are still open. The paper summarizes the status quo with focus on fried potato products.
Regioselective Hydrodebromination of Polybrominated Indoles
Authors: Chelucci Giorgio , Pinna Gérard A. , Pinna Giansalvo
Published: April 2014

The mixture of sodium borohydride and N,N,N′,N′‐tetramethylethylenediamine in combination with a palladium catalyst is a mild and efficient system for the regioselective hydrodebromination of polybrominated indoles with both N‐donating and N‐withdrawing substituents [N‐methyl‐ and N‐(methoxycarbonyl)indoles, respectively].
First Palladium‐Catalyzed Direct Regioselective C‐5 (Het)Arylation of Mono‐ or Disubstituted Thiazolo[3,2‐b][1,2,4]triazoles
Authors: Le Meur Mikaël , Bourg Stéphane , Massip Stéphane , Marchivie Mathieu , Jarry Christian , Guillaumet Gérald , Routier Sylvain
Published: April 2014

An efficient and convenient method was developed for the formation of polysubstituted thiazolo[3,2‐b][1,2,4]triazoles through C‐5 (het)arylation. The direct C–H activation protocol giving access to di‐ and trisubstituted derivatives in excellent yields was optimized. The method is suitable for use with a wide range of (hetero)aryl bromides, and allows access to a collection of C‐5,6 bis(het)aryl derivatives with full regioselectivity. The results are supported by a full description of all final compounds, and X‐ray crystallographic data confirmed that the spectroscopic analyses were interpreted correctly.
Thermodynamically Controlled Regioselective Glycosylation of Fully Unprotected Sugars through Bis(boronate) Intermediates
Authors: Kaji Eisuke , Yamamoto Daisuke , Shirai Yuko , Ishige Koji , Arai Yoshika , Shirahata Tatsuya , Makino Kazuishi , Nishino Takashi
Published: April 2014

Fully unprotected D‐glucose, D‐mannose, and D‐fructose were regioselectively glycosylated with several phenylthioglycosides to afford glycosyl‐β(1→6)‐α/β‐D‐glucopyranose, glycosyl‐β(1→1)‐α‐D‐mannofuranoside, and glycosyl‐β(1→1)‐β‐D‐fructopyranose in good yields. The regioselectivity might have arisen from a thermodynamically controlled bis(phenylboronate) intermediate, which leaves only one free hydroxy group to be glycosylated in complete regioselectivity.
Spinal protein kinase Mζ contributes to the maintenance of peripheral inflammation‐primed persistent nociceptive sensitization after plantar incision
Authors: An K. , Zhen C. , Liu Z.‐H. , Zhao Q. , Liu H.‐P. , Zhong X.‐L. , Huang W.‐Q.
Published: April 2014

Background

Previous studies suggest that persistent post‐surgical pain (PPSP) is correlated with preoperative pain status and amplification of central sensitization. Protein kinase Mζ (PKMζ) is an essential substrate of the late long‐term potentiation underlying central sensitization, which is one mechanism of pain memory formation. However, the potential contributions of spinal PKMζ to PPSP, a condition in which preoperative pain is prevalent, are not known.

Methods

Here, a modified ‘hyperalgesia priming’ model was established to simulate the clinical situation. This model used intraplantar injections of carrageenan (Car) as priming stimuli to elicit persistent nociceptive sensitization after plantar incision in rats. Upon treatment with PKMζ inhibitor ZIP, Scr‐ZIP or protein kinase Cs (PKCs) inhibitor NPC‐15437, altered behaviour and spinal PKMζ/PKCs expression were observed.

Results

A long‐lasting hypersensitivity induced by Car‐priming was identified and precipitated by subsequent plantar incision in this ‘two‐hit’ paradigm. Post‐treatment with ZIP, but not Scr‐ZIP and NPC‐15437, after the resolution of Car‐priming selectively relieved hypersensitivity. In contrast, pre‐priming NPC‐15437 treatment only prevented Car‐induced initial transient hyperalgesia. Immunoassays showed a significant decrease in spinal PKMζ expression after plantar incision with post‐priming ZIP treatment as compared with Scr‐ZIP and NPC‐15437, but no notable differences in PKCs expression were observed.

Conclusions

Spinal PKCs solely contribute to the initial induction of persistent pain, whereas PKMζ plays an essential role in spinal plasticity storage. PKMζ is responsible for the maintenance of peripheral inflammation‐primed PPSP. Therefore, spinal PKMζ may be a therapeutic target to prevent surgery‐induced chronic pain in patients with preoperative pain.
Source contributions and spatiotemporal characteristics of PAHs in sediments: Using three-way source apportionment approach
Authors: Tian Ying-Ze , Shi Guo-Liang , Liu Gui-Rong , Guo Chang-Sheng , Peng Xing , Xu Jian , Zhang Yuan , Feng Yin-Chang
Published: April 2014

Polycyclic aromatic hydrocarbon (PAHs) were measured in sediments from 29 sites throughout Taihu Lake in China during 2 seasons to investigate spatiotemporal characteristics and source contributions using a 3-way source apportionment approach to positive matrix factorization (PMF3). Seasonal and spatial variations of levels and toxicity suggested higher individual carcinogenic PAH concentrations and toxic equivalent quantity (TEQ) in the flooding season. Three-way PAHs dataset (PAH species, spatial variability, and seasonal variability) was analyzed by PMF3, and its results were compared with a widely used 2-way model (PMF2). Consistent results were observed: vehicular emission was the most important contributor (67.08% by PMF2 and 61.83% by PMF3 for the flooding season; 54.21% by PMF2 and 52.94% by PMF3 for dry season), followed by coal combustion and wood combustion in both seasons. The PMF-cluster analysis was employed to investigate spatial variability of source contributions. Findings can introduce the 3-way approach to apportion sources of PAHs and other persistent organic pollutants (POPs) in sediments, offering the advantage of accounting for information on 3-way datasets. Environ Toxicol Chem 2014;33:1747–1753. © 2014 SETAC
Response of the green alga Oophila sp., a salamander endosymbiont, to a PSII-inhibitor under laboratory conditions
Authors: Baxter Leilan , Brain Richard , Rodriguez-Gil Jose Luis , Hosmer Alan , Solomon Keith , Hanson Mark
Published: April 2014

In a rare example of autotroph-vertebrate endosymbiosis, eggs of the yellow-spotted salamander (Ambystoma maculatum) are colonized by a green alga (Oophila sp.) that significantly enhances salamander development. Previous studies have demonstrated the potential for impacts to the salamander embryo when growth of the algae is impaired by exposure to herbicides. To further investigate this relationship, the authors characterized the response of the symbiotic algae (Oophila sp.) alone to the photosystem II (PSII) inhibitor atrazine under controlled laboratory conditions. After extraction of the alga from A. maculatum eggs and optimization of culturing conditions, 4 toxicity assays (96 h each) were conducted. Recovery of the algal population was also assessed after a further 96 h in untreated media. Average median effective concentration (EC50) values of 123 µg L−1 (PSII yield), 169 µg L−1 (optical density), and 299 µg L−1 (growth rate) were obtained after the 96-h exposure. Full recovery of exposed algal populations after 96 h in untreated media was observed for all endpoints, except for optical density at the greatest concentration tested (300 µg L−1). Our results show that, under laboratory conditions, Oophila sp. is generally less sensitive to atrazine than standard test species. Although conditions of growth in standard toxicity tests are not identical to those in the natural environment, these results provide an understanding of the tolerance of this alga to PSII inhibitors as compared with other species. Environ Toxicol Chem 2014;33:1858–1864. © 2014 SETAC
Efficient multiple antenna–relay selection algorithms for MIMO unidirectional–bidirectional cognitive relay networks
Authors: Alsharoa Ahmad , Ghazzai Hakim , Alouini Mohamed‐Slim
Published: April 2014

In this paper, we consider a multiple‐input multiple‐output (MIMO) cooperative cognitive radio (CR) system using amplify‐and‐forward protocol under a spectrum sharing scenario, where licensed users and unlicensed users operate on the same frequency band. Indeed, combined CR, cooperative communication and MIMO antennas provide a smart solution for a more efficient usage of the frequency band and the data rate. The main objective of this work is to maximise the sum rate of the unlicensed users allowed to share the spectrum with the licensed users by respecting a tolerated interference threshold under perfect and imperfect channel state information scenarios. Practical approaches based on iterative and genetic algorithms for multiple antenna–relay selections with generalised MIMO model for both unidirectional and bidirectional transmissions are proposed to solve our formulated optimization problems. Interestingly, selected numerical results show that our proposed approaches reach a performance close to the performance of the optimal solution either with discrete or continuous power distributions while providing a considerable saving in terms of computational complexity. Copyright © 2014 John Wiley & Sons, Ltd.
Distributed and accumulated reinforcement arrangements: Evaluations of efficacy and preference
Authors: DeLeon Iser G. , Chase Julie A. , Frank‐Crawford Michelle A. , Carreau‐Webster Abbey B. , Triggs Mandy M. , Bullock Christopher E. , Jennett Heather K.
Published: April 2014

We assessed the efficacy of, and preference for, accumulated access to reinforcers, which allows uninterrupted engagement with the reinforcers but imposes an inherent delay required to first complete the task. Experiment 1 compared rates of task completion in 4 individuals who had been diagnosed with intellectual disabilities when reinforcement was distributed (i.e., 30‐s access to the reinforcer delivered immediately after each response) and accumulated (i.e., 5‐min access to the reinforcer after completion of multiple consecutive responses). Accumulated reinforcement produced response rates that equaled or exceeded rates during distributed reinforcement for 3 participants. Experiment 2 used a concurrent‐chains schedule to examine preferences for each arrangement. All participants preferred delayed, accumulated access when the reinforcer was an activity. Three participants also preferred accumulated access to edible reinforcers. The collective results suggest that, despite the inherent delay, accumulated reinforcement is just as effective and is often preferred by learners over distributed reinforcement.
Integration of modeling and simulation to support changes to ondansetron dosing following a randomized, double‐blind, placebo‐, and active‐controlled thorough QT study
Authors: Zuo Peiying , Haberer Lynda J. , Fang Lei , Hunt Thomas L. , Ridgway Derry , Russo Mark W.
Published: April 2014

Prolongation of the QT interval has been observed with ondansetron and other members of the 5‐HT3 antagonist class. This is the first thorough QTc study of ondansetron conducted in accordance with ICH E14 guidelines, designed to investigate the effect of single intravenous (IV) doses of ondansetron on cardiac conduction compared to placebo and a positive control, moxifloxacin, in healthy subjects. Statistical analysis of dose‐response showed the maximum mean difference in QTcF, compared to placebo and corrected for baseline (ddQTcF), was less than 10 milliseconds (ms) after an 8 mg IV dose and approximately 20 ms after the 32 mg dose, each infused over 15 minutes. The concentration‐response (Cp‐ddQTcF) model resulted in similar predictions for the 8 and 32 mg and was used to predict the maximum mean ddQTcF (upper 90% CI bound) of 9.2 (11.2) ms for 16 mg IV. As a result, single IV doses of ondansetron greater than 16 mg should no longer be used. Adult cancer patients, under 75 years, may receive up to a maximum initial 15‐minute IV dose of 16 mg, prior to chemotherapy, followed by 2 additional IV or IM doses of 8 mg for the management of chemotherapy‐induced nausea and vomiting (CINV).
Continuous hydrogen production in a trickling bed reactor by using triticale silage as inoculum: effect of simple and complex substrates
Authors: Arreola‐Vargas Jorge , Alatriste‐Mondragón Felipe , Celis Lourdes B. , Razo‐Flores Elías , López‐López Alberto , Méndez‐Acosta Hugo O.
Published: April 2014

BACKGROUND

Previous studies have reported that complexity of the substrate, type of inoculum and reactor configuration strongly affect fermentative hydrogen production. Therefore, the aim of this study was to evaluate the effect of simple (glucose, xylose and sucrose) and complex (acid and enzymatic oat straw hydrolysates) substrates on the continuous hydrogen production in a trickling bed reactor. Novel inoculum (triticale silage) and biofilm support configuration (vertically organized PET tubing) were tested.

RESULTS

The enzymatic hydrolysate was a suitable substrate for hydrogen production, since its hydrogen molar yield was similar to that obtained with glucose, mean values of 1.6 and 1.7 mol H2 mol−1 sugar consumed were obtained, respectively. In contrast, hydrogen was not produced from the acid hydrolysate. The highest hydrogen production rate (840 mL H2 L−1 h−1) was obtained with glucose at an organic loading rate of 160 g COD L−1 d−1. In spite of the high organic loading rate applied, clogging due to excessive biomass growth was not observed. Finally, PCR‐DGGE analysis revealed that bacteria from Clostridium genus were the putative responsible for hydrogen production.

CONCLUSION

This work demonstrates that continuous hydrogen production is affected by complexity of the substrate. Furthermore, it also shows the feasibility of using triticale silage as inoculum in hydrogen production systems. © 2014 Society of Chemical Industry
Sclerostin monoclonal antibody enhanced bone fracture healing in an open osteotomy model in rats
Authors: Suen Pui Kit , He Yi‐Xin , Chow Dick Ho Kiu , Huang Le , Li Chaoyang , Ke Hua Zhu , Ominsky Michael S. , Qin Ling
Published: April 2014

Sclerostin is a negative regulator of bone formation. Sclerostin monoclonal antibody (Scl‐Ab) treatment promoted bone healing in various animal models. To further evaluate the healing efficiency of Scl‐Ab in osteotomy healing, we investigated the time course effects of systemic administration of Scl‐Ab on fracture repair in rat femoral osteotomy model. A total of 120 six‐month‐old male SD rats were subjected to transverse osteotomy at the right femur mid‐shaft. Rats were treated with vehicle or Scl‐Ab treatment for 3, 6, or 9 weeks. Fracture healing was evaluated by radiography, micro‐CT, micro‐CT based angiography, 4‐point bending mechanical test and histological assessment. Scl‐Ab treatment resulted in significantly higher total mineralized callus volume fraction, BMD and enhanced neovascularization. Histologically, Scl‐Ab treatment resulted in a significant reduction in fracture callus cartilage at week 6 and increase in bone volume at week 9, associated with a greater proportion of newly formed bone area at week 6 and 9 by fluorescence microscopy. Mechanical testing showed significantly higher ultimate load in Scl‐Ab treatment group at week 6 and 9. This study has demonstrated that Scl‐Ab treatment enhanced bone healing in a rat femoral osteotomy model, as reflected in increased bone formation, bone mass and bone strength. © 2014 Orthopaedic Research Society. Published by Wiley Periodicals, Inc. J Orthop Res 32:997–1005, 2014.
Inside the glassmaker technology: search of Raman criteria to discriminate between Emile Gallé and Philippe‐Joseph Brocard enamels and pigment signatures
Authors: Caggiani Maria Cristina , Valotteau Claire , Colomban Philippe
Published: April 2014

The development of solid‐state chemistry at the end of the 19th century offered a variety of routes to colour a glass matrix. Eight enamelled glass objects made by Philippe‐Joseph Brocard and two representative objects made by Emile Gallé have been analysed using a mobile Raman instrument at the Musée des arts décoratifs (Paris) in order to compare their colouration technology. White, blue, yellow, green, orange, red, brown and black pigments have been identified. If most of the pigment palette is common to both craftsmen and typical of the second half of the 19th century, innovative uses are recognized for Gallé (wollastonite as an opacifier, manganese oxides in black mixtures) and Brocard (specific black and grey, pigment mixture, shade modification by small addition of white and red pigments). This preliminary work confirms the potential of Raman spectroscopy, not as a simple analytical method but as a way to document the ancient technology of fine art objects and to discriminate between different genuine productions and/or copies. Copyright © 2014 John Wiley & Sons, Ltd.
Recent trends in the use of food additives in the United Kingdom
Authors: Saltmarsh Mike
Published: April 2014

The E number system for food additives was introduced in the 1960s and the E was intended to reassure consumers that permitted additives were safe. In the 1980s full ingredient declarations had to be provided on food products for the first time and manufacturers were permitted to use either the name or the number of the additive on the ingredient list. This paper outlines some of the trends in the sourcing, use and labelling of additives since the introduction of full ingredient listing. Generally, sourcing has become more global with a large number of suppliers being based in China. From an initial use of E numbers in ingredient lists, manufacturers are increasingly using the names of additives. This trend is being extended to avoid the use of anything the consumer might consider an additive, particularly in connection with colours and preservatives. Specifically, the colours used in the Southampton study on the impact of food colours on hyperactivity in children have largely been replaced by colouring foodstuffs, and the preservative used in the study, sodium benzoate, has been replaced by potassium sorbate in the majority of soft drinks. © 2014 Society of Chemical Industry
Metrics of Kaluza–Klein type on the anti‐de Sitter space
Authors: Calvaruso Giovanni , Perrone Domenico
Published: April 2014

We introduce and study a new family of pseudo‐Riemannian metrics on the anti‐de Sitter three‐space . These metrics will be called “of Kaluza‐Klein type” , as they are induced in a natural way by the corresponding metrics defined on the tangent sphere bundle . For any choice of three real parameters , the pseudo‐Riemannian manifold is homogeneous. Moreover, we shall introduce and study some natural almost contact and paracontact structures , compatible with , such that is a homogeneous almost contact (respectively, paracontact) metric structure. These structures will be then used to show the existence of a three‐parameter family of homogeneous metric mixed 3‐structures on the anti‐de Sitter three‐space.