bluuebunny/crossref_metadata_2025 huggingface dataset:
Scaled‐up separation of cellobiohydrolase1 from a cellulase mixture by ion‐exchange chromatography
Authors: Ye Zhuoliang , Lane Andrew N. , Willing Gerold A. , Berson R. Eric
Published: September 2011

Enzymatic hydrolysis of cellulose often involves cellulases produced by Trichoderma reesei, of which cellobiohydrolase1 (CBH1) is the most abundant (about 60% of total cellulases) and plays an important role in the hydrolysis of crystalline cellulose. A method for separating sufficient quantities from the bulk cellulase cocktail is highly desirable for many studies, such as those that aim to characterize binding and hydrolysis kinetics of CBH1. In this work, CBH1 was separated from other Spezyme CP cellulases by ion‐exchange chromatography using an efficient modification of a smaller scale process. The ion‐exchange column was connected to a vacuum manifold system to provide a steady flow through parallel columns and thus achieve scale‐up for enzyme separation. With five 5‐mL columns running in parallel, about 55 mg of CBH1 was separated from 145 mg of Spezyme CP in a single separation. Step elution was used to replace the continuous gradient used at smaller scale. The purified CBH1 was collected in the fraction eluted with a buffer containing 0.33 M salt and showed comparable purity and activity as the enzyme purified by a fast protein liquid chromatography system. The stability of separated CBH1 was studied for up to 2 days and good thermal stability was observed. Separated CBH1 also showed both high adsorption to bacterial microcrystalline cellulose with ∼4 μmol/g maximum adsorption and a Ka of 5.55 ± 2.34 μM−1, and good hydrolytic activity based on atomic force microscopy observations that show a reduction in fiber height. © 2011 American Institute of Chemical Engineers Biotechnol. Prog., 2011
Recovery of Terephthalic Acid from Alkali Reduction Wastewater by Cooling Crystallization
Authors: Wu S.‐C. , Cheng Z.‐M. , Wang S.‐D. , Shan X.‐L.
Published: September 2011

A process for the recovery and purification of terephthalic acid (TA) from alkali reduction wastewater is reported. TA was first precipitated from alkali reduction wastewater by acidification with sulfuric acid, and then the produced crude TA was dissolved in dimethylacetamide (DMA) so that crude TA could be purified from the solution by cooling crystallization. The results indicated that acidification could reduce the chemical oxygen demand of the wastewater by 83 %, and the purity of TA by crystallization could reach 99.91 %. A correlation was proposed in describing the solubility of crude TA in DMA from 303.4 to 358.65 K, which gives a mean relative discrepancy of less than 1.14 %. The cooling rate of the mother liquor had a large influence on the crystal size distribution. At an average cooling rate of 1.18 K min–1, the particle size distribution of TA was narrow and the average size was about 100 μm. In a bench‐scale study, it was demonstrated that the crystallized product can be recycled as the raw material for polyethylene terephthalate production.
Biomimetic Oxidation Reactions of a Naked Manganese(V)–Oxo Porphyrin Complex
Authors: Lanucara Francesco , Crestoni Maria Elisa
Published: September 2011

The intrinsic reactivity of a manganese(V)‐oxo porphyrin complex, a typically fleeting intermediate in catalytic oxidation reactions in solution, has been elucidated in a study focused on its gas‐phase ion‐chemistry. The naked high‐valent MnV‐oxo porphyrin intermediate 1 ([(tpfpp)MnVO]+; tpfpp=meso‐tetrakis(pentafluorophenyl)porphinato dianion), has been obtained by controlled treatment of [(tpfpp)MnIII]Cl (2‐Cl) with iodosylbenzene in methanol, delivered in the gas phase by electrospray ionization and assayed by FT‐ICR mass spectrometry. A direct kinetic study of the reaction with selected substrates, each containing a heteroatom X (X=S, N, P) including amines, sulfides, and phosphites, was thus performed. Ionic products arising from electron transfer (ET), hydride transfer (HT), oxygen‐atom transfer (OAT), and formal addition (Add) may be observed, with a predominance of two‐electron processes, whereas the product of hydrogen‐atom transfer (HAT), [(tpfpp)MnIVOH]+, is never detected. A thermochemical threshold for the formation of the product radical cation allows an evaluation of the electron‐transfer ability of a MnV‐oxo complex, yielding a lower limit of 7.85 eV for the ionization energy of gaseous [(tpfpp)MnIVO]. Linear free‐energy analyses of the reactions of para‐substituted N,N‐dimethylanilines and thioanisoles indicate that a considerable amount of positive charge is developed on the heteroatom in the oxidation transition state. Substrates endowed with different heteroatoms, but similar ionization energy display a comparable reaction efficiency, consistent with a mechanism initiated by ET. For the first time, the kinetic acidity of putative hydroxo intermediates playing a role in catalytic oxidations, [(tpfpp)FeIVOH]+ and [(tpfpp)MnIVOH]+, has been investigated with selected reference bases, revealing a comparatively higher basicity for the ferryl, [(tpfpp)FeIVO], with respect to the manganyl, [(tpfpp)MnIVO], unit. Finally, the neat association reaction of 2 has been studied with various ligands showing that harder ligands are more strongly bound.
ChemInform Abstract: Solving the Structure of Li Ion Battery Materials with Precession Electron Diffraction: Application to Li2CoPO4F.
Authors: Hadermann Joke , Abakumov Artem M. , Turner Stuart , Hafideddine Zainab , Khasanova Nellie R. , Antipov Evgeny V. , Van Tendeloo Gustaaf
Published: September 2011

The crystal structure of Li2CoPO4F is completely solved from precession electron diffraction data, including the location of the Li atoms.
ChemInform Abstract: Perovskite, LiNbO3, Corundum, and Hexagonal Polymorphs of (In1‐xMx)MO3.
Authors: Belik Alexei A. , Furubayashi Takao , Yusa Hitoshi , Takayama‐Muromachi Eiji
Published: September 2011

The LiNbO3 phase (LN‐phase) of the title compound with x = 0.143 and M: Fe0.5Mn0.5 is synthesized from stoichiometric mixtures of In2O3, Mn2O3, and Fe2O3 (Pt capsule, 6 GPa, 1773 K, 30 min).
ChemInform Abstract: Giant Negative Thermal Expansion in the Iron Perovskite SrCu3Fe4O12.
Authors: Yamada Ikuya , et al. et al.
Published: September 2011

Polycrystalline SrCu3Fe4O12 is synthesized from a stoichiometric mixture of Sr(NO3)2, Cu(NO3)2, Fe(NO3)3, and a fivefold molar excess of citric acid dissolved in a mixture of water and ethanediol (433 K, ≈12 h) followed by decomposition of the resulting solid at 723 and 973 K.
ChemInform Abstract: Synthesis and Enhanced Luminescence Properties of Li‐Doped CaTiO3:Pr3+ Ceramic Phosphors.
Authors: Yang Hyun Kyoung , Chung Jong Won , Moon Byung Kee , Choi Byung Chun , Jeong Jung Hyun , Bae Jong Seong , Kim Kwang Ho
Published: September 2011

The title phosphors are prepared by solid state reaction of CaCO3, TiO2, Li2CO3 (0.5, 1, 2, 5 wt.%), and Pr6O11 (800 °C, 4 h, followed by sintering at 1200 °C for 2 h).
ChemInform Abstract: Oxygen‐Deficient R2MoO6‐δ (R: Tb, Dy, Y, Ho, Er, Tm, Yb) with Fluorite Structure as Potential Anodes in Solid Oxide Fuel Cells.
Authors: Aguadero A. , Martinez‐Lope M. J. , Pomjakushin V. , Alonso J. A.
Published: September 2011

The title compounds are synthesized by solid state reaction of stoichiometric mixtures of Ln2O3 (Ln: Y, Dy, Ho, Er, Tm, Yb) and MoO3 (air, 1150 °C, 12 h) followed by treatment in 5% H2/N2 (900 °C, 12 h).
ChemInform Abstract: Ion‐Induced Transformation of Magnetism in a Bimetallic CuFe Prussian Blue Analogue.
Authors: Okubo Masashi , et al. et al.
Published: September 2011

K0.14Cu1.43[Fe(CN)6]·5H2O is synthesized by dropwise addition of an aqueous solution of CuSO4 to an aqueous solution of K3[Fe(CN)6].
ChemInform Abstract: Reversible Sodium Ion Insertion in Single Crystalline Manganese Oxide Nanowires with Long Cycle Life.
Authors: Cao Yuliang , Xiao Lifen , Wang Wei , Choi Daiwon , Nie Zimin , Yu Jianguo , Saraf Laxmikant V. , Yang Zhenguo , Liu Jun
Published: September 2011

Single crystalline Na4Mn9O18 nanowires are synthesized using a polymer‐pyrolysis method.
ChemInform Abstract: 3‐V Full Cell Performance of Anode Framework TiNb2O7/Spinel LiNi0.5Mn1.5O4.
Authors: Han Jian‐Tao , Goodenough John B.
Published: September 2011

A carbon‐coated TiNb2O7 anode and a LiNi0.5Mn1.5O4 cathode are assembled into 3‐V full cell.
ChemInform Abstract: Room Temperature Synthesis of Protonated Layered Titanate Sheets Using Peroxo Titanium Carbonate Complex Solution.
Authors: Sutradhar Narottam , Sinhamahapatra Apurba , Pahari Sandip Kumar , Bajaj Hari C. , Panda Asit Baran
Published: September 2011

A titanium peroxo carbonate complex is prepared from an EtOH solution of Ti(OiPr)4 by precipitation of titanium hydroxide with an ammoniacal H2O solution followed by addition of aqueous (NH4)2CO3 and 30% aq.
ChemInform Abstract: Two Organic Hybrid Thiogermanates [Ni(dien)2](H2dien)Ge2Se6 and [Ni(teta)2]2Ge4S10.
Authors: Liu Xing , Zhou Jian , He Jun , Huang Zhi‐wei
Published: September 2011

Compound (III) crystallizes in the triclinic space group P$\bar 1$ with Z = 1 and consists of discrete [Ge2S6]4‐ anions with [Ni(dien)2]2+ and [H2dien]2+ cations as counterions.
ChemInform Abstract: A Metastable Metal with Decagonal Local Symmetry Obtained by Low‐Temperature Pseudomorphosis.
Authors: Kaiser Martin , Isaeva Anna , Ruck Michael
Published: September 2011

Black crystals of the metastable intermetallic compound Bi28Ni25 are prepared by reduction of Bi28Ni25I5 crystals with a solution of BuLi in boiling hexane (69 °C, argon atmosphere, 2 d; 90% yield).
ChemInform Abstract: Nonenzymatic Dynamic Kinetic Resolution of α‐(Arylthio)‐ and α‐(Alkylthio)alkanoic Acids.
Authors: Yang Xing , Birman Vladimir B.
Published: September 2011

The title resolution proceeds smoothly in the presence of a pyrimidobenzothiazole organocatalyst.
ChemInform Abstract: Generation and Reactivity of Aza‐Oxyallyl Cationic Intermediates: Aza‐[4 + 3] Cycloaddition Reactions for Heterocycle Synthesis.
Authors: Jeffrey Christopher S. , Barnes Korry L. , Eickhoff John A. , Carson Christopher R.
Published: September 2011

Computational and experimental data support that the title reaction proceeds through an aza‐oxyallylic cationic intermediate which is stabilized by the N‐alkoxy substituent.
ChemInform Abstract: Mild and Selective Boronic Acid Catalyzed 1,3‐Transposition of Allylic Alcohols and Meyer—Schuster Rearrangement of Propargylic Alcohols.
Authors: Zheng Hongchao , Lejkowski Michal , Hall Dennis G.
Published: September 2011

Highly electron‐deficient polyfluoroarylboronic acid catalysts (I)—(IV) are applied to the rearrangement of allylic alcohols and propargylic alcohols.
ChemInform Abstract: FeCl3‐Mediated Reaction of Alkynols with Iodine: An Efficient and Convenient Synthetic Route to Vinyl Iodides.
Authors: Su Lei , Lei Chun‐Yan , Fan Wei‐Yong , Liu Liang‐Xian
Published: September 2011

The FeCl3‐mediated reaction of alkynols with iodine results in the formation of a variety of iodocycloenol ethers.
ChemInform Abstract: ZnCl2‐Catalyzed Hydrodefluorination of gem‐Difluoromethylene Derivatives with Lithium Aluminum Hydride.
Authors: Cheng Jianhang , Wu Jingjing , Cao Song
Published: September 2011

A novel system for the process is developed.
ChemInform Abstract: Pd‐Catalyzed Intermolecular C—H Amination with Alkylamines.
Authors: Yoo Eun Jeong , Ma Sandy , Mei Tian‐Sheng , Chan Kelvin S. L. , Yu Jin‐Quan
Published: September 2011

A novel protocol to effect monoselective C—H amination on a broad range of benzamide substrates with electrophilic O‐benzoyl hydroxylamines is described.
ChemInform Abstract: In situ Generated (Hypo)Iodite Catalysts for the Direct α‐Oxyacylation of Carbonyl Compounds with Carboxylic Acids.
Authors: Uyanik Muhammet , Suzuki Daisuke , Yasui Takeshi , Ishihara Kazuaki
Published: September 2011

The introduction of an O‐acyl group at the α‐position of carbonyl compounds is smoothly achieved using tetrabutylammonium iodide catalyst in the presence of hydrogen peroxide or tert‐butyl hydroperoxide.
ChemInform Abstract: Task‐Oriented Use of Ionic Liquids: Efficient Acetylation of Alcohols and Phenols.
Authors: Lopez Ignacio , Bravo Jose Luis , Caraballo Manuel , Barneto Jose Luis , Silvero Guadalupe
Published: September 2011

[bmim]OAc is found to be an appropriate reaction medium.
ChemInform Abstract: Novel Protection—Deprotection Strategies in Diazeniumdiolate Chemistry: Synthesis of V‐IPA/NO.
Authors: Nandurdikar Rahul S. , Keefer Larry K. , Saavedra Joseph E.
Published: September 2011

A five‐step synthesis of potentially liver selective HNO donor V‐IPA/NO (VIII) is elaborated using a protection—deprotection strategy.
ChemInform Abstract: Rh2(S‐PTAD)4‐Catalyzed Asymmetric Cyclopropenation of Aryl Alkynes.
Authors: Briones John F. , Davies Huw M. L.
Published: September 2011

Cyclopropenyl ketones are formed with high enantioselectivities.
ChemInform Abstract: Pd‐Catalyzed [2 + 2 + 1] Coupling of Alkynes and Arenes: Phenol Diazonium Salts as Mechanistic Trapdoors.
Authors: Schmidt Bernd , Berger Rene , Kelling Alexandra , Schilde Uwe
Published: September 2011

A wide range of spirocyclic compounds is synthesized by the present new palladium‐catalyzed coupling reaction of internal alkynes with 4‐phenol diazonium salts.
ChemInform Abstract: Iron‐Catalyzed Stereospecific Activation of Olefinic C—H Bonds with Grignard Reagent for Synthesis of Substituted Olefins.
Authors: Ilies Laurean , Asako Sobi , Nakamura Eiichi
Published: September 2011

The iron‐catalyzed functionalization of acyclic or cyclic olefins which possess a directing group such as pyridine via stereospecific C—H bond activation in the presence of a mild oxidant and an aromatic cosolvent takes place in a (Z)‐specific manner.
ChemInform Abstract: Cooperative Transition‐Metal and Chiral Broensted Acid Catalysis: Enantioselective Hydrogenation of Imines to Form Amines.
Authors: Zhou Shaolin , Fleischer Steffen , Junge Kathrin , Beller Matthias
Published: September 2011

The procedure constitutes an attractive and environmentally favorable alternative to reactions with precious‐metal catalysts.
ChemInform Abstract: Asymmetric Aza‐Henry Reaction of Chiral Fluoroalkyl α,β‐Unsaturated N‐tert‐Butanesulfinyl Ketoimines: An Efficient Approach to Enantiopure Fluoroalkylated α,β‐Diamines and α,β‐Diamino Acids.
Authors: Zhang Fan , Liu Zhen‐Jiang , Liu Jin‐Tao
Published: September 2011

The presence of a fluoroalkyl group is crucial for the successful stereoselective aza‐Henry reaction.
ChemInform Abstract: Tandem Catalysis by Lipase in a Vinyl Acetate Mediated Cross‐Aldol Reaction.
Authors: Kumar Manjeet , Shah Bahwal A. , Taneja Subhash C.
Published: September 2011

Novozym435/NEt3‐catalyzed treatment of isopropenyl acetate with aromatic aldehydes is found to allow new, mild, and efficient access to β‐hydroxy ketones.
ChemInform Abstract: Grignard‐Type Arylation of Aldehydes via a Rhodium‐Catalyzed C—H Activation under Mild Conditions.
Authors: Yang Luo , Correia Camille A. , Li Chao‐Jun
Published: September 2011

The title reaction provides a new and efficient method to prepare a wide range of benzyl and diarylmethyl alcohols.
ChemInform Abstract: Polystyrene‐Supported Enantiopure 1,2‐Diamines: Development of a Most Practical Catalyst for the Asymmetric Transfer Hydrogenation of Ketones.
Authors: Marcos Rocio , Jimeno Ciril , Pericas Miquel A.
Published: September 2011

The Rh complex RCPC is highly efficient for the hydrogenation of alkyl aryl ketones.
ChemInform Abstract: Catalytic Syntheses of γ‐Functionalized α‐Keto Esters from Thioacetals and N,O‐Acetals.
Authors: Krebs Anke , Bolm Carsten
Published: September 2011

Ester (I) reacts with aromatic thioacetals (II) under mild conditions providing the α‐keto‐γ‐thio esters (III).
ChemInform Abstract: Phosphorofluoridic Acid Ammonium Salts and Acids: Synthesis, NMR Properties, and Application as Acid Catalysts.
Authors: Murai Toshiaki , Tonomura Yusuke , Takenaka Toru
Published: September 2011

Highest yields in the synthesis of the compound (III) are achieved by using the shown catalyst.
ChemInform Abstract: Thiourea Dioxide (TUD): A Robust Organocatalyst for Oxidation of Sulfides to Sulfoxides with TBHP under Mild Reaction Conditions.
Authors: Kumar Subodh , Verma Sanny , Jain Suman L. , Sain Bir
Published: September 2011

The process is highly effective for aromatic and aliphatic thioethers and chemoselective in the presence of other functional groups.
ChemInform Abstract: Synthesis of Unsymmetrical Diarylureas via Pd‐Catalyzed C—N Cross‐Coupling Reactions.
Authors: Breitler Simon , Oldenhuis Nathan J. , Fors Brett P. , Buchwald Stephen L.
Published: September 2011

The Pd‐catalyzed reaction of benzylurea with various aryl chlorides, followed by the hydrogenolysis leads to monoarylurea derivatives.
ChemInform Abstract: Iron‐Catalyzed Quick Homocoupling Reaction of Aryl or Alkynyl Grignard Reagents Using a Phosphonium Ionic Liquid Solvent System.
Authors: Kude Keisuke , Hayase Shuichi , Kawatsura Motoi , Itoh Toshiyuki
Published: September 2011

Bulky substituents decrease the yield in the presented reaction.
ChemInform Abstract: Synthesis of New Chiral Schiff Bases Containing Bromo‐ and Iodo‐Functionalized Hydroxynaphthalene Frameworks.
Authors: Wang Ying , Wang Mei , Wang Yu , Chen Yuee , Sun Licheng
Published: September 2011

Halogen derivatives are converted into their corresponding Schiff bases by means of method D as shown for the examples (III), (VIII) and (X).
ChemInform Abstract: Catalytic Asymmetric Conjugate Addition/Oxidative Dearomatization Towards Multifunctional Spirocyclic Compounds.
Authors: Rudolph Alena , Bos Pieter H. , Meetsma Auke , Minnaard Adriaan J. , Feringa Ben L.
Published: September 2011

The convenient one‐pot procedure includes conjugate addition of alkylmagnesium bromides to α,β‐unsaturated esters and subsequent oxidative cyclization.
ChemInform Abstract: Synthesis and Optoelectronic Properties of Some New Thiahelicenes.
Authors: Moussa Souad , Aloui Faouzi , Ben Hassine Bechir
Published: September 2011

New symmetrical, helically chiral penta‐ and heptacyclic aromatic systems containing two thiophene rings [cf.
ChemInform Abstract: Highly Active and Diastereoselective N,O‐ and N,N‐Yttrium Complexes for Intramolecular Hydroamination.
Authors: Lauterwasser Frank , Hayes Paul G. , Piers Warren E. , Schafer Laurel L. , Braese Stefan
Published: September 2011

Complexes (I) and (II) are highly efficient for the reaction of primary aminoalkynes and aminoalkenes giving pyrrolidine and piperidine derivatives.
ChemInform Abstract: Radical Carbonylation of ω‐Alkynylamines Leading to α‐Methylene Lactams. Synthetic Scope and the Mechanistic Insights.
Authors: Ryu Ilhyong , Fukuyama Takahide , Tojino Mami , Uenoyama Yoshitaka , Yonamine Yuka , Terasoma Nozomi , Matsubara Hiroshi
Published: September 2011

The title reaction allows effective access to 5‐ to 8‐membered rings.
ChemInform Abstract: Synthesis and Antitumor Activity of 5‐[1‐(3‐(Dimethylamino)propyl)‐5‐halogenated‐2‐oxoindolin‐ (3Z)‐ylidenemethyl]‐2,4‐dimethyl‐1H‐pyrrole‐3‐carboxamides.
Authors: Lv Kai , Wang Li‐Li , Liu Ming‐Liang , Zhou Xin‐Bo , Fan Shi‐Yong , Liu Hong‐Ying , Zheng Zhi‐Bing , Li Song
Published: September 2011

Design and synthesis of a variety of title compounds (VII) are described.
ChemInform Abstract: A Novel Acid‐Catalyzed C5‐Alkylation of Oxindoles Using Alcohols.
Authors: Reddy Chada Raji , Jithender Enukonda , Krishna Gaddam , Reddy Gunreddy Venkat , Jagadeesh Bharatam
Published: September 2011

A wide range of 5‐substituted oxindoles is available.
ChemInform Abstract: Synthesis and Crystal Structure of (4bRS,9bRS)‐5‐ (2,4‐Dimethoxyphenyl) ‐4b,9b‐7,7‐dimethyldihydroxy‐4b,5,6,7,8,9b‐hexahydroindeno [1,2‐b]indole‐9,10‐dione.
Authors: Lobo Gricela , Zuleta Elimar , Charris Katiuska , Capparelli Mario V. , Briceno Alexander , Angel Jorge , Charris Jaime
Published: September 2011

The title compound (III) exhibits only marginal antitumor and antibacterial activities.
ChemInform Abstract: The Davis—Beirut Reaction: N1,N2‐Disubstituted‐1H‐indazolones via 1,6‐Electrophilic Addition to 3‐alkoxy‐2H‐indazoles.
Authors: Conrad Wayne E. , Fukazawa Ryo , Haddadin Makhluf J. , Kurth Mark J.
Published: September 2011

A variety of indazole substrates undergoes electrophilic reactions leading to the small libraries of N,N′‐disubstituted indazolones.
ChemInform Abstract: Synthesis and Characterization of Some Novel Isoxazolines and Pyrazolines as Potent Antimicrobial Agents.
Authors: Badadhe P. V. , Chavan N. M. , Mandhane P. G. , Joshi R. S. , Nagargoje D. R. , Gill C. H.
Published: September 2011

8 Compounds of type (III), (IV), and (V) are prepared and screened for their antimicrobial activities.
ChemInform Abstract: Importance of an Acid Additive in the Synthesis of Pyrido[1,2‐a]benzimidazoles by Direct Copper‐Catalyzed Amination.
Authors: Masters Kye‐Simeon , Rauws Tom R. M. , Yadav Ashok K. , Herrebout Wouter A. , Van der Veken Benjamin , Maes Bert U. W.
Published: September 2011

The amination is achieved in the presence of catalytic copper and an acid additive.
ChemInform Abstract: Studies on the Palladium‐Catalyzed Direct Alkenylation of 1,2‐Azoles.
Authors: Chappell Ben , Dedman Nathan , Wheeler Simon
Published: September 2011

Electron‐rich heterocycles, such as isoxazoles (I), isothiazoles (IV) and pyrazoles (VI) undergo direct Pd‐catalyzed alkenylation in moderate yields.
ChemInform Abstract: Stereoselective Synthesis of Phenyl‐1,2,3‐triazoles Containing (E)‐Vinyl Halide Group via a One‐Pot, Three‐Component Reaction.
Authors: Zhang Wensheng , Su Changhui , Kuang Chunxiang , Yang Qing
Published: September 2011

Two examples are given, where NCS and NIS are used, resulting in the corresponding vinyl chloro and vinyl iodo derivatives, respectively.
ChemInform Abstract: Synthesis and Biological Evaluation of a Novel Human Stem/Progenitor Cells Proliferation Activator: 4‐(4‐(5‐Mercapto‐1,3,4‐oxadiazol‐2‐yl)phenyl)thiosemicarbazide (Stemazole).
Authors: Sun Ying , Wang Wei , Sun Yuanyuan , Han Mei
Published: September 2011

Stemazole (IXa) and its derivatives are prepared in four steps from methyl aminobenzoates (I) via construction of the oxadiazole ring as the key step.
ChemInform Abstract: L‐Proline as an Efficient Catalyst for the Multi‐Component Synthesis of 6‐Amino‐4‐alkyl/aryl‐3‐methyl‐2,4‐dihydropyrano [2,3‐c]pyrazole‐5‐carbonitriles in Water.
Authors: Mecadon Hormi , Rohman Md. Rumum , Kharbangar Iadeishisha , Laloo Badaker M. , Kharkongor Icydora , Rajbangshi Mantu , Myrboh Bekington
Published: September 2011

A four‐component synthesis of title compounds (IV) using L‐proline as a catalyst is established.
ChemInform Abstract: Ruthenium‐Catalyzed Oxidative Synthesis of 2‐Pyridones Through C—H/N—H Bond Functionalizations.
Authors: Ackermann Lutz , Lygin Alexander V. , Hofmann Nora
Published: September 2011

The reaction proceeds with complete regioselectivity when phenylalkylacetylenes (XIII) are applied.
ChemInform Abstract: Photochemical Intramolecular Cyclization of o‐Alkynylaryl Isocyanides with Organic Dichalcogenides Leading to 2,4‐Bischalcogenated Quinolines.
Authors: Mitamura Takenori , Iwata Kimiyo , Nomoto Akihiro , Ogawa Akiya
Published: September 2011

The method provides a new approach to 2,4‐bischalcogenated quinolines.
ChemInform Abstract: One‐Pot Synthesis of Imidazo[1,2‐a]pyridines from Benzyl Halides or Benzyl Tosylates, 2‐Aminopyridines and Isocyanides.
Authors: Adib Mehdi , Sheikhi Ehsan , Rezaei Narjes
Published: September 2011

Benzyl halides (I) or ‐tosylates (V) are oxidized to aldehydes under mild Kornblum conditions which then undergo a three‐component reaction with various 2‐aminopyridines (II) and isocyanides (III) to afford title compounds (IV)/ (VI) in high yields.
ChemInform Abstract: Fluoroazaindolines by an Uncommon Radical ipso‐Substitution of a C—F Bond.
Authors: Laot Yann , Petit Laurent , Tran Ngoc Diem My , Zard Samir Z.
Published: September 2011

Compound (V) is prepared similarly to compounds (IV).
ChemInform Abstract: Synthesis of Heterocycles Through a Ruthenium‐Catalyzed Tandem Ring‐Closing Metathesis/Isomerization/N‐Acyliminium Cyclization Sequence.
Authors: Ascic Erhad , Jensen Jakob F. , Nielsen Thomas E.
Published: September 2011

Double bonds created during ring‐closing metathesis isomerize to generate reactive iminium intermediates.
ChemInform Abstract: Synthesis and Coordination Chemistry of 4‐Azabenzimidazole Derivatives.
Authors: Jahnke Mareike C. , Brackemeyer Dirk , Pape Tania , Hahn F. Ekkehardt
Published: September 2011

A facile method for the synthesis of the title compounds (III) and (IV) is presented.
ChemInform Abstract: Improved Synthesis of Monoprotected 5‐ and 6‐Amino‐2‐azanorbornanes
Authors: Dacenko Oleksandr P. , Manoylenko Olga V. , Grygorenko Oleksandr O. , Mykhailiuk Pavel K. , Volochnyuk Dmitriy M. , Shishkin Oleg V. , Tolmachev Andrey A.
Published: September 2011

as conformationally rigid diamine scaffolds in the design of neurokinin receptor antagonists
ChemInform Abstract: Synthesis, Structure—Activity Relationship of Novel Substituted 4H‐Chromen‐1,2,3,4‐tetrahydropyrimidine‐5‐carboxylates as Potential Antimycobacterial and Anticancer Agents.
Authors: Raju B. China , Rao R. Nageswara , Suman P. , Yogeeswari P. , Sriram D. , Shaik Thokhir Basha , Kalivendi Shasi Vardhan
Published: September 2011

The synthesis of a series of novel tetrahydropyrimidine derivatives and their screening for in vitro antimycobacterial activity as well as their cytotoxicity against three human cancer cell lines are described.
ChemInform Abstract: Benzothieno[3,2‐e][1,2,4]triazolo[4,3‐c]pyrimidines: Synthesis, Characterization, Antimicrobial Activity, and Incorporation into Solid Lipid Nanoparticles.
Authors: Panchamukhi Shridhar I. , Mulla Jameel Ahmed S. , Shetty Nitinkumar S. , Khazi Mohammed Iqbal A. , Khan Ashraf Y. , Kalashetti Mallikarjun B. , Khazi Imitiyaz Ahmed M.
Published: September 2011

A variety of novel tetracyclic triazolothienopyrimidines (V) (8 examples) with promising antibacterial and antifungal activities is synthesized.
ChemInform Abstract: Selenium‐Catalyzed Reductive Cyclization and Carbocyclization of 2,2′‐Dinitrostilbenes with Carbon Monoxide: One‐Shot Synthesis of Indolo[1,2‐c]quinazolinones.
Authors: Umeda Rui , Morishita Shigeru , Nishiyama Yutaka
Published: September 2011

A practical and selective synthesis of the compounds (III) and (V) is developed.
ChemInform Abstract: Direct Synthesis of 6‐Azabicyclo[3.2.1]oct‐6‐en‐2‐ones and Pyrrolizidines from Divinyl Ketones and Observation of Remarkable Substituent Effects.
Authors: Xu Xianxiu , Li Yifei , Zhang Yu , Zhang Lingjuan , Pan Ling , Liu Qun
Published: September 2011

DBU‐catalyzed treatment of divinyl ketones with isocyanoacetate at 0 or 25 °C allows a new, mild, easy, and stereoselective access to azabicyclooctenones.
ChemInform Abstract: Addition of a Stable Dialkylsilylene to Carbon—Carbon Unsaturated Bonds.
Authors: Ishida Shintaro , Iwamoto Takeaki , Kira Mitsuo
Published: September 2011

The title reaction gives the isolable compounds (III), (V), (VII), (IX), and (XI).
ChemInform Abstract: A General Approach to Enantiomeric γ‐Aminophosphonic Acids Using Chiral Sulfinimine Methodology.
Authors: Lyzwa Piotr , Mikolajczyk Marian
Published: September 2011

The title methodology is used for the preparation of AP4 (IV) which acts as a modulator of the NMDA receptor site.
ChemInform Abstract: Amberlyst‐15‐Catalyzed Facile Synthesis of α‐Amino Phosphonates.
Authors: Sudhakar Dega , Siddaiah Vidavalur , Rao Chunduri Venkata
Published: September 2011

A facile method for the synthesis of the title compounds (III) under mild reaction conditions from N‐tosyl aldimines and phosphite (II) using Amberlyst 15 as heterogeneous catalyst is presented.
ChemInform Abstract: Synthesis and Structure Elucidation of Benzoylated Deoxyfluoropyranosides.
Authors: Esmurziev Aslan M. , Simic Nebojsa , Hoff Baard Helge , Sundby Eirik
Published: September 2011

The fluorination of several benzoylpyranosides using DAST and Deoxo‐Fluor is reported.
ChemInform Abstract: Regioselective NaBH4 and DIBAL‐H Reductions of 3,4‐Dimethoxyhomopiperonylphthalimide: Concise and Efficient Synthesis of Nuevamine and Isonuevamine.
Authors: Wakchaure Prasad B. , Kunte Sunita S. , Argade Narshinha P.
Published: September 2011

The ratio of the formation of nuevamine (IV) and isonuevamine (V) from (III) is strongly dependent on the reducing agent used.
ChemInform Abstract: Inhibition and Structural Reliability of Prenylated Flavones from the Stem Bark of Morus lhou on β‐Secretase (BACE‐1).
Authors: Cho Jung Keun , Ryu Young Bae , Curtis‐Long Marcus J. , Kim Ji Young , Kim Doman , Lee Sun , Lee Woo Song , Park Ki Hun
Published: September 2011

A variety of flavones (8 examples) is isolated by activity‐guided fractionation of the methanolic extracts from Morus Ihou stem bark.
ChemInform Abstract: Optical Spectroscopy of Charge Transfer Transitions in Multiferroic Manganites, Ferrites, and Related Insulators
Authors: Moskvin A. S. , Pisarev R. V.
Published: September 2011

Review: 108 refs.
ChemInform Abstract: Formation and Hydrolysis of Polynuclear Actinide Complexes
Authors: Walther C. , Buchner S. , Fuss M. , Geist A. , Icker M. , Lutzenkirchen J. , Rothe J. , Schimmelpfennig B. , Schwindt O. , Steppert M.
Published: September 2011

Review: 11 refs.
ChemInform Abstract: Asymmetric Benzoin and Stetter Reactions
Authors: DiRocco D. A. , Rovis T.
Published: September 2011

Review: 42 refs.
ChemInform Abstract: Mannich Reaction
Authors: Burns N. Z. , Jacobsen E. N.
Published: September 2011

Review: 79 refs.
ChemInform Abstract: Enzymic Direct Aldol Additions
Authors: Clapes P. , Fessner W.‐D.
Published: September 2011

Review: 184 refs.
ChemInform Abstract: Asymmetric Mukaiyama Aldol Reaction
Authors: Liu L. , Wang D. , Li C.‐J.
Published: September 2011

Review: 84 refs.
ChemInform Abstract: Enantioselective Addition of Metal Alkynylides to Imino Groups
Authors: Carreira E. M. , Aschwanden P.
Published: September 2011

Review: 17 refs.
ChemInform Abstract: Enantioselective Addition of Acetylide Nucleophiles to Carbonyl Compounds
Authors: Carreira E. M. , Frantz D. E.
Published: September 2011

Review: 57 refs.
ChemInform Abstract: Stereoselective Reduction of Imino Groups
Authors: Xu L. , Wu X. , Xiao J.
Published: September 2011

Review: 213 refs.
ChemInform Abstract: Enzymatic Reduction of Carbonyl Groups
Authors: de Wildeman S. , Sereinig N.
Published: September 2011

Review: 243 refs.
ChemInform Abstract: Synthetic Photochemistry of Naphthalimides and Related Compounds
Authors: Oelgemoeller Michael , Kramer Wolfgang H.
Published: September 2011

Review: 209 refs.
ChemInform Abstract: Synthetic Chemistry of Fullerenes
Authors: Deng Shun‐Liu , Tan Yuan‐Zhi , Xie Su‐Yuan
Published: September 2011

Review: 266 refs.
ChemInform Abstract: Furfural and Furfural‐Based Industrial Chemicals
Authors: Dias Ana S. , Lima Sergio , Pillinger Martyn , Valente Anabela A.
Published: September 2011

Review: 85 refs.
ChemInform Abstract: Oxetanes from the Ring Contraction of α‐Triflates of γ‐Lactones: Oxetane Nucleosides and Oxetane Amino Acids
Authors: Jenkinson Sarah F. , Fleet George W. J.
Published: September 2011

Review: 54 refs.
ChemInform Abstract: Glycosidases in Carbohydrate Synthesis: When Organic Chemistry Falls Short
Authors: Bojarova Pavla , Kren Vladimir
Published: September 2011

Review: 104 refs.
ChemInform Abstract: Transition Metals in Organic Synthesis. Part 93. Total Synthesis of Biologically Active Alkaloids Using Transition Metals
Authors: Forke Ronny , Gruner Konstanze K. , Knott Kerstin E. , Auschill Stefan , Agarwal Sameer , Martin Rene , Boehl Markus , Richter Sabine , Tsiavaliaris Georgios , Fedorov Roman , et al. et al.
Published: September 2011

Review: 92 refs.
ChemInform Abstract: Recent Advances and Potential Pharmacological Activities of Benzimidazole Derivatives
Authors: Srikanth L. , Raj V. Varun , Raghunandan N. , Venkateshwerlu L.
Published: September 2011

Review: 30 refs.
ChemInform Abstract: Benzothiazole: Different Methods of Synthesis and Diverse Biological Activities
Authors: Yadav P. S. , Devprakash Devprakash , Senthilkumar G. P.
Published: September 2011

Review: 29 refs.
ChemInform Abstract: Stable Singlet Carbenes as Mimics for Transition Metal Centers
Authors: Martin David , Soleilhavoup Michele , Bertrand Guy
Published: September 2011

Review: 165 refs.
ChemInform Abstract: 2‐Iodoxybenzenesulfonic Acid (IBS) Catalyzed Oxidation of Alcohols
Authors: Uyanik Muhammet , Ishihara Kazuaki
Published: September 2011

Review: 64 refs.
ChemInform Abstract: Squaramides: Physical Properties, Synthesis and Applications
Authors: Storer R. Ian , Aciro Caroline , Jones Lyn H.
Published: September 2011

Review: 70 refs.
ChemInform Abstract: Transition‐Metal‐Catalyzed C—C Bond Formation Through the Fixation of Carbon Dioxide
Authors: Huang Kun , Sun Chang‐Liang , Shi Zhang‐Jie
Published: September 2011

Review: 124 refs.
ChemInform Abstract: The Molecular Level Modification of Surfaces: From Self‐Assembled Monolayers to Complex Molecular Assemblies
Authors: Gooding J. Justin , Ciampi Simone
Published: September 2011

Review: 169 refs.
ChemInform Abstract: Syntheses and Transformations of α‐Azido Ketones and Related Derivatives
Authors: Patonay Tamas , Konya Krisztina , Juhasz‐Toth Eva
Published: September 2011

Review: 273 refs.
ChemInform Abstract: The Synthesis and Application of Polyamino Polycarboxylic Bifunctional Chelating Agents
Authors: Lattuada Luciano , Barge Alessandro , Cravotto Giancarlo , Giovenzana Giovanni Battista , Tei Lorenzo
Published: September 2011

Review: 334 refs.
ChemInform Abstract: Recognition of Amino Acids by Functionalized Calixarenes
Authors: Mutihac Lucia , Lee Jae Hong , Kim Jong Seung , Vicens Jacques
Published: September 2011

Review: 123 refs.
ChemInform Abstract: Synthetic Foldamers
Authors: Guichard Gilles , Huc Ivan
Published: September 2011

Review: 68 refs.
ChemInform Abstract: Role of Solvents in Coordination Supramolecular Systems
Authors: Li Cheng‐Peng , Du Miao
Published: September 2011

Review: 98 refs.
ChemInform Abstract: Profluorescent Nitroxides as Sensitive Probes of Oxidative Change and Free Radical Reactions
Authors: Blinco James P. , Fairfull‐Smith Kathryn E. , Morrow Benjamin J. , Bottle Steven E.
Published: September 2011

Review: 126 refs.
ChemInform Abstract: Design Strategies for Bivalent Ligands Targeting GPCRS
Authors: Shonberg Jeremy , Scammells Peter J. , Capuano Ben
Published: September 2011

Review: 92 refs.
ChemInform Abstract: Ionic Liquids as Active Pharmaceutical Ingredients
Authors: Ferraz Ricardo , Branco Luis C. , Prudencio Cristina , Noronha Joao Paulo , Petrovski Zeljko
Published: September 2011

Review: about 70 refs.
ChemInform Abstract: Studies on Hypervalent Compounds and Synthetic Work Using Heteroaromatic Cations
Authors: Akiba Kin‐ya
Published: September 2011

Review: phosphoranes, sulfuranes, antimony (III), bismuth (III), organotellurium compounds; 306 refs.
ChemInform Abstract: Development of Novel Synthetic Organic Reaction Based on Activation by a Trivalent Indium Salt
Authors: Sakai Norio , Konakahara Takeo
Published: September 2011

Review: ca. 50 refs.
ChemInform Abstract: Transition‐Metal‐Mediated Fluorination of Arenes
Authors: Furuya Takeru , Ritter Tobias
Published: September 2011

Review: about 60 refs.
ChemInform Abstract: Structure and Properties of Functional Oxide Thin Films: Insights from Electronic‐Structure Calculations
Authors: Rondinelli James M. , Spaldin Nicola A.
Published: September 2011

Review: 187 refs.
Comparison of Electrocardiographic Findings Between the Midventricular Ballooning Form and Apical Ballooning Form of Takotsubo Cardiomyopathy
Authors: Kurisu Satoshi , Kato Yasuko , Mitsuba Naoya , Ishibashi Ken , Dohi Yoshihiro , Nishioka Kenji , Kihara Yasuki
Published: September 2011

Background:

Several reports have recently described the variant form of takotsubo cardiomyopathy exhibiting midventricular ballooning. The purpose of this study was to assess electrocardiographic (ECG) findings on admission in patients with midventricular ballooning.

Hypothesis:

ECG findings are different between the midventricular ballooning form and apical ballooning form of takotsubo cardiomyopathy.

Methods:

We reviewed ECGs on admission in 6 patients with midventricular ballooning and 20 patients with apical ballooning. The sum of ST segment elevation in leads V1 to V3 or in leads V4 to V6 was obtained. The number of leads showing ST segment elevation and/or T wave inversion was also obtained. These ECG findings were compared between the 2 groups.

Results:

In midventricular ballooning, ECG changes including ST segment elevation and/or T wave inversion were observed frequently in leads V2 and V3, and were not observed in leads II, III, −aVR, aVF, V5, and V6. On the other hand, in apical ballooning, they were found in all leads. They were most common in leads V4 and V5. The sum of ST segment elevation in leads V1 to V3 was similar (2.6 ± 2.0 mm vs 2.7 ± 2.0 mm, P = not significant), and the sum of ST segment elevation in leads V4 to V6 was significantly lower in midventricular ballooning than apical ballooning (0.4 ± 0.8 mm vs 3.5 ± 3.0 mm, P<0.05). The number of leads showing ST segment elevation and/or T wave inversion was significantly lower in midventricular ballooning than apical ballooning (3.2 ± 1.0 leads vs 6.3 ± 2.2 leads, P<0.01).

Conclusions:

Our data suggested that midventricular ballooning may show limited ECG changes despite broad wall motion abnormality. © 2011 Wiley Periodicals, Inc.

The authors have no funding, financial relationships, or conflicts of interest to disclose.
What Do the 2011 American Heart Association Guidelines Tell Us About Prevention of Cardiovascular Disease in Women?
Authors: Wenger Nanette K.
Published: September 2011

The 2011 Update of the American Heart Association's Cardiovascular Disease Prevention Guideline for Women is designed to help women and their physicians understand cardiovascular Disease (CVD) risks and undertake practical steps that are most effective in preventing heart disease and stroke. Defining a woman's risk status and improving her adherence to preventive lifestyle behaviors and medications is the best strategy to lower the burden of CVD in women. © 2011 Wiley Periodicals, Inc.

The author has no funding or financial relationships of interest to disclose. Author is also author of the Guideline.
Synthesis and Anti‐HIV Activity of Aryl‐2‐[(4‐cyanophenyl)amino]‐4‐pyrimidinone hydrazones as Potent Non‐nucleoside Reverse Transcriptase Inhibitors
Authors: Ma Xiao‐Dong , Yang Shi‐Qiong , Gu Shuang‐Xi , He Qiu‐Qin , Chen Fen‐Er , De Clercq Erik , Balzarini Jan , Pannecouque Christophe
Published: September 2011

A series of novel diarylpyrimidines (DAPYs) with a ketone hydrazone substituent on the methylene linker between the pyrimidine nucleus and the aryl moiety at the C‐4 position were synthesized, and their antiviral activity against human immunodeficiency virus (HIV)‐1 in MT‐4 cells was evaluated. Most compounds of this class exhibited excellent activity against wild‐type HIV‐1, with EC50 values in the range of 1.7–13.2 nM. Of these compounds, 2‐bromophenyl‐2‐[(4‐cyanophenyl)amino]‐4‐pyrimidinone hydrazone (9 k) displayed the most potent anti‐HIV‐1 activity (EC50=1.7±0.6 nM), with excellent selectivity for infected over uninfected cells (SI=5762). In addition, the 4‐methyl phenyl analogue 9 d (EC50=2.4±0.2 nM, SI=18461) showed broad spectrum HIV inhibitory activity, with EC50 values of 2.4±0.2 nM against wild‐type HIV‐1, 5.3±0.4 μM against HIV‐1 double‐mutated strain RES056 (K103N+Y181C), and 5.5 μM against HIV‐2 ROD strain. Furthermore, structure–activity relationship (SAR) data and molecular modeling results for these compounds are also discussed.
Cell labeling approaches for fluorescence‐based in vivo flow cytometry
Authors: Pitsillides Costas M. , Runnels Judith M. , Spencer Joel A. , Zhi Liang , Wu Mei X. , Lin Charles P.
Published: September 2011

We provide an overview of the methods used to label circulating cells for fluorescence detection by in vivo flow cytometry. These methods are useful for cell tracking in small animals without the need to draw blood samples and are particularly useful for the detection of circulating cancer cells and quantification of circulating immune cells. © 2011 International Society for Advancement of Cytometry.
A high‐resolution molecular atlas of the fetal mouse lower urogenital tract
Authors: Abler Lisa L. , Keil Kimberly P. , Mehta Vatsal , Joshi Pinak S. , Schmitz Christopher T. , Vezina Chad M.
Published: September 2011

Epithelial‐stromal interactions in the lower urogenital tract (LUT) are integral to prostatic and seminal vesicle development in males, vaginal and uterine development in females, and urethral development in both sexes. Gene expression profiling of isolated LUT stroma and epithelium has unraveled mechanisms of LUT development, but such studies are confounded by heterogeneous and ill‐defined cell sub‐populations contained within each tissue compartment. We used in situ hybridization to synthesize a high‐resolution molecular atlas of 17‐day post‐coitus fetal mouse LUT. We identified mRNAs that mark selective cell populations of the seminal vesicle, ejaculatory duct, prostate, urethra, and vagina, subdividing these tissues into 16 stromal and 8 epithelial sub‐compartments. These results provide a powerful tool for mapping LUT gene expression patterns and also reveal previously uncharacterized sub‐compartments that may play mechanistic roles in LUT development of which we were previously unaware. Developmental Dynamics 240:2364–2377, 2011. © 2011 Wiley‐Liss, Inc.
Summary of ‘Combined oral contraceptive pills for treatment of acne’
Authors: Editorial Office Evidence‐Based Child Health
Published: September 2011

This is a summary of Cochrane review, published in this issue of EBCH, first published as: Arowojolu AO, Gallo MF, Lopez LM, Grimes DA, Garner SE. Combined oral contraceptive pills for treatment of acne. Cochrane Database of Systematic Reviews 2009, Issue 3. Art. No.: CD004425. DOI: 10.1002/14651858.CD004425.pub4.acne Copyright © 2011 The Cochrane Collaboration. Published by John Wiley & Sons, Ltd. The Cochrane Collaboration
Variation in MHC genotypes in two populations of house sparrow (Passer domesticus) with different population histories
Authors: Borg Åsa Alexandra , Pedersen Sindre Andre , Jensen Henrik , Westerdahl Helena
Published: September 2011

Small populations are likely to have a low genetic ability for disease resistance due to loss of genetic variation through inbreeding and genetic drift. In vertebrates, the highest genetic diversity of the immune system is located at genes within the major histocompatibility complex (MHC). Interestingly, parasite‐mediated selection is thought to potentially maintain variation at MHC loci even in populations that are monomorphic at other loci. Therefore, general loss of genetic variation in the genome may not necessarily be associated with low variation at MHC loci. We evaluated inter‐ and intrapopulation variation in MHC genotypes between an inbred (Aldra) and a relatively outbred population (Hestmannøy) of house sparrows (Passer domesticus) in a metapopulation at Helgeland, Norway. Genomic (gDNA) and transcribed (cDNA) alleles of functional MHC class I and IIB loci, along with neutral noncoding microsatellite markers, were analyzed to obtain relevant estimates of genetic variation. We found lower allelic richness in microsatellites in the inbred population, but high genetic variation in MHC class I and IIB loci in both populations. This suggests that also the inbred population could be under balancing selection to maintain genetic variation for pathogen resistance.
Development and validation of a capillary electrophoresis assay for the determination of the stereoisomeric purity of chloroquine enantiomers
Authors: Wongwan Sudaporn , Scriba Gerhard K. E.
Published: September 2011

A stereoselective CE assay for the determination of the enantiomeric purity of (R)‐(−)‐chloroquine and (S)‐(+)‐chloroquine was developed and validated. The separations were performed in a 50.2/40 cm uncoated fused silica capillary at 20°C using a 100 mM sodium phosphate buffer, pH 2.5, containing 30 mg/mL sulfobutylether(VII)‐β‐cyclodextrin as background electrolyte operated at an applied voltage of –25 kV and 20°C. The detection wavelength was 225 nm. Carbamazepine was used as internal standard. The assay was validated in the range of 0.05–1.0% for the respective minor chloroquine enantiomer based on a concentration of 3 mg/mL of the major enantiomer, either (R)‐(−)‐chloroquine or (S)‐(+)‐chloroquine. The method was applied to analyze the stereoisomeric purity of synthetic samples of the chloroquine enantiomers.
Capillary electrophoresis and hollow fiber liquid‐phase microextraction for the enantioselective determination of albendazole sulfoxide after biotransformation of albendazole by an endophytic fungus
Authors: Carrão Daniel B. , Borges Keyller B. , Barth Thiago , Pupo Mônica T. , Bonato Pierina S. , de Oliveira Anderson R. Moraes
Published: September 2011

Hollow fiber liquid‐phase microextraction and CE were applied for the determination of albendazole sulfoxide (ASOX) enantiomers in liquid culture medium after a fungal biotransformation study. The analytes were extracted from 1 mL of liquid culture medium spiked with the internal standard (rac‐hydroxychloroquine) and buffered with 0.50 mol/L phosphate buffer, pH 10. The analytes were extracted into 1‐octanol impregnated in the pores of the hollow fiber, and into an acid acceptor solution inside the polypropylene hollow fiber. The electrophoretic separations were carried out in 0.05 mol/L tris(hydroxymethyl)aminomethane buffer, pH 9.3, containing 3.0% w/v sulfated‐β‐CD (S‐β‐CD) with a constant voltage of +15 kV and detection at 220 nm. The method was linear over the concentration range of 250–5000 ng/mL for each ASOX enantiomer. Within‐day and between‐day assay precision and accuracy for the analytes were studied at three concentration levels and the values of RSD% and relative error % were lower than 15%. The developed method was applied for the determination of ASOX after a biotransformation study employing the endophytic fungus Penicillium crustosum (VR4). This study showed that the endophytic fungus was able to metabolize the albendazole to ASOX enantioselectively. In addition, it was demonstrated that hollow fiber liquid‐phase microextraction coupled to CE can be an excellent and environmentally friendly technique for the analysis of samples obtained in biotransformation studies.