bluuebunny/crossref_metadata_2025_split huggingface dataset:
Validation of a liquid chromatography‐triple quadrupole mass spectrometric method for the determination of 5‐nitro‐5′‐hydroxy‐indirubin‐3′‐oxime (AGM‐130) in human plasma and its application to microdose clinical trial
Authors: Park Min‐Ho , Lee Yun Young , Cho Kyung Hee , La Sookie , Lee Hee Joo , Yim Dong‐Seok , Ban Sooho , Park Moon‐Young , Kim Yong‐Chul , Kim Yoon‐Gyoon , Shin Young G. 
Published: July 2015

AbstractA liquid chromatography–triple quadrupole mass spectrometric (LC‐MS/MS) method was developed and validated for the determination of 5‐nitro‐5′‐hydroxy‐indirubin‐3′‐oxime (AGM‐130) in human plasma to support a microdose clinical trial. The method consisted of a liquid–liquid extraction for sample preparation and LC‐MS/MS analysis in the positive ion mode using TurboIonSprayTM for analysis. d3‐AGM‐130 was used as the internal standard. A linear regression (weighted 1/concentration) was used to fit calibration curves over the concentration range of 10–2000 pg/mL for AGM‐130. There were no endogenous interference components in the blank human plasma tested. The accuracy at the lower limit of quantitation was 96.6% with a precision (coefficient of variation, CV) of 4.4%. For quality control samples at 30, 160 and 1600 pg/mL, the between run CV was ≤5.0 %. Between‐run accuracy ranged from 98.1 to 101.0%. AGM‐130 was stable in 50% acetonitrile for 168 h at 4°C and 6 h at room temperature. AGM‐130 was also stable in human plasma at room temperature for 6 h and through three freeze–thaw cycles. The variability of selected samples for the incurred sample reanalysis was ≤12.7% when compared with the original sample concentrations. This validated LC‐MS/MS method for determination of AGM‐130 was used to support a phase 0 microdose clinical trial. Copyright © 2015 John Wiley & Sons, Ltd.
Validation of a sensitive HPLC/fluorescence method for assessment of ciprofloxacin levels in plasma and prostate microdialysate samples from rats
Authors: Zimmermann Estevan Sonego , Torres Bruna Gaelzer Silva , Dalla Costa Teresa 
Published: July 2015

AbstractChronic bacterial prostatitis treatment consists of broad‐spectrum antibiotic therapy for long periods of time. Drug penetration into the prostate makes the treatment a challenged. Ciprofloxacin is one of the most prescribed drugs for this treatment. A liquid chromatography with fluorescence detection method was developed and validated for determining ciprofloxacin concentrations in two different matrices: plasma and prostate microdialysate. Ciprofloxacin was separated on a C18 column eluted with a mobile phase constituted of a mixture of 0.4% aqueous triethylamine:methanol:acetonitrile (75:15:10, v/v/v) and 0.4% aqueous triethylamine:acetonitrile (88:12, v/v) for microdialysate and plasma samples, respectively. Linearity was obtained over a concentration range of 5–1000 ng/mL (microdialysate) and 10–2000 ng/mL (plasma), with coefficients of determination ≥0.9956. Precision was determined from the analysis of six quality control samples and showed RSD values <11.1 and 7.4% for intra and inter‐assay precision, respectively. The accuracy ranged from 85.6 to 114.3%. The method was applied to a preliminary pharmacokinetic study to investigate ciprofloxacin concentrations in prostate, sampled by microdialysis, and plasma after a 7 mg/kg intravenous dose to Wistar rats. The method showed high sensitivity using only protein precipitation as plasma sample clean‐up and was successfully applied to investigate ciprofloxacin prostate penetration. Copyright © 2015 John Wiley & Sons, Ltd.
Metabolic shifts induced by human H460 cells in tumor‐bearing mice
Authors: Liu Linsheng , Wang Yaqiong , Zheng Tian , Cao Bei , Li Mengjie , Shi Jian , Aa Nan , Wang Xinwen , Zhao Chunyan , Aa Jiye , Wang Guangji 
Published: July 2015

AbstractTumor markers are most popularly used in diagnosis of various cancers clinically. However, the confounding factors of individual background diversities, such as genetics, food preferences, living styles, physical exercises, etc., greatly challenge the identification of tumor markers. Study of the metabolic impact of inoculated tumors on model animals can facilitate the identification of metabolomic markers relevant to tumor insult. In this study, serum metabolites from nude mice (n = 14) inoculated with human H460 cells (human nonsmall cell lung carcinoma) were profiled using gas chromatography time‐of‐flight mass spectrometry. The mice with inoculated tumors showed an obviously different metabolic pattern from the control; identification of the discriminatory metabolites suggested the metabolic perturbation of free fatty acids, amino acids, glycolysis and tricarboxylic acid (TCA) cycle turnover. The significantly decreased TCA intermediates, free fatty acids, 3‐hydroxybutyric acid and fluctuating amino acids (t‐test, p < 0.05) in serum of tumor‐bearing mice characterized the metabolic impact of local inoculated H460 tumor cells on the whole system. This indicates that they are candidate metabolomic markers for translational study of lung cancer, clinically. Copyright © 2015 John Wiley & Sons, Ltd.
Achieving Exceptional Photocatalytic Activity and Selectivity through a Well‐Controlled Short‐Ordered Structure: A Case Study of NaxTaOy⋅n H2O
Authors: Su Yiguo , Lang Junyu , Du Chunfang , Bian Fenggang , Wang Xiaojing 
Published: July 2015

AbstractThe present work reports the preparation of a short‐ordered NaxTaOy⋅n H2O catalyst that exhibits exceptional and highly efficient photocatalytic reactivity toward aerobic oxidation relative to its crystalline counterpart. Synchrotron radiation wide‐angle X‐ray scattering and transmission electron microscopy results indicated that the as‐synthesized catalyst shows short‐ordered features with well‐controlled short‐range ordering limits and defect chemistry. The short‐ordered structure of NaxTaOy⋅n H2O predicted large amounts of defective centers and high surface areas that may play critical roles in visible‐light harvesting and photocatalytic aerobic oxidation. This work may provide a novel strategy for the development of short‐ordered catalytic systems with well‐controlled defect chemistry that exhibit highly efficient photocatalytic properties.
Photoelectrocatalytic Oxidation of Methyl Orange on a TiO2 Nanotubular Anode Using a Flow Cell
Authors: José Martín de Vidales María , Mais Laura , Sáez Cristina , Cañizares Pablo , Walsh Frank C. , Rodrigo Manuel A. , Rodrigues Christiane de Arruda , Ponce de León Carlos 
Published: July 2015

AbstractMethyl orange from water was removed by photocatalytic anodic oxidation using a titanium dioxide array surface. The coating was prepared by anodizing a titanium plate in an ethylene glycol electrolyte‐containing NH4F followed by heat treatment to realize a photocatalytic surface under UV light. Scanning electron microscopy imaging showed that the array coating consisted of closely spaced nanotubes perpendicular to the titanium plate. The aqueous solution of methyl orange was circulated through a rectangular channel flow cell containing the coated anode. The effects of electrolyte flow rate and applied potential on the oxidation rate and efficiency were evaluated. At higher mean linear flow rates, the efficiency of the oxidation process improved, indicating a mass transport‐controlled process. At more positive applied potentials, the TiO2 structure deteriorated resulting in a lower oxidation efficiency.
Optimization of Titania Post‐Necking Treatment of TaON Photoanodes to Enhance Water‐Oxidation Activity under Visible‐Light Irradiation
Authors: Gujral Satnam Singh , Simonov Alexandr N. , Higashi Masanobu , Abe Ryu , Spiccia Leone 
Published: July 2015

AbstractA post‐necking treatment of porous screen‐printed TaON films with titania is optimized to improve their photocatalytic activity for water oxidation under visible‐light irradiation (λ>400 nm). Post‐necking was achieved by applying TiCl4 solutions in ethanol or water, or Ti(iOPr)2(acac)2 (acac=acetylacetonate) in isopropanol to the films, followed by calcination at 450 °C in air. Under voltammetric and chronoamperometric conditions in Na2SO4 (0.1 M, pH 6), a 25‐fold enhancement in oxidative photocurrent densities is achieved upon post‐necking of TaON by using ethanolic TiCl4, whereas aqueous TiCl4 and Ti(iOPr)2(acac)2 precursors afforded improvements of eight‐ and sixfold, respectively. SEM and electrochemical impedance spectroscopy studies confirm that post‐necking improves the interconnectivity of the particles and facilitates charge transfer within the photoanode and at the electrode–electrolyte interface. The highest improvement in activity was achieved by using ethanolic TiCl4 to deposit 10–20 wt % TiO2 on the TaON films, whereas higher loadings deteriorated the performance.
Shape‐Controlled Growth of Carbon Nanostructures: Yield and Mechanism
Authors: Ma Yao , Sun Xiao , Yang Nianjun , Xia Junhai , Zhang Lei , Jiang Xin 
Published: July 2015

AbstractCarbon nanostructures with precisely controlled shapes are difficult materials to synthesize. A facet‐selective‐catalytic process was thus proposed to synthesize polymer‐linked carbon nanostructures with different shapes, covering straight carbon nanofiber, carbon nano Y‐junction, carbon nano‐hexapus, and carbon nano‐octopus. A thermal chemical vapor deposition process was applied to grow these multi‐branched carbon nanostructures at temperatures lower than 350 °C. Cu nanoparticles were utilized as the catalyst and acetylene as the reaction gas. The growth of those multi‐branched nanostructures was realized through the selective growth of polymer‐like sheets on certain indexed facets of Cu catalyst. The vapor–facet–solid (VFS) mechanism, a new growth mode, has been proposed to interpret such a growth in the steps of formation, diffusion, and coupling of carbon‐containing oligomers, as well as their final precipitation to form nanostructures on the selective Cu facets.
Interpreted Recognition Process: A Highly Sensitive and Selective Luminescence Chemosensor
Authors: Zhang Huabin , Hu Ping , Zhang Qikai , Huang Mingdong , Lu Can‐Zhong , Malgras Victor , Yamauchi Yusuke , Zhang Jian , Du Shao‐Wu 
Published: July 2015

AbstractA luminescence‐sensing process based on coordination compound [H2N(CH3)2]3[Tb(dipic)3] was developed. It shows fast response (within 1 min), high selectivity, and is ultrasensitive to detect Fe3+ or Cr3+ in aqueous solution and living cells (KSV values are calculated to be 3.6×104 L mol−1 for Fe3+ and 1.9×104 L mol−1 for Cr3+). The whole recognition process has been witnessed through electrospray ionization mass spectrometry (ESI‐MS) analysis, and the ligand‐transfer‐induced luminescence‐quenching mechanism is interpreted. This work contributes to extend the potential applications of lanthanide coordination compounds (LnCCs) in the fields of biological and environmental technologies.
Single‐Site Zeolite‐Anchored Organoiridium Carbonyl Complexes: Characterization of Structure and Reactivity by Spectroscopy and Computational Chemistry
Authors: Martinez‐Macias Claudia , Chen Mingyang , Dixon David A. , Gates Bruce C. 
Published: July 2015

AbstractA family of HY zeolite‐supported cationic organoiridium carbonyl complexes was formed by reaction of Ir(CO)2(acac) (acac=acetylacetonate) to form supported Ir(CO)2 complexes, which were treated at 298 K and 1 atm with flowing gas‐phase reactants, including C2H4, H2, 12CO, 13CO, and D2O. Mass spectrometry was used to identify effluent gases, and infrared and X‐ray absorption spectroscopies were used to characterize the supported species, with the results bolstered by DFT calculations. Because the support is crystalline and presents a nearly uniform array of bonding sites for the iridium species, these were characterized by a high degree of uniformity, which allowed a precise determination of the species involved in the replacement, for example, of one CO ligand of each Ir(CO)2 complex with ethylene. The supported species include the following: Ir(CO)2, Ir(CO)(C2H4)2, Ir(CO)(C2H4), Ir(CO)(C2H5), and (tentatively) Ir(CO)(H). The data determine a reaction network involving all of these species.
Concise Total Synthesis of Ivorenolide B
Authors: Ungeheuer Felix , Fürstner Alois 
Published: July 2015

AbstractAn expeditious route to the potential immunosuppressive lead compound ivorenolide B (1) is described, which relies on the formation of the distinctive 1,3‐diyne subunit embedded into the 17‐membered framework of this target by ring‐closing alkyne metathesis (RCAM). This key transformation was accomplished with the aid of the molybdenum alkylidyne complex 7, which turned out to be compatible with the acid sensitive propargylic alcohol substituents as well as the terminal alkyne unit present in the cyclization precursor. As the presence of such functionality had been detrimental for alkyne metathesis until very recently, this example illustrates the excellent application profile of this new catalyst as well as the rapidly increasing scope of the transformation. Its structural outreach can be further increased by subjecting cyclo‐1,3‐diynes to appropriate post‐metathetic transformations, most notably with the help of alkynophilic gold or palladium catalysts. This aspect is illustrated by the conversion of the model compound 4 into various cyclophane products.
Efficient Synthesis of Differentiated syn‐1,2‐Diol Derivatives by Asymmetric Transfer Hydrogenation–Dynamic Kinetic Resolution of α‐Alkoxy‐Substituted β‐Ketoesters
Authors: Monnereau Laure , Cartigny Damien , Scalone Michelangelo , Ayad Tahar , Ratovelomanana‐Vidal Virginie 
Published: July 2015

AbstractAsymmetric transfer hydrogenation was applied to a wide range of racemic aryl α‐alkoxy‐β‐ketoesters in the presence of well‐defined, commercially available, chiral catalyst RuII–(N‐p‐toluenesulfonyl‐1,2‐diphenylethylenediamine) and a 5:2 mixture of formic acid and triethylamine as the hydrogen source. Under these conditions, dynamic kinetic resolution was efficiently promoted to provide the corresponding syn α‐alkoxy‐β‐hydroxyesters derived from substituted aromatic and heteroaromatic aldehydes with a high level of diastereoselectivity (diastereomeric ratio (d.r.)>99:1) and an almost perfect enantioselectivity (enantiomeric excess (ee)>99 %). Additionally, after extensive screening of the reaction conditions, the use of RuII‐ and RhIII‐tethered precatalysts extended this process to more‐challenging substrates that bore alkenyl‐, alkynyl‐, and alkyl substituents to provide the corresponding syn α‐alkoxy‐β‐hydroxyesters with excellent enantiocontrol (up to 99 % ee) and good to perfect diastereocontrol (d.r.>99:1). Lastly, the synthetic utility of the present protocol was demonstrated by application to the asymmetric synthesis of chiral ester ethyl (2S)‐2‐ethoxy‐3‐(4‐hydroxyphenyl)‐propanoate, which is an important pharmacophore in a number of peroxisome proliferator‐activated receptor α/γ dual agonist advanced drug candidates used for the treatment of type‐II diabetes.
Chiral Memory in Silylium Ions
Authors: Ducos P. , Liautard V. , Robert F. , Landais Y. 
Published: July 2015

AbstractThe configurational stability of the chiral silicon center in Lewis base‐stabilized silyliums has been studied. Complete retention of configuration at silicon is observed at low temperature in silylium ions stabilized by lone‐pair interactions. In contrast, loss of chiral memory is observed with systems involving π‐interactions. Epimerization of the silicon center was observed by simply allowing equilibration of the diastereomeric silyliums at RT or by adding a catalytic amount of a chelating solvent. Conditions for the transfer of axial chirality to Si‐centered chirality were shown to rely on the strength of the Lewis base‐silylium ion interaction.
Prospects of β‐Secretase Inhibitors for the Treatment of Alzheimer’s Disease
Authors: Ghosh Arun K. , Tang Jordan 
Published: July 2015

Abstractβ‐Secretase continues to be an attractive drug discovery target for the therapeutic intervention of Alzheimer’s disease (AD). This enzyme plays a critical role in the production of neurotoxic β‐amyloid (Aβ) peptides in the brain. Over the years, extensive research efforts have led to the development of many promising classes of inhibitors against this protease. Many small‐molecule, peptidomimetic, and nonpeptide β‐secretase inhibitors have now overcome the key challenging development hurdles such as selectivity and brain penetration. A number of inhibitors have also shown further promise in reducing brain Aβ and rescuing cognitive decline in animal models. Recently, several β‐secretase inhibitors have entered into preclinical and phase I studies, and at least one of these inhibitors has advanced to phase II/III human trials. The outlook on β‐secretase inhibitor drugs for the treatment of AD patients is discussed herein.
Implementation and Characterization of Flow Injection in Dissolution Dynamic Nuclear Polarization NMR Spectroscopy
Authors: Chen Hsueh‐Ying , Hilty Christian 
Published: July 2015

AbstractThe use of dissolution dynamic nuclear polarization (D‐DNP) offers substantially increased signals in liquid‐state NMR spectroscopy. A challenge in realizing this potential lies in the transfer of the hyperpolarized sample to the NMR detector without loss of hyperpolarization. Here, the use of a flow injection method using high‐pressure liquid leads to improved performance compared to the more common gas‐driven injection, by suppressing residual fluid motions during the NMR experiment while still achieving a short injection time. Apparent diffusion coefficients are determined from pulsed field gradient echo measurements, and are shown to fall below 1.5 times the value of a static sample within 0.8 s. Due to the single‐scan nature of D‐DNP, pulsed field gradients are often the only choice for coherence selection or encoding, but their application requires stationary fluid. Sample delivery driven by a high‐pressure liquid will improve the applicability of these types of D‐DNP advanced experiments.
Carbon‐Based Materials for Lithium‐Ion Batteries, Electrochemical Capacitors, and Their Hybrid Devices
Authors: Yao Fei , Pham Duy Tho , Lee Young Hee 
Published: July 2015

AbstractA rapidly developing market for portable electronic devices and hybrid electrical vehicles requires an urgent supply of mature energy‐storage systems. As a result, lithium‐ion batteries and electrochemical capacitors have lately attracted broad attention. Nevertheless, it is well known that both devices have their own drawbacks. With the fast development of nanoscience and nanotechnology, various structures and materials have been proposed to overcome the deficiencies of both devices to improve their electrochemical performance further. In this Review, electrochemical storage mechanisms based on carbon materials for both lithium‐ion batteries and electrochemical capacitors are introduced. Non‐faradic processes (electric double‐layer capacitance) and faradic reactions (pseudocapacitance and intercalation) are generally explained. Electrochemical performance based on different types of electrolytes is briefly reviewed. Furthermore, impedance behavior based on Nyquist plots is discussed. We demonstrate the influence of cell conductivity, electrode/electrolyte interface, and ion diffusion on impedance performance. We illustrate that relaxation time, which is closely related to ion diffusion, can be extracted from Nyquist plots and compared between lithium‐ion batteries and electrochemical capacitors. Finally, recent progress in the design of anodes for lithium‐ion batteries, electrochemical capacitors, and their hybrid devices based on carbonaceous materials are reviewed. Challenges and future perspectives are further discussed.
Increased utilization, verification, and clinical implications of immunocytochemistry: Experience in a northern New England hospital
Authors: Sauter Jennifer L. , Ambaye Abiy B. , Mount Sharon L. 
Published: July 2015

BackgroundWe report our experience in utilization, verification, and clinical implications of antibodies for use in diagnostic immunocytochemistry (ICC).MethodsA computer search identified cytology cases utilizing ICC and corresponding surgical pathology material. Alcohol‐fixed liquid based cytology (LBC) specimens were generated from surgical pathology bench specimens. ICC on LBC and immunohistochemistry on formalin fixed paraffin embedded tissue (FFPE) were performed in parallel for 71 commonly used antibodies. Cytology and corresponding surgical pathology reports were reviewed for all cases in which antibodies failed verification studies but had been used in the four years prior to implementation of our verification process.ResultsFrom 2007 to 2011, the number of cytology cases in which ICC was performed increased from 98 (or 5% of all non‐Pap test/nonurine cytology cases in our laboratory) to 306 (or 15%). Verification studies revealed calretinin, CD5, c‐kit/CD117, inhibin, napsin A, OCT 3/4, and PAX‐5 to be nonreliable in LBC despite consistent immunoreactivity in concurrent IHC on surgical specimens. No antibodies were found to be immunoreactive on LBC but nonreactive on FFPE. No adverse clinical outcomes resulted from the use of nonverified antibodies.ConclusionsUtilization of ICC at our institution has increased dramatically in recent years. Our verification process confirmed reliability in the majority of antibodies, but did identify several inconsistent antibodies. Although, in our series, no adverse clinical outcomes resulted from preverification use of these inconsistent antibodies, we encourage other institutions to confirm reliability of antibodies prior to use for diagnostic ICC. Diagn. Cytopathol. 2015;43:688–695. © 2015 Wiley Periodicals, Inc.
Movement of regulatory RNA between animal cells
Authors: Jose Antony M. 
Published: July 2015

SummaryRecent studies suggest that RNA can move from one cell to another and regulate genes through specific base‐pairing. Mechanisms that modify or select RNA for secretion from a cell are unclear. Secreted RNA can be stable enough to be detected in the extracellular environment and can enter the cytosol of distant cells to regulate genes. Mechanisms that import RNA into the cytosol of an animal cell can enable uptake of RNA from many sources including other organisms. This role of RNA is akin to that of steroid hormones, which cross cell membranes to regulate genes. The potential diagnostic use of RNA in human extracellular fluids has ignited interest in understanding mechanisms that enable the movement of RNA between animal cells. Genetic model systems will be essential to gain more confidence in proposed mechanisms of RNA transport and to connect an extracellular RNA with a specific biological function. Studies in the worm C. elegans and in other animals have begun to reveal parts of this novel mechanism of cell‐to‐cell communication. Here, I summarize the current state of this nascent field, highlight the many unknowns, and suggest future directions. genesis 53:395–416, 2015. © 2015 Wiley Periodicals, Inc.