bluuebunny/crossref_metadata_2025_split huggingface dataset:
How Awareness of Possible Evidence Induces Forthcoming Counter‐Interrogation Strategies
Authors: Luke Timothy J. , Dawson Evan , Hartwig Maria , Granhag Pär Anders 
Published: March 2014

SummaryWe propose that suspects' counter‐interrogation strategies vary as a function of their perception of the interrogator's knowledge about the events in question. The present study investigates the verbal behavior of guilty and innocent suspects when they are aware that there may be incriminating evidence against them. Participants (N = 143) took part in either a simulated act of terrorism or a benign task. They were then interviewed about their activities. Participants were randomly assigned to receive no additional information or to be informed that an investigative team may have collected evidence from surveillance cameras. Results suggest that when alerted to possible evidence against them, guilty suspects adopt either extremely withholding or extremely forthcoming verbal strategies. Theoretical implications of these results are discussed. Copyright © 2014 John Wiley & Sons, Ltd.
Proof‐of‐Concept Study of a Web‐Based Methotrexate Decision Aid for Patients With Rheumatoid Arthritis
Authors: Li Linda C. , Adam Paul M. , Backman Catherine L. , Lineker Sydney , Jones C. Allyson , Lacaille Diane , Townsend Anne F. , Yacyshyn Elaine , Yousefi Charlene , Tugwell Peter , Leese Jenny , Stacey Dawn 
Published: March 2014

ObjectiveTo assess the extent to which an online patient decision aid reduced decisional conflict and improved self‐management knowledge/skills in patients who were considering methotrexate for rheumatoid arthritis (RA).MethodsWe used a mixed‐methods pre‐post study design. Eligible participants had a diagnosis of RA, had been prescribed methotrexate but were unsure about starting it, and had access to the internet. Outcome included the Decisional Conflict Scale, the Methotrexate in RA Knowledge Test, and the Effective Consumer Scale. Paired t‐tests were used to assess changes before and after the intervention. Randomly selected participants were interviewed at the end of the study about their experiences with the decision aid.ResultsOf 30 participants, 23 were women. Mean ± SD age was 54.9 ± 14.9 years and the median disease duration was 1 year (interquartile range 0.3–5.0 years). Mean ± SD decisional conflict changed from 49.50 ± 23.17 preintervention to 21.83 ± 24.12 postintervention (change −27.67 [95% confidence interval −39.89, −15.44]; P < 0.001). Knowledge of methotrexate improved (mean ± SD 30.62 ± 9.26 preintervention and 41.67 ± 6.81 postintervention; P < 0.001), but there was no change in effective consumer attributes (mean ± SD 68.24 ± 12.46 preintervention and 72.94 ± 12.74 postintervention; P = 0.15). Three themes emerged from interviews of 11 participants: seeking confirmation of one's own knowledge of methotrexate, amplifying reluctance when they encountered information contradicting their own experiences, and clarifying thoughts about the next step during the process.ConclusionPatients' decisional conflict and knowledge improved after using the patient decision aid. Interview findings further highlighted the power of patients' prior knowledge and experiences with RA on how they approach the information presented in a decision aid.
Enantioselective Synthesis of Azaflavanones Using Organocatalytic 6‐endo Aza‐Michael Addition
Authors: Cheng Shuanghua , Zhao Lili , Yu Shouyun 
Published: March 2014

AbstractA method to prepare highly enantioenriched azaflavanones using an organocatalytic 6‐endo aza‐Michael addition has been described. A variety of 2‐aryl‐, 2‐vinyl‐ and 2‐methylazaflavanones were prepared in good yields (53–84%) and excellent enantioselectivities (97.6:2.4 to 99.3:0.7 er).magnified image
Direct and Single‐Molecule Visualization of the Solution‐State Structures of G‐Hairpin and G‐Triplex Intermediates
Authors: Rajendran Arivazhagan , Endo Masayuki , Hidaka Kumi , Sugiyama Hiroshi 
Published: March 2014

AbstractWe present the direct and single‐molecule visualization of the in‐pathway intermediates of the G‐quadruplex folding that have been inaccessible by any experimental method employed to date. Using DNA origami as a novel tool for the structural control and high‐speed atomic force microscopy (HS‐AFM) for direct visualization, we captured images of the unprecedented solution‐state structures of a tetramolecular antiparallel and (3+1)‐type G‐quadruplex intermediates, such as G‐hairpin and G‐triplex, with nanometer precision. No such structural information was reported previously with any direct or indirect technique, solution or solid‐state, single‐molecule or bulk studies, and at any resolution. Based on our results, we proposed a folding mechanism of these G‐quadruplexes.
Steuerung der α‐Synuclein‐Aggregation durch Bindung einer β‐Haarnadel
Authors: Mirecka Ewa A. , Shaykhalishahi Hamed , Gauhar Aziz , Akgül Şerife , Lecher Justin , Willbold Dieter , Stoldt Matthias , Hoyer Wolfgang 
Published: March 2014

AbstractFehlfaltung, Aggregation und Amyloidfibrillenbildung des Proteins α‐Synuclein (α‐syn) sind an der Pathogenese der Parkinson‐Krankheit und weiterer Synucleinopathien beteiligt. Die Entwicklung der Amyloid‐Toxizität steht in Zusammenhang mit der Bildung partiell gefalteter Aggregationsintermediate. Hier beschreiben wir die Entwicklung einer Klasse gegen α‐syn gerichteter Bindeproteine, die wir als β‐Wrapine (β‐Wrap‐Proteine) bezeichnen. Die NMR‐Struktur eines α‐syn:β‐Wrapin‐Komplexes zeigt eine β‐Haarnadel‐Konformation von α‐syn im Sequenzbereich α‐syn(37–54). Substöchiometrische Mengen des Bindeproteins inhibieren die α‐syn‐Aggregation und ‐Toxizität, das β‐Wrapin greift folglich in die Bildung der Aggregationskeime ein.
DNA mit 3′‐5′‐Disulfid‐Verknüpfung – schnelle chemische Ligation durch isosteren Ersatz
Authors: Patzke Volker , McCaskill John S. , von Kiedrowski Günter 
Published: March 2014

AbstractDie Bemühungen, die chemische Ligation von Oligonukleotiden ohne biochemische Enzyme zu etablieren, haben zu einer Vielzahl an synthetischen Analoga geführt und damit die Oligomer‐Ligation um neue Oligonukleotide, Peptide und Hybride, wie PNA, bereichert.1 Wichtigste Anforderungen an potenzielle PCR‐freie Diagnosewerkzeuge sind eine schnelle templatierte chemische DNA‐Ligation mit hoher Paarungsselektivität, sowie eine empfindliche Detektionsmethode. Hier berichten wir über eine Oligonukleotid‐Festphasensynthese von 5′‐ oder 3′‐Mercapto‐didesoxynukleotiden. Die chemische Ligation liefert 3′‐5′‐Disulfid‐Bindungen anstelle der 3′‐5′‐Phosphordiester‐Bindung. Unter Verwendung einer Fluoreszenzmethode beschreiben wir eine der schnellsten Ligationsreaktionen mit Halbwertszeiten in der Größenordnung von Sekunden. Durch die Wahl der DNA‐Modifikation und der 3′‐5′‐Orientierung der Aktivierung wird die nicht templatierte Ligation effektiv unterdrückt. Der Temperatureinfluss auf die templatierte Ligation wir aufgezeigt.
Ein niedermolekulares Ligand‐Wirkstoff‐Konjugat zur Behandlung von Carboanhydrase IX exprimierenden Tumoren
Authors: Krall Nikolaus , Pretto Francesca , Decurtins Willy , Bernardes Gonçalo J. L. , Supuran Claudiu T. , Neri Dario 
Published: March 2014

AbstractAntikörper‐Wirkstoff‐Konjugate sind eine vielversprechende Klasse neuer Krebsmedikamente. Die Verwendung niedermolekularer Liganden für den zielgerichteten Transport zytotoxischer Substanzen in solide Tumoren ist dagegen weniger gut entwickelt. Hier beschreiben wir zum ersten Mal kleine Ligand‐Wirkstoff‐Konjugate zur Behandlung von Carboanhydrase IX exprimierenden Tumoren. Mit Ligand‐Fluoreszenzfarbstoff‐Konjugaten zeigen wir, dass solche Moleküle sich bevorzugt in Antigen exprimierenden Läsionen anreichern, schnell ihr Ziel erreichen und tief in den Tumor eindringen können. Ferner sind derartige Konstrukte durch Totalsynthese herstellbar. Ein über eine Disulfidbrücke verbundenes Wirkstoff‐Konjugat bestehend aus dem Maytansinoid DM1 als zytotoxischer Nutzlast und einem Derivat von Acetazolamid als Transportligand zeigte eine hohe Wirksamkeit gegen SKRC52‐Nierenkleinzellkarzinom in vivo. Die klinisch eingesetzten Standardtherapien Sunitinib und Sorafenib hatten dagegen keine Aktivität.
Rhodium(III)‐Catalyzed Alkenylation Reactions of 8‐Methylquinolines with Alkynes by C(sp3)H Activation
Authors: Liu Bingxian , Zhou Tao , Li Bin , Xu Shansheng , Song Haibin , Wang Baiquan 
Published: March 2014

AbstractThe alkenylation reactions of 8‐methylquinolines with alkynes, catalyzed by [{Cp*RhCl2}2], proceeds efficiently to give 8‐allylquinolines in good yields by C(sp3)H bond activation. These reactions are highly regio‐ and stereoselective. A catalytically competent five‐membered rhodacycle has been structurally characterized, thus revealing a key intermediate in the catalytic cycle.
Functionalizing Single Crystals: Incorporation of Nanoparticles Inside Gel‐Grown Calcite Crystals
Authors: Liu Yujing , Yuan Wentao , Shi Ye , Chen Xiaoqiang , Wang Yong , Chen Hongzheng , Li Hanying 
Published: March 2014

AbstractSynthetic single crystals are usually homogeneous solids. Biogenic single crystals, however, can incorporate biomacromolecules and become inhomogeneous solids so that their properties are also extrinsically regulated by the incorporated materials. The discrepancy between the properties of synthetic and biogenic single crystals leads to the idea to modify the internal structure of synthetic crystals to achieve nonintrinsic properties by incorporation of foreign material. Intrinsically colorless and diamagnetic calcite single crystals are turned into colored and paramagnetic solids, through incorporation of Au and Fe3O4 nanoparticles without significantly disrupting the crystalline lattice of calcite. The crystals incorporate the nanoparticles and gel fibers when grown in agarose gel media containing the nanoparticles, whereas the solution‐grown crystals do not. As such, our work extends the long‐history gel method for crystallization into a platform to functionalize single‐crystalline materials.
Metal‐Triflate‐Catalyzed Synthesis of Polycyclic Tertiary Alcohols by Cyclization of γ‐Allenic Ketones
Authors: Diaf Ilhem , Lemière Gilles , Duñach Elisabet 
Published: March 2014

AbstractIt has been established that bismuth(III) triflate catalyzes the cyclization of γ‐allenic ketones under mild reaction conditions. This reaction allows the selective formation of polycyclic tertiary alcohols from cyclic ketone derivatives. The resulting dienols can engage in stereoselective cycloadditions to efficiently afford complex polycyclic systems.
Eine konvergente Totalsynthese des Telomerase‐Inhibitors (±)‐γ‐Rubromycin
Authors: Wilsdorf Michael , Reißig Hans‐Ulrich 
Published: March 2014

AbstractDer Telomeraseinhibitor γ‐Rubromycin wurde in seiner racemischen Form in einer Gesamtausbeute von 3.8 % hergestellt. Der Schlüsselschritt der Synthesesequenz ist eine effiziente säurekatalysierte Spiroketalisierung unter Aufbau der zentralen Spiroketaleinheit. Die Synthese des erforderlichen, elektronisch ausbalancierten Spiroketalvorläufers erfolgte durch das konvergente Zusammenführen eines naphthylsubstituierten Aldehyds, eines α‐Methoxyallyl‐γ‐silyl‐substituierten Phosphonats als zentralem C3‐Baustein und eines hoch funktionalisierten Aryl‐Grignard‐Reagens. Ein weiteres Merkmal der Synthese ist eine späte Isocumarinbildung bei gleichzeitiger Protodesilylierung zu einem als Methylarylether geschützten γ‐Rubromycin‐Vorläufer.
Sequestration of a β‐Hairpin for Control of α‐Synuclein Aggregation
Authors: Mirecka Ewa A. , Shaykhalishahi Hamed , Gauhar Aziz , Akgül Şerife , Lecher Justin , Willbold Dieter , Stoldt Matthias , Hoyer Wolfgang 
Published: March 2014

AbstractThe misfolding and aggregation of the protein α‐synuclein (α‐syn), which results in the formation of amyloid fibrils, is involved in the pathogenesis of Parkinson’s disease and other synucleinopathies. The emergence of amyloid toxicity is associated with the formation of partially folded aggregation intermediates. Here, we engineered a class of binding proteins termed β‐wrapins (β‐wrap proteins) with affinity for α‐synuclein (α‐syn). The NMR structure of an α‐syn:β‐wrapin complex reveals a β‐hairpin of α‐syn comprising the sequence region α‐syn(37–54). The β‐wrapin inhibits α‐syn aggregation and toxicity at substoichiometric concentrations, demonstrating that it interferes with the nucleation of aggregation.
Disturbed B Cell Homeostasis in Newly Diagnosed Giant Cell Arteritis and Polymyalgia Rheumatica
Authors: van der Geest Kornelis S. M. , Abdulahad Wayel H. , Chalan Paulina , Rutgers Abraham , Horst Gerda , Huitema Minke G. , Roffel Mirjam P. , Roozendaal Caroline , Kluin Philip M. , Bos Nicolaas A. , Boots Annemieke M. H. , Brouwer Elisabeth 
Published: March 2014

ObjectiveSeveral lines of evidence indicate that B cells may be involved in the immunopathology of giant cell arteritis (GCA) and polymyalgia rheumatica (PMR). This study was undertaken to examine the distribution of defined B cell subsets, including effector B (Beff) cells and regulatory B (Breg) cells, in patients with GCA and patients with PMR before and after corticosteroid treatment.MethodsCirculating B cells were analyzed in 34 newly diagnosed, untreated patients with GCA or PMR, and in 44 followup samples from patients with GCA or PMR who received corticosteroids for 2 weeks or 3 months. For comparison, 40 age‐matched healthy controls and 11 rheumatoid arthritis (RA) patients were included. Serum BAFF levels were determined, and temporal arteries were studied by immunohistochemistry.ResultsPatients newly diagnosed as having GCA or PMR, but not patients with RA, had decreased numbers of circulating B cells compared to healthy controls. B cell numbers recovered rapidly in treated patients with GCA and PMR in remission. This recovery was not achieved by compensatory hyperproliferation or enhanced bone marrow production. B cell numbers inversely correlated with erythrocyte sedimentation rates, C‐reactive protein levels, and serum BAFF levels. Tumor necrosis factor α–positive Beff cells, but not interleukin‐10 (IL‐10)–positive Breg cells, were decreased in patients newly diagnosed as having GCA or PMR. Following treatment, circulating numbers of Beff cells normalized. The returning Beff cells demonstrated an enhanced capacity to produce IL‐6. Few B cells were found in temporal artery biopsy specimens from GCA patients.ConclusionWe show for the first time that the distribution of B cells is highly disturbed in GCA and PMR and that B cells likely contribute to the enhanced IL‐6 response in both diseases.
Gold‐Catalyzed 6‐Exo‐Dig Cycloisomerization: A Versatile Approach to Functionalized Phenanthrenes
Authors: Shu Chao , Li Long , Chen Cheng‐Bin , Shen Hong‐Cheng , Ye Long‐Wu 
Published: March 2014

AbstractA novel gold‐catalyzed 6‐exo‐dig cycloisomerization of o‐propargylbiaryls has been developed that provides ready access to functionalized phenanthrenes in largely good to excellent yields. Notable features of this method are readily available starting materials, mild reaction conditions, and broad substrate scope.
A validated HPLC method for the determination of dimethyl‐4,4′‐dimethoxy‐5,6,5′,6′‐dimethylene dioxybiphenyl‐2,2′‐dicarboxylate (DDB) with fluorescence detection in raw material and pill form: application to an in vitro dissolution test and a content uniformity test
Authors: Walash Mohamed I. , Ibrahim Fawzia , El Abass Samah Abo 
Published: March 2014

ABSTRACTA simple, sensitive and rapid HPLC method with fluorescence detection for the determination of dimethyl‐4,4′‐dimethoxy‐5,6,5′,6′‐dimethylene dioxybiphenyl‐2,2′‐dicarboxylate (DDB) in the raw material and pill form was developed. Liquid chromatography was performed on a C18 column (250 × 4.6 mm i.d., 5 µm particle size), the mobile phase consisted of methanol and 0.05 M sodium dihydrogen phosphate buffer (80 : 20, v/v), and the apparent pH of the mobile phase was adjusted to 3. The fluorescence detector was operated at excitation/emission wavelengths of 275/400 nm. The proposed method allows the determination of DDB within concentration range 0.1–1.5 µg/mL with a limit of detection of 0.032 µg/mL, a limit of quantification of 0.097 µg/mL and a correlation coefficient of 0.9997. The proposed method has been successfully applied for the analysis of DDB in its pills with a percentage recovery of 98.45 ± 0.32. The method was fully validated according to ICH guidelines. Moreover, the high sensitivity of the method permits its use in an in vitro dissolution test for DDB under simulated intestinal conditions. In addition, the proposed method was extended to a content uniformity test according to USP guidelines. Copyright © 2014 John Wiley & Sons, Ltd.
Binding free energy calculations between bovine β‐lactoglobulin and four fatty acids using the MMGBSA method
Authors: Bello Martiniano 
Published: March 2014

ABSTRACTThe bovine dairy protein β‐lactoglobulin (βlg) is a promiscuous protein that has the ability to bind several hydrophobic ligands. In this study, based on known experimental data, the dynamic interaction mechanism between bovine βlg and four fatty acids was investigated by a protocol combining molecular dynamics (MD) simulations and molecular mechanics generalized Born surface area (MMGBSA) binding free energy calculations. Energetic analyses revealed binding free energy trends that corroborated known experimental findings; larger ligand size corresponded to greater binding affinity. Finally, binding free energy decomposition provided detailed information about the key residues stabilizing the complex. © 2014 Wiley Periodicals, Inc. Biopolymers 101: 1010–1018, 2014.
A purge and trap technique to capture volatile compounds combined with comprehensive two‐dimensional gas chromatography/time‐of‐flight mass spectrometry to investigate the effect of sulfur‐fumigation on Radix Angelicae Dahuricae
Authors: Cao Gang , Li Qinglin , Zhang Jida , Cai Hao , Cai Baochang 
Published: March 2014

ABSTRACTSulfur‐fumigation is known to reduce volatile compounds that are the main active components in herbs used in herbal medicine. We investigated changes in chemical composition between sun‐dried and sulfur‐fumigated Radix Angelicae Dahuricae using a purge and trap technique to capture volatile compounds, and two‐dimensional gas chromatography/time‐of‐flight mass spectrometry for identification. Using sun‐dried Radix Angelicae Dahuricae samples as a reference, the results showed that 73 volatile compounds, including 12 sulfide compounds, were found to be present only in sulfur‐fumigated samples. Furthermore, 32 volatile compounds that were found in sun‐dried Radix Angelicae Dahuricae samples disappeared after sulfur‐fumigation. The proposed method can be applied to accurately discriminate sulfur‐fumigated Radix Angelicae Dahuricae from different commercial sources. Copyright © 2014 John Wiley & Sons, Ltd.
Joint MS‐based platforms for comprehensive comparison of rat plasma and serum metabolic profiling
Authors: Lin Zhang , Zhang Zhimin , Lu Hongmei , Jin Yisu , Yi Lunzhao , Liang Yizeng 
Published: March 2014

ABSTRACTMetabolomics is a rapidly growing field in the comprehensive understanding of cellular and organism‐specific responses associated with perturbations induced by medicines, chemicals and environment. Blood matrices are frequently used in clinical and biological studies. In this study, we compared metabolic profiling between rat plasma and serum using complementary platforms of gas chromatography–mass spectrometry (GC‐MS) and liquid chromatography–quadruple time‐of‐flight–mass spectrometry (LC‐QTOF‐MS). The sample types that were tested included plasma prepared with K2EDTA and serum collected using venous blood collection protocols. The results of peak area variation for each detected metabolite/feature in the quality control samples showed a good reproducibility in LC‐QTOF‐MS and better reproducibility in GC‐MS. In GC‐MS analysis: (a) 25.8% of the defined metabolites differed serum from plasma profiling (t‐test, p < 0.05); and (b) serum possessed higher sensitivity than plasma for its generally higher peak intensity in the metabolic profiling. In LC‐QTOF‐MS analysis, 13 (in positive ion mode) and seven (in negative ion mode) important metabolites were identified as mainly contributing to the separation between serum and plasma. Copyright © 2014 John Wiley & Sons, Ltd.
Development and validation of an HPLC method for tetracycline‐related USP monographs
Authors: Hussien Emad M. 
Published: March 2014

ABSTRACTA novel reversed‐phase HPLC method was developed and validated for the assay of tetracycline hydrochloride and the limit of 4‐epianhydrotetracycline hydrochloride impurity in tetracycline hydrochloride commercial bulk and pharmaceutical products. The method employed L1 (3 µm, 150 × 4.6 mm) columns, a mobile phase of 0.1% phosphoric acid and acetonitrile at a flow rate of 1.0 mL/min, and detection at 280 nm. The separation was performed in HPLC gradient mode. Forced degradation studies showed that tetracycline eluted as a spectrally pure peak and was well resolved from its degradation products. The fast degradation of tetracycline hydrochloride and 4‐epianhydrotetracycline hydrochloride in solution was retarded by controlling the autosampler temperature at 4 °C and using 0.1% H3PO4 as diluent. The robustness of the method was tested starting with the maximum variations allowed in the US Pharmacopeia (USP) general chapter Chromatography <621>. The method was linear over the range 80–120% of the assay concentration (0.1 mg/mL) for tetracycline hydrochloride and 50–150% of the acceptance criteria specified in the individual USP monographs for 4‐epianhydrotetracycline hydrochloride. The limit of quantification for 4‐epianhydrotetracycline hydrochloride was 0.1 µg/mL, 20 times lower than the acceptance criteria. The method was specific, precise, accurate and robust. Copyright © 2014 John Wiley & Sons, Ltd.
Liquid chromatography–tandem mass spectrometric assay for the multikinase inhibitor regorafenib in plasma
Authors: Luethi Dino , Durmus Selvi , Schinkel Alfred H. , Schellens Jan H. M. , Beijnen Jos H. , Sparidans Rolf W. 
Published: March 2014

ABSTRACTRegorafenib has recently been approved for the treatment of colorectal cancer. A bioanalytical liquid chromatography–tandem mass spectrometric assay for this multikinase inhibitor was developed and validated in plasma. The concentration range of the assay was 25–25,000 ng/mL. Protein precipitation with acetonitrile was used as sample pre‐treatment with sorafenib as internal standard. The extract was diluted with methanol (25%, v/v) and then injected onto the sub‐2 µm particle, bridged ethylsilicia hybrid trifunctional bonded C18 column. Isocratic elution using 0.02% (v/v) formic acid in a methanol–water mixture was used. Compounds were monitored by a triple quadrupole mass spectrometer in the selected reaction monitoring mode after positive electrospray ionization. Double logarithmic calibration was used; within‐day precisions, between‐day precisions, and accuracies were 3.2–9.2, 4.1–12.3 and 94.8–103.0%, respectively. High drug stability was observed under all relevant storage conditions. The assay was used to measure drug concentrations in a pharmacokinetic study in wild‐type FVB mice. Copyright © 2014 John Wiley & Sons, Ltd.