bluuebunny/crossref_metadata_2025 huggingface dataset:
SPOT Synthesis of 1,3,5‐Trisubstituted Hydantoins on Cellulose Membranes
Authors: Heine Niklas , Schneider‐Mergener Jens , Wenschuh Holger
Published: June 2005

For Abstract see ChemInform Abstract in Full Text.
Product Class 3: 1,3‐Oxathiolium Salts and Related Compounds
Authors: Perst H. , Klenke C.
Published: June 2005

For Abstract see ChemInform Abstract in Full Text.
Enantioselective [2 + 1] Cycloaddition: Cyclopropanation with Zinc Carbenoids
Authors: Denmark Scott E. , Beutner Gregory
Published: June 2005

For Abstract see ChemInform Abstract in Full Text.
Elimination Reactions
Authors: Knipe A. C.
Published: June 2005

For Abstract see ChemInform Abstract in Full Text.
Carbanions and Electrophilic Aliphatic Substitution
Authors: Knipe A. C.
Published: June 2005

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Electrophilic Aromatic Substitution
Authors: Coombes R. G.
Published: June 2005

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Carbenes and Nitrenes
Authors: Knight J. G.
Published: June 2005

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Synthetic Methods. Part 2. Pericyclic Methods
Authors: Stevenson Paul J.
Published: June 2005

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Palladium‐Catalyzed Alkynylation
Authors: Negishi Ei‐ichi , Anastasia Luigi
Published: June 2005

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Constituents of the Pericarps of Mallotus japonicus (Euphorbiaceae)
Authors: Arisawa Munehisa
Published: June 2005

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Bottom‐up Synthesis and Morphological Control of High‐Axial‐Ratio Nanostructures Through Molecular Self‐Assembly
Authors: Shimizu Toshimi
Published: June 2005

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Cyclopropanation and Other Reactions of Palladium—Carbene (And Carbyne) Complexes
Authors: Reiser Oliver
Published: June 2005

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Aspartic Proteases Involved in Alzheimer′s Disease
Authors: Schmidt Boris
Published: June 2005

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Radical Catalysis in Coenzyme B12‐Dependent Isomerization (Eliminating) Reactions
Authors: Toraya Tetsuo
Published: June 2005

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Molecules with Helical Structure: How To Build a Molecular Spiral Staircase.
Authors: Schmuck Carsten
Published: June 2005

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Local Field Experiments in Liquid Crystals
Authors: Caldarelli Stefano
Published: June 2005

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Indirect Nuclear Spin—Spin Coupling Tensors
Authors: Wasylishen Roderick E.
Published: June 2005

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Accurate Determination of Nuclear Quadrupole Coupling Constants and Other NMR Parameters in Liquids from the Combination of Molecular Dynamics Simulations and ab initio Calculations
Authors: Searles Debra J. , Huber Hanspeter
Published: June 2005

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Nuclear Magnetic Resonance Spectroscopy in Macromolecular Science
Authors: Spiess Hans Wolfgang
Published: June 2005

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The First Ozonide of a Phosphorus Oxide — Preparation, Characterization, and Structure of P4O18.
Authors: Dimitrov Anton , Ziemer Burkhard , Hunnius Wolf‐Dietrich , Meisel Manfred
Published: June 2005

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Highly Active Delaminated Ti‐MWW for Epoxidation of Bulky Cycloalkenes with Hydrogen Peroxide.
Authors: Nuntasri Duangamol , Wu Peng , Tatsumi Takashi
Published: June 2005

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Diastereoselective Baylis—Hillman Reaction: Use of Sugar Derived Aldehydes as Chiral Electrophiles.
Authors: Krishna Palakodety Radha , Kannan Vembaiyan , Sharma Gangavaram V. M. , Rao Mallem H. V. Ramana
Published: June 2005

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Synthesis of 3‐Alkylidenebicyclo[3.2.1]octan‐8‐one Skeleton from the Baylis—Hillman Acetates.
Authors: Kim Jae Nyoung , Kim Jeong Mi , Lee Ka Young
Published: June 2005

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A Study on the Conversion of Indanones into Carbostyrils.
Authors: Torisawa Yasuhiro , Nishi Takao , Minamikawa Jun‐ichi
Published: June 2005

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Chemical Oxidation Studies of β‐Hydroxysulfides with tris(4‐Bromophenyl)aminium Hexachloroantimonate: Diastereoselective Sulfoxide Obtaining and Pinacol‐Type Rearrangement.
Authors: Donnici Claudio Luis , Guimaraes Sibele , de Melo Angelita Cristine
Published: June 2005

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Efficient Epoxidation of Olefins with ≥ 99% Selectivity and Use of Hydrogen Peroxide.
Authors: Kamata Keigo , Yonehara Koji , Sumida Yasutaka , Yamaguchi Kazuya , Hikichi Shiro , Mizuno Noritaka
Published: June 2005

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Heck Reaction of Vinyl Bromides with Alkenes in the Presence of a Tetraphosphine/Palladium Catalyst.
Authors: Berthiol Florian , Doucet Henri , Santelli Maurice
Published: June 2005

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Zinc Tetrafluoroborate Catalyzed Efficient Conversion of Aldehydes to Geminal Diacetates and Cyanoacetates.
Authors: Ranu Brindaban C. , Dutta Jyotirmoy , Das Arijit
Published: June 2005

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Synthesis of Primary Amines and N‐Methylamines by the Electrophilic Amination of Grignard Reagents with 2‐Imidazolidinone O‐Sulfonyloxime.
Authors: Kitamura Mitsuru , Chiba Shunsuke , Narasaka Koichi
Published: June 2005

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Electron Deficient Dienes. Part 4. A Synthetic Equivalent of 4‐Methyleneglutaconic Acids, Its Mono and Diethyl Esters and Their Use in a Concise General Synthesis of Isophthalic Acids and Isophthalates.
Authors: Bodwell Graham J. , Hawco Krista M. , Satou Teizi
Published: June 2005

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Enantioselective Catalysis. Part 148. Carbohydrate‐Derived Oxime Ethers Stable Towards Hydrolysis—‐Syntheses of Ligands and Complexes and a Study of Their Catalytic Properties.
Authors: Brunner Henri , Schoenherr Maximilian , Zabel Manfred
Published: June 2005

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Application of Microwaves in Organic Synthesis: A Rapid and Efficient Synthesis of New 3‐Aryl‐2‐imino‐4‐methyl‐2,5‐dihydrofurans and 3‐Aryl‐4‐methyl‐2‐(5H)‐furanones.
Authors: Villemin Didier , Liao Liang
Published: June 2005

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Regioselective C—C Bond Formation Reactions on 2,3‐Dibromo‐ and 2,3,5‐Tribromobenzofuran as an Access to Multiply Substituted Benzofurans. Total Syntheses of Eupomatenoids 3, 4, 5, 6, and 15.
Authors: Bach Thorsten , Bartels Marc
Published: June 2005

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Axially Chiral 3,3′‐Bi(1‐benzothiophene)‐2,2′‐dicarboxylic Acid and Its Derivatives.
Authors: Mezlova Marie , Petrickova Hana , Malon Petr , Kozmik Vaclav , Svoboda Jiri
Published: June 2005

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Synthesis of Functionalized 2,3‐Dihydropyrroles Promoted by Samarium Diiodide.
Authors: Xu Xiaoliang , Zhang Yongmin
Published: June 2005

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A Novel Entry into a New Class of Spiro Heterocyclic Framework: A Facile Synthesis of Dispiro[oxindole‐1,2,3,4‐tetrahydro‐naphthalen‐1‐one]pyrrolidines and Spiro[1,2,3,4‐tetrahydro‐naphthalen‐1‐one]pyrrolidines.
Authors: Raj A. Amal , Raghunathan R.
Published: June 2005

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A New Entry to Polyfunctionalized 4,5‐trans Disubstituted Oxazolidin‐2‐ones from L‐Aspartic Acid.
Authors: Luppi Gianluigi , Tomasini Claudia
Published: June 2005

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1,3‐Dipolar Cycloadditions of D‐Erythrose‐ and D‐Threose‐Derived Alkenes with Nitrones.
Authors: Blanarikova‐Hlobilova Iva , Fisera Lubor , Pronayova Nad'a , Koman Marian
Published: June 2005

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New Reactions of Carbon Suboxide with Alkynes.
Authors: Casu Laura , Bonsignore Leonardo , Cottiglia Filippo , Loy Giuseppe , Maccioni Elias
Published: June 2005

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Synthesis Antifungal and Antibacterial Screening of 3‐Phenyl‐1,4,5‐trihydro‐pyrazol and 2,4‐Dihydro[1,2,4]triazol‐3‐one Derivatives of 4‐Hydroxy‐2‐oxo‐2H‐1‐benzopyran.
Authors: Mulwad V. V. , Shirodkar Jyoti M.
Published: June 2005

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Versatile Synthesis of 3,5‐Disubstituted 2‐Fluoropyridines and 2‐Pyridones.
Authors: Sutherland Andrew , Gallagher Timothy
Published: June 2005

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A Synthesis of Racemic Thalidomide.
Authors: Chang Meng‐Yang , Chen Shui‐Tein , Chang Nein‐Chen
Published: June 2005

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Amination of 4‐Azafluorene under Chichibabin Reaction Conditions. Some Chemical Transformations of 1‐Amino‐4‐azafluorene.
Authors: Varlamov A. V. , Levov A. N. , Toze F. , Chernyshev A. I. , Davydov V. V. , Ryabov M. A. , Egorova O. A.
Published: June 2005

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Synthesis of Fused Cyclopentano‐ and Pyradazino‐Derivatives Incorporating Pyridoquinoline Compound.
Authors: Soleiman H. A. , Kharafallah A. K. , Shindy H. A.
Published: June 2005

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PTSA‐Catalyzed Friedlaender Condensation in the Solid State.
Authors: Mogilaiah K. , Sudhakar G. Rama
Published: June 2005

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Decarboxylation in the Synthesis of 4‐Alkyl‐, 4‐Alkenyl‐ and 4‐Acylpyrimidines.
Authors: Herstad Gunnar , Benneche Tore
Published: June 2005

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3‐(Benzimidazolyl‐2)‐2‐iminocoumarins in Reactions with Aromatic Aldehydes.
Authors: Gorobets N. Yu. , Abakumov V. V.
Published: June 2005

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Novel Preparation of 2,1‐Benzothiazine Derivatives from Sulfonamides with [Hydroxy(tosyloxy)iodo]arenes.
Authors: Misu Yuhta , Togo Hideo
Published: June 2005

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A New Route for the Convenient Synthesis of 5‐Amino‐6‐aryl‐3‐ (5‐aryl‐1,3,4‐oxadiazol‐2‐yl)‐5,6‐dihydro‐2‐thioxo‐1,3‐thiazin‐4‐ones.
Authors: Yadav L. D. S. , Singh Sarvesh
Published: June 2005

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Synthesis of 1,5‐Benzothia/oxazepines as Potent Neuroleptic Agents.
Authors: Bajaj Kiran , Srivastava V. K. , Kumar Ashok
Published: June 2005

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Three‐Component One‐Pot Synthesis of α‐Hydroxylamino Phosphonates Using Ionic Liquids.
Authors: Yadav J. S. , Reddy B. V. S. , Sreedhar P.
Published: June 2005

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Synthesis of a New Type of 1,1‐Bisphosphonates Bearing S‐, and N‐Heterocycles, Based on the Reactions of Methylenebisphosphonate with Alkenes.
Authors: Abdou Wafaa M. , Ganoub Neven A. F. , El‐Khoshnieh Yehia O.
Published: June 2005

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The Alkylation of Aminophosphanes: A New Synthesis of Iminophosphoranes.
Authors: Alajarin Mateo , Lopez‐Leonardo Carmen , Llamas‐Lorente Pilar
Published: June 2005

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First Total Synthesis of (.+‐.)‐Hedaol B.
Authors: Li Ying , Lu Biao , Li Chunhong , Li Yulin
Published: June 2005

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The First Stereoselective Synthesis of Orostanal Isolated from a Marine Sponge Stelletta hiwasaensis.
Authors: Liu Bo , Zhou Wei‐Shan
Published: June 2005

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Steroidal Saponins from Rhizomes of Tupistra wattii Hook. f.
Authors: Shen Ping , Wang San‐Long , Liu Xi‐Kui , Yang Chong‐Ren , Cai Bing , Yao Xin‐Sheng
Published: June 2005

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Synthesis of Cholesteryl Esters of Heterocyclic Analogues of Cinnamic Acid and Hetaroyloxycinnamic Acids by the Wittig Reaction.
Authors: Listvan V. N. , Listvan V. V. , Shekel' A. N.
Published: June 2005

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Synthesis of Spirocycles via Ring Closing Metathesis of Heterocycles Carrying gem‐Diallyl Substituents Obtained via Ring Opening of (Halomethyl)cyclopropanes with Allyltributyltin.
Authors: Gurjar Mukund K. , Ravindranadh Somu V. , Sankar Kuppusamy , Karmakar Sukhen , Cherian Joseph , Chorghade Mukund S.
Published: June 2005

For Abstract see ChemInform Abstract in Full Text.
Biologically Active Indole and Bisindole Alkaloids from Tabernaemontana divaricata.
Authors: Kam Toh‐Seok , Pang Huey‐Shen , Lim Tuck‐Meng
Published: June 2005

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Synthesis of Optically Active N6‐Alkyl Derivatives of (R)‐3‐(Adenin‐9‐yl)‐2‐hydroxypropanoic Acid and Related Compounds.
Authors: Krecmerova Marcela , Budesinsky Milos , Masojidkova Milena , Holy Antonin
Published: June 2005

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Synthesis of Kojic Acid Derivatives Containing Phenolic Hydroxy Groups.
Authors: Kadokawa J. , Nishikura T. , Muraoka R. , Tagaya H. , Fukuoka N.
Published: June 2005

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A Well‐Confined Redox Route to Silver Nanoparticles on the Surface of MoO3.
Authors: Dong Wenjun , Feng Shouhua , Shi Zhan , Li Liansheng , Xu Yuehua
Published: June 2005

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The R2M+ Group 13 Organometallic Fragment Chelated by P‐Centered Ligands
Authors: Mahalakshmi Lepakshaiah , Stalke Dietmar
Published: June 2005

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Supramolecular Interactions in Structures of Organic Antimony and Bismuth Compounds
Authors: Balazs Gabor , Breunig Hans Joachim
Published: June 2005

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Recent Advances in the Synthesis of Retinoids
Authors: Dominguez Beatriz , Alvarez Rosana , de Lera Angel R.
Published: June 2005

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Fragmentation and Cleavage Reactions Mediated by Samarium Iodide. Part 2. α‐ and β‐Elimination Reactions of C‐X Substrates
Authors: Williams D. Bradley G. , Caddy Judy , Blann Kevin
Published: June 2005

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Recent Developments in the Field of A2A and A3 Adenosine Receptor Antagonists
Authors: Baraldi Pier Giovanni , Tabrizi Mojgan Aghazadeh , Bovero Andrea , Avitabile Barbara , Preti Delia , Fruttarolo Francesca , Romagnoli Romeo , Varani Katia , Borea Pier Andrea
Published: June 2005

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Overview of the Suzuki Protocol with Boron
Authors: Suzuki Akira
Published: June 2005

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Recent Advances in Glycomics and Glycogenetics
Authors: Khersonsky Sonya M. , Ho Christine M. , Garcia Mary‐anne F. , Chang Young‐Tae
Published: June 2005

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Small Molecules as Inhibitors of Cyclin‐Dependent Kinases
Authors: Huwe Axel , Mazitschek Ralph , Giannis Athanassios
Published: June 2005

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The Effect of Pressure on Organic Reactions: Basic Principles and Mechanistic Applications
Authors: Wurche Frank , Klarner Frank‐Gerrit
Published: June 2005

For Abstract see ChemInform Abstract in Full Text.
Micromorphology of Cotiga Mound, West Virginia
Authors: Cremeens D.L.
Published: June 2005

Micromorphology samples from Cotiga Mound (ca. 2100 yr B.P.) reveal distinct microstructures associated with mound construction and post‐construction pedogenesis of the mound materials. The interface between layers of basketloads displays sharp, irregular contacts with little to no evidence of pedoturbation, suggesting rapid construction. Evidence of clay and iron translocation, along with well‐preserved charcoal fragments containing identifiable cell structure, were observed in samples collected from hearth features. Both the prepared surface and associated central burial feature at the base of the mound have a complex microstructure, characterized by charcoal layers and zones of clay accumulation, along with microstratification in the prepared surface. Clay translocation, formation of a complex void network, and ironmanganese accumulation were the dominant pedogenic processes that modified the completed mound. © 2005 Wiley Periodicals, Inc.
Paleoindian environmental change and landscape response in Barger Gulch, Middle Park, Colorado
Authors: Mayer James H. , Surovell Todd A. , Waguespack Nicole M. , Kornfeld Marcel , Reider Richard G. , Frison George C.
Published: June 2005

Middle Park, a high‐altitude basin in the Southern Rocky Mountains of north‐central Colorado, contains at least 59 known Paleoindian localities. At Barger Gulch Locality B, an extensive Folsom assemblage (˜10,500 14C yr B.P.) occurs within a buried soil. Radiocarbon ages of charcoal and soil organic matter, as well as stratigraphic positions of artifacts, indicate the soil is a composite of a truncated, latest‐Pleistocene soil and a younger mollic epipedon formed between ˜6000 and 5200 14C yr B.P. and partially welded onto the older soil following erosion and truncation. Radiocarbon ages from an alluvial terrace adjacent to the excavation area indicate that erosion followed by aggradation occurred between ˜10,200 and 9700 14C yr B.P., and that the erosion is likely related to truncation of the latest‐Pleistocene soil. Erosion along the main axis of Barger Gulch occurring between ˜10,000 and 9700 14C yr B.P. was followed by rapid aggradation between ˜9700 and 9550 14C yr B.P., which, along with the erosion at Locality B, coincides with the abrupt onset of monsoonal precipitation following cooling in the region ˜11,000–10,000 14C yr B.P. during the Younger Dryas oscillation. Buried soils dated between ˜9500 and 8000 14C yr B.P. indicate relative landscape stability and soil formation throughout Middle Park. Morphological characteristics displayed by early Holocene soils suggest pedogenesis under parkland vegetation in areas currently characterized by sagebrush steppe. The expansion of forest cover into lower elevations during the early Holocene may have resulted in lower productivity in regards to mammalian fauna, and may partly explain the abundance of early Paleoindian sites (˜11,000–10,000 14C yr B.P., 76%) relative to late Paleoindian sites (˜10,000–8000 14C yr B.P., 24%) documented in Middle Park. © 2005 Wiley Periodicals, Inc.
Kinetic study of hydrolysis of benzoates. Part XXIV—Variation of the ortho substituent effect with solvent in the alkaline hydrolysis of substituted phenyl benzoates
Authors: Nummert Vilve , Piirsalu Mare , Mäemets Vahur , Koppel Ilmar
Published: June 2005

The second‐order rate constants k2 (M−1 s−1) for the alkaline hydrolysis of meta‐, para‐ and ortho‐substituted phenyl benzoates, C6H5CO2C6H4X, in aqueous 0.5 M n‐Bu4NBr were measured spectrophotometrically. The dependence of substituent effects, especially ortho inductive, resonance and steric terms on different solvent parameters, was studied using the following equation:

where Δlog k=log kX−log kH, σI, σR0 and EsB are the inductive, resonance and steric substituent constants and E, Y and P are the solvent electrophilicity, polarity and polarizability parameters, respectively. In data treatment $\Delta E = E_{\rm S} - E_{{\rm H}_2 {\rm O}}, \ \Delta Y = Y_{\rm S} - Y_{{\rm H}_2 {\rm O}} \ {\rm and} \ \Delta P = P_{\rm S} - P_{{\rm H}_2 {\rm O}}$ were used. The solvent electrophilicity was found to be the main factor responsible for changes in the ortho, para and meta polar substituent effects with medium. The variation of the ortho inductive term with the solvent electrophilicity ES was found to be ca threefold smaller than that for para substituents, whereas the ortho resonance term appeared to vary with solvent very similarly to that for para substituents. The steric term of ortho substituents was found to be approximately independent of solvent parameters. The ortho effect caused by the supplementary inductive effect from ortho position was found to disappear in a solvent whose electrophilic solvating power is comparable to that of 60% aqueous ethanol (E ≈ 13.3). Copyright © 2005 John Wiley & Sons, Ltd.
Water‐swollen highly oxygen permeable membranes: Analytical technique and syntheses
Authors: Erdodi G. , Kennedy J. P.
Published: June 2005

A generally accepted method for the determination of high oxygen permeabilities (Dk >100 barrers) of water‐immersed membranes is unavailable. We designed and developed a generally applicable method, together with simple equipment, to measure the oxygen permeability up to Dk ∼800 barrers of highly oxygen permeable membranes in contact with water. A theory of the methodology is also presented, giving particular attention to the boundary layer effect and the edge effect. The practical applicability of our technique is demonstrated by preparing and using highly oxygen permeable water‐logged membranes, such as polydimethylsiloxane and polysiloxane copolymers important for medicine. According to our measurements, the Dk's of polydimethylsiloxane, poly(dimethylsiloxane0.80‐co‐diethylsiloxane0.20), and poly(dimethylsiloxane0.84‐co‐diphenylsiloxane0.16) are 792 ± 26, 505 ± 10, and 249 ± 10 barrers, respectively. Evidently, the oxygen permeabilities of polysiloxanes are strongly reduced by substituting the OSiMe2 repeat unit with the structurally similar OSiEt2 and OSiPh2 repeats. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 3491–3501, 2005
Advanced flame‐retardant epoxy resins from phosphorus‐containing diol
Authors: Alcón M. José , Ribera Gemma , Galià Marina , Cádiz Virginia
Published: June 2005

Phosphorus‐containing epoxy systems were prepared from isobutylbis(hydroxypropyl)phosphine oxide (IHPO) and diglycidyl ether of bisphenol A (DGEBA). Diethyl‐N,N‐bis(2‐hydroxyethyl) aminomethyl phosphonate (Fyrol 6) could not be incorporated into the epoxy backbone by a reaction with either epichlorohydrin or DGEBA because intramolecular cyclization took place. The curing behavior of the IHPO–DGEBA prepolymer with two primary amines was studied, and materials with moderate glass‐transition temperatures were obtained. V‐0 materials were obtained when the resins were tested for ignition resistance with the UL‐94 test. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 3510–3515, 2005
Characterization of the improvised explosive urea nitrate using electrospray ionization and atmospheric pressure chemical ionization
Authors: Tamiri Tsippy
Published: June 2005

Mass spectra of urea nitrate were measured in electrospray ionization and in atmospheric pressure chemical ionization in the negative mode. In both ionization methods two characteristic adduct ions containing the intact molecule [urea nitrate+NO3]− and [urea nitrate+HNO3+NO3]− are shown. The structure of the two adduct ions was deduced using measurements of isotopically labeled urea nitrate. Collision‐induced dissociation measurements of the adduct ions show typical losses enabling the identification of urea nitrate in trace amounts. Using these methods urea nitrate was identified in real cases. Copyright © 2005 John Wiley & Sons, Ltd.
Development of a rapid method for the determination of glimepiride in human plasma using liquid‐liquid extraction based on 96‐well format micro‐tubes and liquid chromatography/tandem mass spectrometry
Authors: Dotsikas Yannis , Kousoulos Constantinos , Tsatsou Georgia , Loukas Yannis L.
Published: June 2005

A semi‐automated liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed for the determination of glimepiride in human plasma. The plasma samples were treated by liquid‐liquid extraction (LLE) in 1.2 mL 96‐well format micro‐tubes. Glimepiride and the internal standard (IS) glibenclamide were extracted from human plasma by LLE, using a mixture of ethyl acetate/diethyl ether 50:50 (v/v) as the organic solvent. After vortexing, centrifugation and freezing, the supernatant organic solvent was evaporated. The analyte and IS were dissolved in a small volume of a reconstitution solution, an aliquot of which was analyzed by reversed‐phase LC/MS/MS with positive ion electrospray ionization, using multiple reaction monitoring. The method proved to be sensitive and specific for both drugs, and statistical evaluation revealed excellent linearity for the range of concentrations 2.0–500.0 ng/mL with very good accuracy and inter‐ and intra‐day precisions. The proposed method enabled the rapid and reliable determination of glimepiride in pharmacokinetic or bioequivalence studies after per os administration of a 3 or 4 mg tablet of glimepiride. Copyright © 2005 John Wiley & Sons, Ltd.
On‐line desalting and determination of morphine, morphine‐3‐glucuronide and morphine‐6‐glucuronide in microdialysis and plasma samples using column switching and liquid chromatography/tandem mass spectrometry
Authors: Bengtsson Jörgen , Jansson Britt , Hammarlund‐Udenaes Margareta
Published: June 2005

A sensitive and reproducible method for the determination of morphine and the metabolites morphine‐3‐glucuronide (M3G) and morphine‐6‐glucuronide (M6G) was developed. The method was validated for perfusion fluid used in microdialysis as well as for sheep and human plasma. A C18 guard column was used to desalt the samples before analytical separation on a ZIC HILIC (hydrophilic interaction chromatography) column and detection with tandem mass spectrometry (MS/MS). The mobile phases were 0.05% trifluoroacetic acid (TFA) for desalting and acetonitrile/5 mM ammonium acetate (70:30) for separation. Microdialysis samples (5 µL) were directly injected onto the system. The lower limits of quantification (LLOQ) for morphine, M3G and M6G were 0.50, 0.22 and 0.55 ng/mL, respectively, and the method was linear from LLOQ to 200 ng/mL. For plasma, a volume of 100 µL was precipitated with acetonitrile containing internal standards (deuterated morphine and metabolites). The supernatant was evaporated and reconstituted in 0.05% TFA before the desalting process. The LLOQs for sheep plasma were 2.0 and 3.1 ng/mL and the ranges were 2.0–2000 and 3.1–3100 ng/mL for morphine and M3G, respectively. For human plasma, the LLOQs were 0.78, 1.49 and 0.53 ng/mL and the ranges were 0.78–500, 1.49–1000 and 0.53–500 ng/mL for morphine, M3G and M6G, respectively. Copyright © 2005 John Wiley & Sons, Ltd.
Dissociation of peptide ions by fast atom bombardment in a quadrupole ion trap
Authors: Misharin Alexander S. , Silivra Oleg A. , Kjeldsen Frank , Zubarev Roman A.
Published: June 2005

A new technique for fragmentation of cations and anions of peptides stored in ion traps including radiofrequency devices is described. The technique involves irradiation of peptide ions by a beam of particles generated by a fast atom bombardment (FAB) gun. This irradiation leads to fragmentation of NCα backbone bonds (c‐ and z‐fragments) and SS bonds for cations and Cα–C backbone bonds (a‐ and x‐fragments) for anions of peptides. The fragmentation patterns observed are hypothesized to be due to the interaction of peptide ions with metastable, electronically excited species generated by the FAB gun. Interaction of a metastable atom A* with a peptide n‐cation Mn+ leads to the electron transfer from the metastable atom to the polycation through the formation of an ion‐pair collision complex A+. · · · M(n‐1)+. and subsequent fragmentation of the peptide cation. Thus, for polycations, this metastable‐induced dissociation of ions (MIDI) is similar to the phenomenon of electron capture dissociation (ECD). Interaction of A* with an anion leads to the deexcitation of the metastable species and detachment of an electron from the anion. This in turn leads to backbone fragmentation similar to that in electron detachment dissociation (EDD). The MIDI technique is robust and efficient, and it is applicable to peptides in as low charge states as 2+ or 2−. Copyright © 2005 John Wiley & Sons, Ltd.
Comparison of negative and positive ion electrospray ionization mass spectra of calmodulin and its complex with trifluoperazine
Authors: Watt Stephen J. , Oakley Aaron , Sheil Margaret M. , Beck Jennifer L.
Published: June 2005

The protein calmodulin (apoCaM) undergoes a conformational change when it binds calcium. This structure of the protein (Ca4CaM) is a dumbbell‐shaped molecule that undergoes a further profound conformational change on binding of the antipsychotic drug trifluoperazine (TFP). Experimental conditions were developed to prepare samples of apoCaM, Ca4CaM and Ca4CaM/TFP that were substantially free of sodium. The effects of the conformational changes of calmodulin on the charge‐state distributions observed in positive ion and negative ion electrospray ionization (ESI) mass spectra were examined. Conversion of apoCaM into Ca4CaM was concomitant with a change in the negative ion ESI mass spectrum whereby the 16− ion was the most abundant ion observed for the apo form and the 8− ion was the most abundant for the complex. In contrast, in the positive ion ESI mass spectra of apoCaM and Ca4CaM, the most abundant species in each case was the 8+ ion. When a complex of Ca4CaM with TFP was prepared, the most abundant species was the 5+ ion. This is consistent with a conformational change of Ca4CaM that rendered some basic sites inaccessible to ionization in the ESI process. Using the same Ca4CaM/TFP mixture, no complex with TFP was observed in negative ion ESI mass spectra. These observations are discussed in the context of the structural changes that are known to occur in calmodulin, and suggestions are made to explain the apparently conflicting data. The results reported here reflect on the validity of using differences in charge‐state distributions observed in ESI mass spectra to assess conformational changes in proteins. Copyright © 2005 John Wiley & Sons, Ltd.
Structural characterization of flavonol di‐O‐glycosides from Farsetia aegyptia by electrospray ionization and collision‐induced dissociation mass spectrometry
Authors: Shahat Abdelaaty A. , Cuyckens Filip , Wang Wu , Abdel‐Shafeek Khaled A. , Husseiny Husseiny A. , Apers Sandra , Van Miert Sabine , Pieters Luc , Vlietinck Arnold J. , Claeys Magda
Published: June 2005

This study reports the application of mass spectrometric methods to characterize unknown flavonoids of the herb Farsetia aegyptia Turra (Crucifereae). High‐performance liquid chromatography was performed in combination with UV‐photodiode array detection (LC/UV‐DAD) and electrospray ionization mass spectrometry (LC/ESI‐MS) in both positive and negative ion modes. Collision‐induced dissociation (CID) mass spectral data were obtained off‐line by nanospray (nano‐ESI) analysis, which provided a wealth of information and led to the structural proposal of the flavonol di‐O‐glycosides present in the herb extract. In addition to the mass spectral data, we also report NMR data for the major compound which allowed the completion of its structural elucidation. The Farsetia aegyptia Turra herb extract was found to contain three flavonol di‐O‐glycosides containing a monosaccharidic residue linked to the 3‐O position and a disaccharidic residue linked to the 7‐O position; the major compound was characterized as the new flavonoid, isorhamnetin 3‐O‐α‐L‐arabinoside 7‐O‐[β‐D‐glucosyl‐1 → 2]‐αLrhamnoside. Different types of CID spectra, i.e., low‐energy [M+H]+, [M+Na]+ and [MH]− spectra as well as high‐energy [M+Na]+ spectra, were evaluated with respect to their utility to locate the O‐linked saccharidic residues in flavonol di‐O‐glycosides and to determine the sequence in the disaccharidic part. In agreement with previously published data, the 3‐O‐glycosyl residue was more readily lost from the protonated molecule than the 7‐O‐glycosyl residue. The opposite behavior was noted for the fragmentation of the deprotonated and sodiated molecules. Radical ions were observed in the high‐energy [M+Na]+ CID spectra which provided supporting information on the glycosylation positions. Copyright © 2005 John Wiley & Sons, Ltd.
Acetonitrile‐induced unfolding of the photosystem II manganese‐stabilizing protein studied by electrospray mass spectrometry
Authors: Zhang Li , Zhang Feng , Zhang Su‐Yan , Guo Yin‐Long , Xu Chun‐He
Published: June 2005

In this paper an acetonitrile‐induced unfolding of the manganese‐stabilizing protein (MSP) of photosystem II was discovered. More distinct unfolding states of MSP were identified than previously by using mainly electrospray ionization mass spectrometry (ESI‐MS), together with fluorescence spectra and far‐UV circular dichroism (CD) at pH 2.0, 6.2 or 11.6, and with acetonitrile concentrations from 0 to 50%. At pH 6.2 with acetonitrile concentration changing from 0 to 10%, relatively broad charge‐state distributions and poor intensity were observed in ESI‐MS, indicating the presence of coexisting conformers. It was concluded that the structure of the MSP protein is unlikely to be a tightly folded form. When the concentration of acetonitrile was 20–40%, simulating the state in the biological membrane, changes in the state of unfolding of MSP were observed to a certain extent using ESI‐MS, fluorescence and CD spectroscopy. The charge‐state distribution in ESI‐MS was found to move toward high states (from 13+ to 27+ to 15+ to 31+) with increasing acetonitrile concentration. At pH 2.0, the MSP structure is rearranged into an unfolded state, and at pH 11.6 the MSP structure is induced to assume another unordered state by deprotonation of appropriate residues. An interesting observation was that a second peak envelope emerged with 20–50% acetonitrile in the medium at pH 11.6. Copyright © 2005 John Wiley & Sons, Ltd.
Multimodal Treatment of Gastrointestinal Tract Tumors:Consequences for Surgery
Authors: Síewert J. Rüdiger , Stein Hubert J. , von Rahden Burkhard H.A.
Published: June 2005

Formerly an exclusive business of surgery, gastrointestinal (GI) tumors are nowadays increasingly approached with multimodal strategies. Neoadjuvant concepts have had a particularly far‐reaching impact on surgery and have contributed to improved survival. Modern pre‐treatment staging and risk assessment provide the basis for decision on one of three general treatment concepts (1) Early cancers, confined to the mucosal/submucosal layers, are approached with primary surgery, without prior antineoplastic therapy. (2) Systemically metastasized tumors receive merely palliative treatment. (3) Locally advanced cancers are increasingly approached with neoadjuvant strategies. The benefit from these preoperative protocols is proven for diverse entities, but is evidently confined to a specific subgroup patients, i.e., the responders to neoadjuvant treatment. These are the ones benefiting most from subsequent surgical resection, which is required to ensure complete removal of the residual tumor tissue, as complete tumor regression occurs very rarely and cannot be proven without a specimen. The fact that responders will benefit and non‐responders will not benefit or will even deteriorate during the neoadjuvant treatment makes early response prediction most demanding. An amazing new approach is the use of position emission tomography with fluro‐desoxyglucose (FDG‐PET) to assess the “metabolic response,” which is possible as early as 14 days after initiation of the neoadjuvant protocol. This strategy offers the chance for modulating the surgical approach in accord i.e., with such metrobolic response termination of the protocol and proceeding to resection in the case of non‐response.

The future of GI cancer surgery is multimodal therapy in a response‐based fashion and requires reponse‐based trials for further evaluation.
High Hospital Volume Is Associated with Better Outcomes for Breast Cancer Surgery: Analysis of 233,247 Patients
Authors: Guller Ulrich , Safford Shawn , Pietrobon Ricardo , Heberer Michael , Oertli Daniel , Jain Nitin B.
Published: June 2005

Background:

The relationship between hospital volume and outcomes needs to be further elucidated for low‐risk procedures such as surgical therapy of localized breast cancer. The objective of this investigation was to assess the relationship between hospital volume and outcomes for breast cancer surgery.

Methods:

A total of 233,247 patients who underwent breast‐conserving therapy (BCT) and breast‐ablative therapy (BAT) for localized breast cancer were extracted from 13 years (1988–2000) of the Nationwide Inpatient Samples. Hospital volume was classified as low (<30 cases/year), intermediate (≥ 30 to <70cases/year), and high (≥ 70 cases/year). Multiple linear and logistic regression analyses were used to assess the risk‐adjusted association between hospital volume and outcomes.

Results:

In risk‐adjusted analyses, patients operated on at low‐volume hospitals were 3.04 (p = 0.03) times more likely to die after BCT compared with patients operated on at high‐volume hospitals. Similarly, low‐volume hospitals had a significantly higher likelihood of postoperative complications (odds ratio [OR] = 1.73, p = 0.01 for BCT; OR = 1.44, p < 0.001 for BAT) compared with high‐volume hospitals. Compared with low‐volume hospitals, length of hospital stay was significantly shorter and nonroutine patient discharge significantly lower for high‐volume providers for both BCT and BAT (all p < 0.001). Patients were also significantly less likely to undergo BCT if operated on in a low‐ or intermediate‐volume hospital compared with a high‐volume provider (p < 0.001).

Conclusions:

High‐volume hospitals had significantly lower nonroutine patient discharge, postoperative morbidity and mortality, shorter length of hospital stay, and higher likelihood of performing BCT. Referral of patients with localized breast cancer to high‐volume hospitals may be justified.
Yeast HAT1 and HAT2 deletions have different life‐span and transcriptome phenotypes
Authors: Rosaleny Lorena E. , Antúnez Oreto , Ruiz-García Ana B. , Pérez-Ortín José E. , Tordera Vicente
Published: June 2005

HAT‐B is a yeast histone acetyltransferase composed of Hat1, Hat2 and Hif1 proteins. We demonstrate that a hat2 mutant or a hat1hat2 double mutant, but not a hat1 mutant, have an extended life‐span. Transcriptome analysis shows that the single hat mutants are not very different from wild type. However, the comparison of the hat1 and hat2 transcriptomes shows that they are different. The hat1hat2 double mutant shows a transcriptional phenotype similar to that of the hat1 mutant but strongly enhanced. These results indicate that Hat2p could have additional functions in the cell to those of Hat1p.
Internal Fixation of Unstable Fracture Dislocations of the Proximal Interphalangeal Joint
Authors: GRANT I. , BERGER A. C. , THAM S. K. Y.
Published: June 2005

We report a group of 14 patients with fracture dislocations of the proximal interphalangeal joint with fracture fragments of adequate size to allow reduction of the proximal interphalangeal joint and internal mini screw fixation of the bone fragment attached to the palmar plate to the base of the middle phalanx. Three years after surgery, (range 25–52 months) the average total active range of motion of the proximal interphalangeal joint was 100° (range 65–115°) for the acute group (operation within 14 days of injury, n = 7) and 86° (range 60–110°) for the chronic group (operation on average 46 days after injury, range 21–120 days, n = 7). Longer delay from injury was associated with a decreased total range of motion ( P = 0.028). Further subluxation occurred in three chronic group patients, one required further surgery. The key to successful treatment of this injury is the re-establishment of joint congruity and early mobilization. With appropriate patient selection, pain free, satisfactory range of motion can be achieved. There is a risk of persistent subluxation or dislocation, particularly if treatment is delayed.
Psychological risk factors of incidence of breast cancer: a prospective cohort study in Finland
Authors: ARO A. R. , KONING H. J. DE , SCHRECK M. , HENRIKSSON M. , ANTTILA A. , PUKKALA E.
Published: June 2005

Background. Belief that depression and other psychological factors predict breast cancer is common, but there have been few prospective epidemiological studies on this relationship.

Method. The relationship between depression, personality traits, illness attitudes, life events and health history, and breast cancer risk was studied in a prospective, 6–9 year follow-up of a cohort study of 10892 Finnish women of 48–50 years of age at the baseline. Cancer cases were obtained from the Cancer Registry of Finland. Multivariate logistic regression analysis was performed controlling for socioeconomic factors, family history of cancer, parity, and health behaviours.

Results. Breast cancer incidence in the cohort was 1·15 times the average in age group 50–59. There was no evidence of depression, trait anxiety, cynical distrust, or coping being significant predictors of breast cancer incidence.

Conclusion. In this cohort study with the 6–9 year follow-up, psychological factors such as depression, trait anxiety, cynical distrust, or coping did not increase breast cancer risk.
Anomalous visual experiences, negative symptoms, perceptual organization and the magnocellular pathway in schizophrenia: a shared construct?
Authors: KÉRI SZABOLCS , KISS IMRE , KELEMEN OGUZ , BENEDEK GYÖRGY , JANKA ZOLTÁN
Published: June 2005

Background. Schizophrenia is associated with impaired visual information processing. The aim of this study was to investigate the relationship between anomalous perceptual experiences, positive and negative symptoms, perceptual organization, rapid categorization of natural images and magnocellular (M) and parvocellular (P) visual pathway functioning.

Method. Thirty-five unmedicated patients with schizophrenia and 20 matched healthy control volunteers participated. Anomalous perceptual experiences were assessed with the Bonn Scale for the Assessment Basic Symptoms (BSABS). General intellectual functions were evaluated with the revised version of the Wechsler Adult Intelligence Scale. The 1–9 version of the Continuous Performance Test (CPT) was used to investigate sustained attention. The following psychophysical tests were used: detection of Gabor patches with collinear and orthogonal flankers (perceptual organization), categorization of briefly presented natural scenes (rapid visual processing), low-contrast and frequency-doubling vernier threshold (M pathway functioning), isoluminant colour vernier threshold and high spatial frequency discrimination (P pathway functioning).

Results. The patients with schizophrenia were impaired on test of perceptual organization, rapid visual processing and M pathway functioning. There was a significant correlation between BSABS scores, negative symptoms, perceptual organization, rapid visual processing and M pathway functioning. Positive symptoms, IQ, CPT and P pathway measures did not correlate with these parameters. The best predictor of the BSABS score was the perceptual organization deficit.

Conclusions. These results raise the possibility that multiple facets of visual information processing deficits can be explained by M pathway dysfunctions in schizophrenia, resulting in impaired attentional modulation of perceptual organization and of natural image categorization.
Evaluating the contribution of changes in isoprene emissions to surface ozone trends over the eastern United States
Authors: Fiore Arlene M. , Horowitz Larry W. , Purves Drew W. , Levy Hiram , Evans Mathew J. , Wang Yuxuan , Li Qinbin , Yantosca Robert M.
Published: June 2005

Reducing surface ozone (O3) to concentrations in compliance with the national air quality standard has proven to be challenging, despite tighter controls on O3 precursor emissions over the past few decades. New evidence indicates that isoprene emissions changed considerably from the mid‐1980s to the mid‐1990s owing to land‐use changes in the eastern United States (Purves et al., 2004). Over this period, U.S. anthropogenic VOC (AVOC) emissions decreased substantially. Here we apply two chemical transport models (GEOS‐CHEM and MOZART‐2) to test the hypothesis, put forth by Purves et al. (2004), that the absence of decreasing O3 trends over much of the eastern United States may reflect a balance between increases in isoprene emissions and decreases in AVOC emissions. We find little evidence for this hypothesis; over most of the domain, mean July afternoon (1300–1700 local time) surface O3 is more responsive (ranging from −9 to +7 ppbv) to the reported changes in anthropogenic NOx emissions than to the concurrent isoprene (−2 to +2 ppbv) or AVOC (−2 to 0 ppbv) emission changes. The estimated magnitude of the O3 response to anthropogenic NOx emission changes, however, depends on the base isoprene emission inventory used in the model. The combined effect of the reported changes in eastern U.S. anthropogenic plus biogenic emissions is insufficient to explain observed changes in mean July afternoon surface O3 concentrations, suggesting a possible role for decadal changes in meteorology, hemispheric background O3, or subgrid‐scale chemistry. We demonstrate that two major uncertainties, the base isoprene emission inventory and the fate of isoprene nitrates (which influence surface O3 in the model by −15 to +4 and +4 to +12 ppbv, respectively), preclude a well‐constrained quantification of the present‐day contribution of biogenic or anthropogenic emissions to surface O3 concentrations, particularly in the high‐isoprene‐emitting southeastern United States. Better constraints on isoprene emissions and chemistry are needed to quantitatively address the role of isoprene in eastern U.S. air quality.
Aeration for plant root respiration in a tidal marsh
Authors: Li Hailong , Li Ling , Lockington David
Published: June 2005

This paper investigates the tidal effects on aeration conditions for plant root respiration in a tidal marsh. We extend the work of Ursino et al. (2004) by using a two‐phase model for air and water flows in the marsh. Simulations have been conducted to examine directly the link between the airflow dynamics and the aeration condition in the marsh soil. The results show that the effects of entrapped air on water movement in the vadose zone are significant in certain circumstances. Single‐phase models based on Richards' equation, which neglect such effects, may not be adequate for quantifying the aeration condition in tidal marsh. The optimal aeration condition, represented by the maximum of the integral magnitude of tidally advected air mass (TAAM) flux, is found to occur near the tidal creek for the four soil textures simulated. This may explain the observation that some salt marsh plant species grow better near tidal creeks than in the inner marsh areas. Our analyses, based on the two‐phase model and predicted TAAM flux magnitude, provide further insight into the “positive feedback” mechanism proposed by Ursino et al. (2004). That is, pioneer plants may grow successfully near the creek where the root aeration condition is optimal. The roots of the pioneer plants can soften and loosen the rhizosphere soil, which increases the evapotranspiration rate, the soil porosity, and absolute permeability and weakens the capillary effects. These, in turn, improve further the root aeration conditions and may lead to colonization by plants less resistant to anaerobic conditions.
Perpendicular magnetization of epitaxial CrPtx films
Authors: Hu Y. M. , Huang J. C. A. , Chen C. W. , Lee C. H. , Lin M. J.
Published: June 2005

Perpendicular magnetization and Kerr effects of epitaxial CrPtx films have been studied as functions of the crystal orientation, alloy composition, and growth temperature. The orientation dependence studies reveal that only the (111)-oriented CrPtx films possess perpendicular magnetization, while the (311) and (100) films are magnetized in plane. The composition and temperature dependencies show that the CrPtx films possess optimal perpendicular magnetization and Kerr effect at x∼3 and growth temperature ∼850±25°C. Anisotropic ordering parameter along the (nearly) in-plane and plane-normal directions was observed. The optimal composition and temperature conditions are accompanied by the highest plane-normal L12 ordering parameter.