bluuebunny/crossref_metadata_2025 huggingface dataset:
Role of the interface in the melt‐rheology properties of linear low‐density polyethylene/low‐density polyethylene blends: Effect of the molecular architecture of the dispersed phase
Authors: Robledo N. , Vega J. F. , Nieto J. , Martínez‐Salazar J.
Published: September 2010

We studied the melt linear viscoelastic and elongational properties of blends consisting of a Ziegler–Natta linear low‐density polyethylene (LLDPE) and different LDPEs. The weight fraction of the LDPE used in the blends was 15%. The linear viscoelastic characterization was performed at different temperatures for all of the blends to determine the thermorheological behavior in the melt state. The blends fulfilled the time–temperature superposition but exhibited a broad linear viscoelastic response, which was further than that expected for miscible blends and even immiscible systems with a sharp interface. A rheological study of the application of the Palierne model revealed that in addition to the droplet shape relaxation, another mechanism was present at lower frequencies. We discuss the results by hypothesizing a strong interaction between the high‐molecular‐weight linear fraction of the LLDPE matrix and a fraction of molecules of the dispersed phase, which formed a thick interface with its own viscoelastic properties. A clear change in this additional mechanism was observed, depending on the dispersed minor‐phase properties, which produced an impact on the processing of the blends, and more precisely, on the values of the melt strength in the melt‐spinning experiments. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011
Synthesis and thermal behavior of poly(methyl methacrylate)/Maghnia bentonite nanocomposite prepared at room temperature via in situ polymerization initiated by a new Ni(II)α‐benzoinoxime complex
Authors: Ouaad Kamel , Djadoun Saïd , Ferfera‐Harrar Hafida , Sbirrazzuoli Nicolas , Vincent Luc
Published: September 2010

Poly(methyl methacrylate) (PMMA) and poly(methyl methacrylate)/clay nanocomposite (PMMA/OBT) were successfully prepared in dioxan at room temperature via in situ radical polymerization initiated by a new Ni(II)α‐ Benzoinoxime complex as a single component in presence of 3% by weight of an organically modified bentonite (OBT) (originated from Maghnia, Algeria) and characterized by FTIR, 1H‐NMR and viscometry. Mainly intercalated and partially exfoliated PMMA/OBT nanocomposite was elaborated and evidenced by X‐Ray diffraction (XRD) and transmission electron microscopy (TEM). The intrinsic viscosity of PMMA/OBT nanocomposite is much higher than the one of pure PMMA prepared under the same conditions. Differential scanning calorimetry (DSC) displayed an increase of 10°C in the glass transition temperature of the elaborated PMMA/OBT nanocomposite relative to the one of pure PMMA. Moreover, the TGA analysis confirms a significant improvement of the thermal stability of PMMA/OBT nanocomposite compared to virgin PMMA: the onset degradation temperature of the nanocomposite, carried out under nitrogen atmosphere, increased by more than 45°C. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011
Statistical evaluation of non‐profile analyses for the in vitro bioequivalence
Authors: Chiu Shih‐Ting , Tsai Pei‐Ying , Liu Jen‐pei
Published: September 2010

For locally acting drug products such as nasal aerosols and nasal sprays, the 2003 US Food and Drug Administration (FDA) draft guidance suggests that bioequivalence between generic and brand‐name products be established through in vitro tests. In addition, for non‐profile analyses based on spray content uniformity, droplet size distribution, spray pattern, priming, and re‐priming, the draft US FDA guidance recommends that the population bioequivalence (PBE) between generic and innovator's products be demonstrated. However, the linearized criterion recommended in the draft FDA guidance does not take into consideration the variations due to batches, samples, and life stages. Hence, under a two‐stage nested random effects model, we apply the methods of modified large‐sample (MLS) and generalized pivotal quantities (GPQs) to construct the upper 95% confidence limit for in vitro PBE criterion with consideration of variance components as the statistical testing procedures for establishing the in vitro BE. A simulation study was conducted to compare empirical size and empirical power among the three methods. A numerical example illustrates the proposed methods. Copyright © 2010 John Wiley & Sons, Ltd.
Comparison of PARAFAC and PARALIND in modeling three‐way fluorescence data array with special linear dependences in three modes: a case study in 2‐naphthol
Authors: Chen Hao , Zheng Binghui , Song Yonghui
Published: September 2010

Owing to excited‐state proton transfer in 2‐naphthol solutions, the fluorescence excitation–emission matrices (EEMs) have factors that are highly dependent in three modes. For the first time such EEMs are used to compare the capability of PARALIND (PARAFAC with linear dependence) and conventional PARAFAC in modeling three‐way EEMs having linearly dependent factors in three modes. Two primary conclusions have been drawn. First, the results indicate that a 3‐factor PARAFAC model fit the data better than two PARALIND models (type 1 and 2) in this case while equally well with a specially PARALIND model (type 3); second, a negative core consistency (CC) in the 3‐factor PARAFAC model is reported but the type 3 PARALIND model reports a nearly 100 CC. This work has demonstrated that a properly constrained PARALIND can fit the very special EEMs of 2‐naphthol. The presence of negative CC associated with a perfect PARAFAC model would imply the presence of very special linear dependences in EEMs, which would be used as an “alarm” for the investigators to interpret the data more carefully when dealing with complicated environmental EEMs in the absence of a priori knowledge. Copyright © 2010 John Wiley & Sons, Ltd.
Investigation in monolayers of double‐chain fluorocarbon amphiphiles Effect of headgroups on molecular packing and interaction between hydrocarbon and fluorocarbon monolayers
Authors: Liang Kang‐Ning , Hui Yong‐Zheng
Published: September 2010

The surface pressure‐area diagrams of double‐chain fluorocarbon amphiphiles with different headgroup compositions show that the amphiphiles arrange almost perpendicularly to the water subphase and the structure of headgroups exerts significant influence on the amphiphile packing. Strong hydrogen bonding and weak electrostatic interaction favor the formation of stable monolayers. Perfluorooctanoic acid (FOA) cannot form monolayer at water/air interface and can only form liquid monolayer in subphase of calcium nitrate solution. Complete phase separation of palmitic acid and a fluorocarbon amphiphile with shorter hydrocarbon spacer group, 1, could be demonstrated in monolayers by using the phase rule of Crisp. The creation of phase‐separated monolayers is possible when the monolayer is composed of a mixture of palmitic acid and a fluorocarbon amphiphile with longer hydrocarbon spacer group, 2. It can be suggested that the miscibility of hydrocarbon amphiphiles with fluorocarbon amphiphiles is determined by the hydrocarbon fraction of fluorocarbon amphiphiles.
The structure and hydrogen bond of tert‐butoxycarbonyl‐D, L‐isoleucyl‐glycyl methyl ester
Authors: Yang Qing‐Chuan , Dai Sheng , Tang You‐Qi
Published: September 2010

The crystal structure of tert‐butoxycarbonyl‐D, L‐isoleucyl‐glycyl methyl ester was determined by the X‐ray method. The space group is P21 with a = 9.115(3), b= 12.075(4), c = 16.258(5) Å, β = 89.84(3) and Z = 4. It was observed that in the peptides which contain IleGly fragment the carbonyl group of Gly residue has less tendency to form hydrogen bond than that of Ile residue. This tendency was supported by the atomic net charges calculated with the quantum mechanics program CNDO/2.
Preparation of new mixed ligand complexes of lanthanide acetylacetonate with dibenzo‐18‐crown‐6 and their IR spectra
Authors: Yao Ke‐Min , Wang Xiao‐Ling
Published: September 2010

Fourteen new mixed ligand complexes of lanthanide acetylacetonate and dibenzo‐18‐ crown‐6 (DB18C6) were prepared by three different methods. The composition of the complexes was shown to be Ln(acac)· DB18C6 by elemental analysis and X‐ray powder diffraction. Infrared spectra of the complexes were investigated, and the results indicate that their absorption bands in the region of 400—4000 cm−1are complicated and without much difference from each other, but in the far infrared region various absorption bands of Ln—O can be observed and they changes regularly with the atomic number of lanthanides.
The synthesis and crystal structure of a trinuclear molybdenum cluster compound [Mo3(μ‐O)(μ‐S)3(μ(μ‐OAc)2(dtp)2·(Py)]·0.5H2O
Authors: Lu Shao‐Fang , Huang Jian‐Quan , Huang Zi‐Xiang , Zhang Bin , Huang Jin‐Ling
Published: September 2010

[Mo3,OS3(dtp)4(H2O)] reacts with NaOAc·3H2O in Py to give the title compound. The crystal data are as follows: [Mo2OS3)(OAc)2(dtp)2·Py]−0.5H,O(dtp = [S3P(OC2H5)2]−, Py = C5H5N); M = 976.64; triclinic; space group P1; a=11.704(5), b=14.169(7), c= 11.688 (5) Å α=109.94(4) β = 91.53(4), γ = 91.93(4)°; V= 1819(1) Å2; Z=2; Dc = 1.78 g·cm−3 λ(Mo Kα) = 0.71069 Å μ=15.15 cm−1; F(000) = 970 T=296 K; final R=0.071 for 1652 reflections with I>3σ(I). In the molecule, the [Mo3OS3] core is surrounded by two bridging OAc groups and two terminal chelate dtp groups attached to the {Mo3} triangle in a symmetric style, and the Py ligand is coordinated to the Mo atom at the apex of {Mo3} triangle with the nitrogen. This novel configuration is obtained for the first time with Mo—N bond length being 2.27 (2) Å and three Mo—Mo bond lengths 2.584 (4), 2.587 (4) and 2.657(4) Å, respectively. As a whole, the molecule has a virtual C2 symmetry.
Retention behavior of high performance ion chromatography using binary eluants
Authors: Su Tian‐Sheng , Yan Ji‐Min
Published: September 2010

The retention behavior of high performance ion chromatography using binary eluants is given. The relationship between log(tR) and log(1/[E]) is linear, which has been demonstrated experimentally with mixed anion solution.
The reaction of perfluoroalkanesulfonyl halides IX. The syntheses of bisperfluoroalkyl butadienes and perfluoroalkylated dienoates
Authors: Huang Wei‐Yuan , Zhang Han‐Zhong
Published: September 2010

The title compounds were prepared in good yield through the reaction of perfluoroalkyl butadiene and 2,4‐dienoates with perfluoroalkanesulfonyl bromide in the presence of benzoyl peroxide followed by HBr elimination.
The spin delocalization substituent parameter σ˙. 7. Meta‐substituent effects on the cyclodimerization of trifluorostyrenes. A test for the σ˙JJ approach
Authors: Jiang Xi‐Kui , Ji Guo‐Zhen , Zhang Xiu‐Lian , Guo Hong‐Xun
Published: September 2010

Rate constants (k's) of the thermal cyclodimerization of ten meta‐substituted trifluorostyrenes (m‐Y‐TFS's) have been measured in the temperature range 110–160°C. On the basis of these k's and the σmb values derived from 19F NMR data the spin‐delocalization substituent constant σ˙m values of these ten meta‐substituents have been calculated. The averaged σ˙m values are: m‐Et, 0.09; m‐t‐Bu, 0.11; m‐F, 0.03; m‐Cl,−0.05; m‐Br, 0.12: m‐CF3, −0.07; m‐OMe, 0.10; m‐NO2, −0.002; m‐CN, 0.11 and m‐CO2Me, 0.08. Both the smallness of these values and the nonexistence of correlation between Hammett‐Type polar σX and these σ˙m values support our belief that the σj̇J approach is reliable and trustworthy.
Cyclization of 2,6‐dialkoxy acetophenone hydrazones in the presence of polyphosphoric acid (PPA)
Authors: Qiu Yu‐Zhu , Zhang Zheng , Zhong Zhen‐Qi , Hu Hong‐Wen
Published: September 2010

Cyclization of a series of 2,6‐dialkoxy acetophenone hydrazones gave 3‐methyl‐4‐alkoxyindazoles with elimination of the 2‐ or 6‐alkoxy group in the presence of PPA. The reaction mechanism was discussed.
Studies on the synthesis of amino acids XIII. Dibenzylation of 2‐phenyl‐2‐oxazolin‐5‐one
Authors: Du Zheng‐Ming , Chen Ji‐Jun , Shi Yao‐Zeng , Hu Hong‐Wen
Published: September 2010

4,4‐Dibenzyl‐2‐phenyl‐2‐oxazollin‐5‐ones are prepared by one step reaction of 2‐phenyl‐2‐oxazolin‐5‐one with magnesium methyl carbonate (MMC) and benzylhalides. It is a novel and convenient method for the synthesis of α,α‐disubstituted α‐amino acids by hydrolysis of 4,4‐dibenzyl‐2‐phenyl‐2‐oxazolin‐5‐ones.
Combined Wavelet Transform with Curve‐fitting for Objective Optimization of the Parameters in Fourier Self‐deconvolution
Authors: Zhang Xiu‐Qi , Zheng Jian‐Bin , Gao Hong
Published: September 2010

Fourier self‐deconvolution was the most effective technique in resolving overlapping bands, in which deconvolution function results in deconvolution and apodization smoothes the magnified noise. Yet, the choice of the original half‐width of each component and breaking point for truncation is often very subjective. In this paper, the method of combined wavelet transform with curve fitting was described with the advantages of an enhancement of signal to noise ratio as well as the improved fitting condition, and was applied to objective optimization of the original half‐widths of components in unresolved bands for Fourier self‐deconvolution. Again, a noise was separated from a noisy signal by wavelet transform, therefore, the breaking point of apodization function can be determined directly in frequency domain. Accordingly, some artifacts in Fourier self‐deconvolution were minimized significantly.
Studies on the Physical Adsorption Equilibria of Gases on Porous Solids over a Wide Temperature Range Spanning the Critical Region—Adsorption on Microporous Activated Carbon
Authors: Zhou Ya‐Ping , Bai Shu‐Pei , Zhou Li , Yang Bin
Published: September 2010

Adsorption equilibria of nitrogen and methane on microporous ( < 2 nm) activated carbon were measured for a wide temperature range (103‐298 K) spanning the critical region. Information relating to Henry constants, the isosteric heat of adsorption, and the amount of limiting adsorption were evaluated. All isotherms show type‐I features for both sub‐ and supercritical temperatures. A new isotherm equation and a consideration for the importance of the effect of the adsorbed phase volume allow this kind of isotherms to be modeled satisfactorily. The model parameter of the saturated amount of absolute adsorption (n0t) equals the limiting adsorption amount (nitm), leaving the physical meaning of the latter clarified, and the exponent parameter (q) proves to be an appropriate index of surface heterogeneity.
Synthesis of Diazacrown Ethers with Chromophores and Their Photoinduced Charge‐Separation with Methyl Viologen
Authors: Li Jiu‐Yan , Zhang Li‐Ping , Wu Li‐Zhu , Wang Bo‐Jie , Tung Chen‐Ho
Published: September 2010

Two 4,13‐diaza‐18‐crown‐6 ethers with either two pyrenyl or two carbazolyl groups were synthesized. The two crown ethers can form complexes with methyl viologen in methanol solution. Photoirradiation of the complexes resulted in the electron transfer from the excited states of the chromophores to methyl viologen as demonstrated by the quenching of the chromophore fluorescence and the detection of the absorption spectrum of the generated viologen radical cation. The back electron transfer in these systems was inhibited by the electrostatic repulsion between the positively charged viologen radical cation and the generated chromophore radical cation. Long‐lived charge separation states (up to tens of min) were observed.
Triphenylamine Derivatives Containing Nitronyl Nitroxide and Iminyl Nitroxide‐Syntheses, Characterization, Crystal Structures and Magnetic Studies
Authors: Zhang De‐Qing , Wang Zhe‐Ming , Ding Liang , Zhang Bin , Xu Wei , Zhu Dao‐Ben , Yan Chun‐Hua
Published: September 2010

New triphenylamine derivatives 1, 2, 3, and 4 were synthesized and characterized by IR, FAB‐MS, EPR and EA. All of them displayed similar absorption and fluorescence spectra except compound 1, for which a possible explanation was proposed. Quasi‐reversible oxidation waves at about 0.76 V (vs. SCE) and 1.1 V for nitronyl nitroxide and iminyl nitroxide respectively as well as irreversible one at about 1.5 V for triphenylamine group were detected with cyclic voltammetry for compounds 1, 2, 3 and 4. Crystal structures of 2 and 4 were determined by X‐ray diffraction analysis. Their crystal data are as follows: for 2: monoclinic, C2/c, a = 1.69914 (4), b = 1.37435(5), c = 1.24621(5) ran, β= 106.553(2)°, V = 2.7896(2) nm3 Z = 4; for 4: orthorhombic, Pbca, a = 1.95970(6), b = 1.33096(4), c = 4.84691(14) nm, V = 12.6421(7) nm3, Z = 8. Magnetic studies indicated that all of them showed antiferromagnetic properties in solid state, but with strong intermolecular spin‐spin coupling as indicated by the relatively large values of 6, in particular for 4 (θ = −12 K). Possible spin‐spin interaction mechanism was suggested based on the crystal structures of 2 and 4.
Conductivity of I2‐Doped Hightrans‐1,4‐Polybutadiene
Authors: Shi Chen‐Jun , Xue Huai‐Guo , Shen Zhi‐Quan , Zhang Yi‐Feng , Li Yong‐Fang , Yang Chun‐He
Published: September 2010

Hightrans‐l,4‐polybutadiene ( −96% (trans)) was prepared by lanthanum naphthenate catalytic system. The conductivity of obtained polybutadiene doped with iodine reaches about −100 s/cm, which is 2 orders of magnitude higher than the value reported.4,5During the I2‐doping, the conjugated sequence was formed through double bond shifting reaction. According to the relationship between conductivity and temperature, conducting mechanism of doped hightrans‐l,4‐polybutadiene is fit on variable range hoping (VRH) model.
A Novel Greenish Blue‐emitting Amorphous Molecular Material: 2,5‐Bis {4‐[2‐naphthyl (phenyl) amino ] phenyl} thiophene
Authors: Liu Ping , Tong Zhen
Published: September 2010

A novel greenish blue‐emitting amorphous molecular material, 2,5‐bis{4‐[2‐naphthyl(phenyl)amino]phenyl thiophene (BN‐pA‐1T), was designed and synthesized. Its molecular properties, glass‐forming property, and application to an organic EL device were investigated.
Production of Carbon Nanotubes over Pre‐reduced LaCoO3 by Using Fluidized‐bed Catalytic Reactor
Authors: Liu Bao‐Chun , Tang Shui‐Hua , Liang Qi , Gao Li‐Zhen , Zhang Bo‐Lan , Qu Mei‐Zhen , Yu Zuo‐Long
Published: September 2010

A technique has been developed to grow carbon nanotubes by flowing acetylene over pre‐reduced LaCoO3 catalyst in a fluidized‐bed catalytic reactor. Carbon nanotubes were characterized by means of SEM and TEM. The pre‐reduced LaCoO3 catalyst was found to be effective in producing carbon nanotubes with even diameter. The effects of reduction temperature of LaCoO3 on the growth of carbon nanotubes were investigated. This process can easily be scaled up.
Synthesis and Antibacterial Activity of 3‐(5‐Methylisoxazol‐3‐yl) −1,2,4‐triazolo [3,4‐b]‐1,3,4‐thiadiazine Derivatives
Authors: Hui Xin‐Ping , Xu Peng‐Fei , Wang Qin , Zhang Qi , Zhang Zi‐Yi
Published: September 2010

The condensed products 2‐10 of 4‐amino‐5‐mercapto‐3‐(5‐methylisoxazol‐3‐yl)‐l,2,4‐triazole (1) with chloroacetaldehyde, 2‐bromocyclohexanone, chloranil, ωbromo‐ω‐(1H‐1, 2,4‐triazol‐l‐yl)acetophenone, 2‐bromo‐4′‐substituted acetophenones and 2‐bromo‐6′‐methoxy‐2′‐acetonaphthone were described. The antibacterial activities were also evaluated.
2D Hydrogen Bonded Copper (II) Coordination Network Constructed by the Combination of Flexible and Rigid Ligands
Authors: Xie Yong‐Shu , Liu Qing‐Liang , Du Chen‐Xia , Jiang Hui , Xu Xiao‐Long , Zhu Yu , Xue Yi
Published: September 2010

Complex [Cu(2,2′‐bipy)(H2L1)] (ClO4)2(1) has been synthesized by the self‐assembly of Cu(ClO4)2 with a rigid ligand 2,2′‐bipyridine and a flexible potential tetradentate ligand N, N'‐bis(hydroxyethyl)ethylenediamine (H2L1). Crystal analyses reveal that the potentially tetradentate ligand H2L1 acts in a tridentate mode by the coordination of one hydroxyl oxygen atom and two amino nitrogen atoms. The Cu(II) atom coordinates additionally with two bipyridyl nitrogen atoms, giving a distorted square pyramidal geometry. Each complex molecule is connected with four surrounding molecules along the ac plane by multiple hydrogen bonds, leading to 2D sheets constituted with 0.7874 nm × 1.0891 nm metallomacrocyclic rectangles. Each vertex of the rectangle is occupied by a copper atom, and the four sides are comprised of multiple hydrogen bonds.
Synthesis of Transition Metal‐Modified Carbon Nitride Polymers for Selective Hydrocarbon Oxidation
Authors: Ding Zhengxin , Chen Xiufang , Antonietti Markus , Wang Xinchen
Published: September 2010

Modification of graphitic carbon nitride (g‐C3N4) photocatalyst with transition metals was achieved with a simple soft‐chemical approach using dicyandiamide monomer and metal chloride as precursors, in combination with a thermal‐induced polycondensation at 600 °C under nitrogen atmosphere. The resultant organic–inorganic hybrid materials were thoroughly characterized by a variety of techniques, including X‐ray diffraction (XRD), UV/Vis spectroscopy, X‐ray photoelectron spectroscopy (XPS), N2‐sorption, transmission electron microscopy (TEM), photoluminescence (PL), and FTIR. Benzene hydroxylation and styrene epoxidation reactions were employed to evaluate the catalytic/photocatalytic activity of the synthesized g‐C3N4‐based catalysts. Results showed that Fe‐ and Cu‐modified g‐C3N4 were active for the hydroxylation of benzene to phenol using H2O2 under mild conditions. It was also found that g‐C3N4 could promote the catalytic epoxidation of styrene using molecular oxygen as the primary oxidant; after modification with Co and Fe, the catalytic performance for styrene epoxidation with O2 could be significantly improved, especially when coupled with visible‐light irradiation.
Variables affecting the quantitation of CD22 in neoplastic B cells
Authors: Jasper Gregory A. , Arun Indu , Venzon David , Kreitman Robert J. , Wayne Alan S. , Yuan Constance M. , Marti Gerald E. , Stetler‐Stevenson Maryalice
Published: September 2010

Background:

Quantitative flow cytometry (QFCM) is being applied in the clinical flow cytometry laboratory for diagnosis, prognosis, and assessment of patients receiving antibody‐based therapy. ABC values and the effect of technical variables on CD22 quantitation in acute lymphoblastic leukemia (ALL), chronic lymphocytic leukemia (CLL), mantle cell lymphoma (MCL), follicular lymphoma (FCL), hairy cell leukemia (HCL) and normal B cells were studied.

Methods:

The QuantiBrite System® was used to determine the level of CD22 expression (mean antibody bound per cell, ABC) by malignant and normal B cells. The intra‐assay variability, number of cells required for precision, effect of delayed processing as well as shipment of peripheral blood specimens (delayed processing and exposure to noncontrolled environments), and the effect of paraformaldehyde fixation on assay results were studied.

Results:

The QuantiBRITE method of measuring CD22 ABC is precise (median CV 1.6%, 95% confidence interval, 1.2–2.3%) but a threshold of 250 malignant cells is required for reliable CD22 ABC values. Delayed processing and overnight shipment of specimens resulted in significantly different ABC values whereas fixation for up to 12 h had no significant effect. ABC measurements determined that CD22 expression is lower than normal in ALL, CLL, FCL, and MCL but higher than normal in HCL.

Conclusions:

CD22 expression was atypical in the hematolymphoid malignancies studied and may have diagnostic utility. Technical variables such as cell number analyzed and delayed processing or overnight shipment of specimens impact significantly on the measurement of antigen expression by QFCM in the clinical laboratory. Published 2010 Wiley‐Liss, Inc.
Screening for the synthetic cannabinoid JWH‐018 and its major metabolites in human doping controls
Authors: Möller Ines , Wintermeyer Annette , Bender Katja , Jübner Martin , Thomas Andreas , Krug Oliver , Schänzer Wilhelm , Thevis Mario
Published: September 2010

Referred to as ‘spice’, several new drugs, advertised as herbal blends, have appeared on the market in the last few years, in which the synthetic cannabinoids JWH‐018 and a C8homologue of CP 47,497 were identified as major active ingredients. Due to their reported cannabis‐like effects, many European countries have banned these substances. The World Anti‐Doping Agency has also explicitly prohibited synthetic cannabinoids in elite sport in‐competition. Since urine specimens have been the preferred doping control samples, the elucidation of the metabolic pathways of these substances is of particular importance to implement them in sports drug testing programmes. In a recent report, anin vitrophase‐I metabolism study of JWH‐018 was presented yielding mainly hydroxylated andN‐dealkylated metabolites. Due to these findings, a urine sample of a healthy man declaring to have smoked a ‘spice’ product was screened for potential phase‐I and ‐II metabolites by high‐resolution/high‐accuracy mass spectrometry in the present report. The majority of the phase‐I metabolites observed in earlierin vitrostudies of JWH‐018 were detected in this urine specimen and furthermore most of their respective monoglucuronides. As no intact JWH‐018 was detectable, the monohydroxylated metabolite being the most abundant one was chosen as a target analyte for sports drug testing purposes; a detection method was subsequently developed and validated in accordance to conventional screening protocols based on enzymatic hydrolysis, liquid‐liquid extraction, and liquid chromatography/electrospray tandem mass spectrometry analysis. The method was applied to approximately 7500 urine doping control samples yielding two JWH‐018 findings and demonstrated its capability for a sensitive and selective identification of JWH‐018 and its metabolites in human urine. Copyright © 2010 John Wiley & Sons, Ltd.
Simultaneous spectrofluorimetric determination of amlodipine besylate and valsartan in their combined tablets
Authors: Shaalan Rasha A. , Belal Tarek S.
Published: September 2010

Amlodipine, a dihydropyridine calcium channel blocker, and valsartan, an angiotensin II receptor blocker, are co‐formulated in a single‐dose combination for the treatment of hypertension. The combination is used by patients whose blood pressure is not adequately controlled on either component monotherapy. This work describes a simple, sensitive, and reliable spectrofluorimetric method for the simultaneous determination of the two antihypertensive drugs; amlodipine besylate (AML) and valsartan (VAL) in their combined tablets. The method involved measurement of the native fluorescence at 455 nm (λEx 360 nm) and 378 nm (λEx 245 nm) for AML and VAL, respectively. Analytical performance of the proposed spectrofluorimetric procedure was statistically validated with respect to linearity, ranges, precision, accuracy, selectivity, robustness, detection, and quantification limits. Regression analysis showed good correlation between fluorescence intensity and concentration over the concentration ranges 0.2–3.6 and 0.008–0.080 µg mL−1 for AML and VAL, respectively. The limits of detection were 0.025 and 0.0012 µg mL−1 for AML and VAL, respectively. The proposed method was successfully applied for the assay of the two drugs in their combined pharmaceutical tablets with recoveries not less than 98.85%. No interference was observed from common pharmaceutical additives. The results were favourably compared with those obtained by a reference spectrophotometric method. Copyright © 2010 John Wiley & Sons, Ltd.
5‐HT1A receptor binding is increased after recovery from bulimia nervosa compared to control women and is associated with behavioral inhibition in both groups
Authors: Bailer Ursula F. , Bloss Cinnamon S. , Frank Guido K. , Price Julie C. , Meltzer Carolyn C. , Mathis Chester A. , Geyer Mark A. , Wagner Angela , Becker Carl R. , Schork Nicholas J. , Kaye Walter H.
Published: September 2010

Objective

Because altered serotonin (5‐HT) function appears to persist after recovery from bulimia nervosa (RBN), we investigated the 5‐HT1A receptor, which could contribute to regulation of appetite, mood, impulse control, or the response to antidepressants.

Method

Thirteen RBN individuals were compared to 21 healthy control women (CW) using positron emission tomography and [carbonyl‐11C]WAY100635 ([11C]WAY).

Results

RBN had a 23–34% elevation of [11C]WAY binding potential (BP)P in subgenual cingulate, mesial temporal, and parietal regions after adjustments for multiple comparisons. For CW, [11C]WAY BPP was related negatively to novelty seeking, whereas for RBN, [11C]WAY BPP was related positively to harm avoidance and negatively related to sensation seeking.

Discussion

Alterations of 5‐HT1A receptor function may provide new insight into efficacy of 5‐HT medication in BN, as well as symptoms such as the ability to inhibit or self‐control the expression of behaviors related to stimulus seeking, aggression, and impulsivity. © 2010 by Wiley Periodicals, Inc. Int J Eat Disord 2011
The efficacy of a brief motivational intervention for individuals with eating disorders: A randomized control trial
Authors: Geller Josie , Brown Krista E. , Srikameswaran Suja
Published: September 2010

Objective

Individuals with eating disorders are often ambivalent about recovery, and previous research has shown that readiness for change predicts enrollment in intensive treatment, symptom change, dropout, and relapse. Given the demonstrated importance of readiness for change, researchers and clinicians have turned to investigating interventions designed to enhance motivation. The purpose of this research was to determine the efficacy of Readiness and Motivation Therapy (RMT), a five‐session individual preparatory intervention for individuals with eating disorders.

Method

Participants completed the Readiness and Motivation Interview and measures of eating disorder symptomatology, self‐esteem, and psychiatric symptoms at intake. One hundred eighty‐one participants were randomly assigned to the treatment (RMT) or wait‐list control condition and were reassessed at 6‐week and 3‐month follow‐up; 113 completed assessments at all three time points and primary analyses were based on these individuals.

Results

Surprisingly, improvements in readiness for change, depression, drive for thinness, and bulimia symptoms occurred over time in both RMT and control conditions. However, at post and at follow‐up, individuals who received RMT were less likely to have high ambivalence than were those from the control condition.

Discussion

RMT may be of benefit to highly reluctant, clinically challenging patients and help them make better use of future, action‐oriented treatment. © 2010 by Wiley Periodicals, Inc. Int J Eat Disord 2011
Suppression of electromagnetic radiation noise from wireless modules in the millimeter‐wave band by means of alumina containing carbon black
Authors: Takase Yasuharu , Hashimoto Osamu , Matsumoto Kouta , Kumada Taketo
Published: September 2010

Unwanted electromagnetic (EM) radiation generated from wireless modules in the millimeter‐wave band used for car radar creates errors and results in performance degradation of electronic equipment. In this paper, to reduce these unwanted EM waves, an optimal design to add the function of EM wave absorption to the lid for the module is examined. Alumina‐containing carbon black is used as a wave absorption material for the lid. Absorption of 20 dB or more is obtained as a measured result with the cover added for EM wave absorption at 60 GHz. The wireless module was also analyzed in the millimeter‐wave band with the designed material used for the lid. The radiation and the reflection of electric power were greatly reduced by the loss electric power from the lid. Therefore, effective data for suppressing unwanted EM radiation noise from wireless modules in the millimeter‐wave band can be provided. © 2010 Wiley Periodicals, Inc. Electron Comm Jpn, 93(10): 25–33, 2010; Published online in Wiley Online Library (wileyonlinelibrary.com). DOI 10.1002/ecj.10216 3
Synthesis, Characterization and Luminescence Properties of Dipyridin‐2‐ylamine Ligands and Their Bis(2,2′‐bipyridyl)ruthenium(II) Complexes and Labelling Studies of Papain from Carica papaya
Authors: Haquette Pierre , Jacques Julien , Dagorne Samuel , Fosse Céline , Salmain Michèle
Published: September 2010

Two luminescent polypyridyl RuII complexes including dipyridin‐2‐ylamine (dpa) ligands functionalized by a maleimide group, namely [Ru(bpy)2(1a–b)](PF6)2 (bpy = 2,2′‐bipyridyl; 1a = 1‐[4‐(dipyridin‐2‐ylamino)butyl]‐1H‐pyrrole‐2,5‐dione; 1b = 1‐[5‐(dipyridin‐2‐ylamino)pentyl]‐1H‐pyrrole‐2,5‐dione), were synthesized, and the X‐ray structure of [Ru(bpy)2(1b)](PF6)2 was solved. The photophysical properties of these complexes and the starting dipyridin‐2‐ylamine ligands were studied. Upon excitation at their maximum of absorption, the dpa ligands exhibited weak luminescence because of quenching by the maleimide group. Conversely, the complexes displayed noticeable luminescence, with an emission wavelength at 600 nm that originated from a metal‐to‐ligand charge‐transfer (MLCT) triplet state. Reaction of the ligands and the complexes with the cysteine endoproteinase papain was shown to occur at the single free cysteine (Cys25) as expected by the usual reactivity of maleimides. The resulting bioconjugates displayed luminescence assigned to the attached fluorophore, and luminescence enhancement was observed with respect to the starting reagents. The circular dichroism spectrum of one of the papain–RuII bioconjugates displayed a typical bisignate band in the near‐UV range, indicating that the reaction of papain with the rac complex appeared to be stereoselective in favour of the Δ enantiomer.
Methylation of Ylidene‐Triazenes: Insight and Guidance for 1,3‐Dipolar Cycloaddition Reactions
Authors: Tennyson Andrew G. , Moorhead Eric J. , Madison Brian L. , Er Joyce A. V. , Lynch Vincent M. , Bielawski Christopher W.
Published: September 2010

Reaction of 1,3‐dimesitylimidazolylidene (1) with p‐functionalized phenyl azides 2 (a: H, b: OCH3, c: NO2) afforded the respective imidazolylidene‐triazenes 3 in good yields (65–99 %). Subsequent treatment with methyl iodide produced the corresponding methylated products 4 in near‐quantitative yields (99 %). Analysis by NOESY 1D NMR spectroscopy and single‐crystal X‐ray diffraction revealed that the methylation reaction was regioselective and occurred at the nitrogen atom most distal from the heterocycle. Consistent with the formation of ionic salts, the 1H NMR signals for the imidazole protons in 4 were shifted > 0.5 ppm downfield compared to 1, indicating the accumulation of positive charge. Similarly, the λmax values recorded for 4 exhibited a much narrower range than those for 3 (16 vs. 77 nm, respectively), suggesting that the frontier orbital energies within the former were dominated by Coulombic effects (i.e., the acquisition of positive charge) as opposed to electronic effects from the electron‐donating or withdrawing groups of the aryl azide. Whereas computational analyses revealed that the observed regioselectivity of the methylation reaction may be explained by thermodynamics, kinetic factors (e.g., sterics) may also be important contributors and render one reaction pathway significantly more accessible due to a lower activation energy.
Determination of genetic damage and urinary metabolites in fuel filling station attendants
Authors: Rekhadevi P.V. , Mahboob M. , Rahman M.F. , Grover Paramjit
Published: September 2010

Fuel (diesel and petrol) constitutes a complex mixture of volatile flammable liquid hydrocarbons among them benzene (BZ), toluene (TOL), and xylene (XYL) are considered to be the most hazardous, predominantly BZ because of its carcinogenic potency. Exposure to these compounds may have an impact on the health of the exposed subjects. Hence, genotoxicity and quantitative analysis of these compounds was performed in blood and urine samples of 200 workers exposed to fuel in filling stations and compared to controls. The level of genetic damage was determined by micronucleus test (MNT) in buccal epithelial cells (BEC) and chromosomal aberrations (CA) assay in peripheral blood lymphocytes (PBL) of fuel filling station attendants (FFSA) and compared to a matched control group. Urine analysis for BZ and its metabolites, phenol (Ph), trans, trans‐Muconic Acid (t, t‐MA), and S‐Phenyl Mercapturic Acid (S‐PMA) was done in all the study subjects. The results of our study revealed that exposure to BTX in petrol vapors induced a statistically significant increase in the frequency of micronuclei (MN) and CA in the exposed subjects than in controls (P < 0.05). There was a significant rise in the levels of urinary BZ, Ph, t, t‐MA, and S‐PMA in the exposed subjects. Our study highlights the significance of MNT, CA, and urinary metabolites as potential biological exposure indices of genetic damage in FFSA. This study suggests the need for regular monitoring of FFSA for possible exposure to BTX as a precautionary and preventive step to minimize exposure and reduce the associated health risks. Environ. Mol. Mutagen., 2011. © 2010 Wiley‐Liss, Inc.
Bi‐directional coupled tuned mass dampers for the seismic response control of two‐way asymmetric‐plan buildings
Authors: Lin Jui‐Liang , Tsai Keh‐Chyuan , Yu Yi‐Jer
Published: September 2010

This paper proposes bi‐directional coupled tuned mass dampers (BiCTMDs) for the seismic response control of two‐way asymmetric‐plan buildings subjected to bi‐directional ground motions. The proposed BiCTMD was developed from the three‐degree‐of‐freedom modal system, which represents the vibration mode of a two‐way asymmetric‐plan building. The performance of the proposed BiCTMD for the seismic response control of elastic two‐way asymmetric‐plan buildings was verified by investigating the reductions of the amplitudes of the associated frequency response functions. In addition, the investigation showed that the proposed BiCTMD is effective in reducing the seismic damage of inelastic asymmetric‐plan buildings. Therefore, the BiCTMD is an effective approach for the seismic response control of both elastic and inelastic two‐way asymmetric‐plan buildings. Copyright © 2010 John Wiley & Sons, Ltd.
Response of white sucker (Catostomus commersoni) to pulp and paper mill effluent in the Androscoggin River, Maine, USA
Authors: Mower Barry F , Munkittrick Kelly R , McMaster Mark E , Van Beneden Rebecca J
Published: September 2010

Adverse effects of pulp and paper mill effluent on fish populations have been well documented in many countries over the last two decades. Some of the initial studies were at mills with conventional chlorine bleaching and no secondary effluent treatment. Following installation of secondary treatment, changes in bleaching technology to elemental chlorine-free bleaching, and other process changes, adverse effects on fish were reduced or eliminated at some mills. Because no two mills are exactly alike, it is difficult to predict adverse impacts of any given mill on fish populations. In 1994, a study of female white sucker (Catostomus commersoni) in the Androscoggin River, Maine, USA, showed induction of mixed function oxidase, reductions in gonad size and plasma estradiol, and an increase in plasma testosterone in fish downstream of discharges from three large bleached kraft pulp and paper mills, and host community municipal sewage treatment plants (STP). After all three mills switched to elemental chlorine-free bleaching in the late 1990s, studies from 2001 to 2003 found that the pattern of reproductive impacts on white sucker populations measured in 1994 was not repeated. In addition, population estimates of white sucker from 2002 to 2003 using mark–recapture techniques found that densities and biomass were well within the range of those of a reference population, and of those reported in the literature for unimpacted populations. Detailed studies immediately above and below each mill/sewage treatment plant showed no evidence of reproductive effects. However, a clear pattern of eutrophication was noted, which increased cumulatively downstream below each mill/STP. Environ. Toxicol. Chem. 2011;30:142–153. © 2010 SETAC
Chronic toxicity of chloride to freshwater species: Effects of hardness and implications for water quality guidelines
Authors: Elphick James R.F , Bergh Kelli D , Bailey Howard C
Published: September 2010

Toxicity tests using nine freshwater species (Ceriodaphnia dubia, Daphnia magna, Oncorhynchus mykiss, Pimephales promelas, Lumbriculus variegatus, Tubifex tubifex, Chironomus dilutus, Hyallela azteca, and Brachionus calyciflorus) were conducted to evaluate their sensitivity to chloride. Acute-to-chronic ratios (ACRs) from these tests indicate the ACR of 7.59 employed by the United States Environmental Protection Agency (U.S. EPA) in deriving its water quality guideline for chloride may be conservative; a revised ACR of 3.50 is presented here. The endpoints used to calculate the ACR included 24-h to 96-h median lethal concentrations (LC50s) for acute tests, and 48-h to 54-d inhibition concentration (ICx) values for growth or reproduction for chronic exposures. Data from the present chronic toxicity tests, and other investigators, were used to propose a water quality guideline for long-term exposure to chloride using a species sensitivity distribution (SSD) approach. The 5th percentile from the SSD was calculated as 307 mg/L and proposed as the water quality guideline. Cladocerans were the most sensitive species in the dataset. Ceriodaphnia dubia was used to evaluate the relationship between water hardness and sensitivity to chloride. A strong relationship was observed and was used to establish a hardness-related equation to modify the proposed water quality guideline on the basis of water hardness, resulting in values ranging from 64 mg/L chloride at 10 mg/L hardness to 388 mg/L chloride at 160 mg/L hardness (as CaCO3). These data suggest that current water quality guidelines for chloride may be overly conservative in water with moderate-to-high hardness, and may not be sufficiently protective under soft-water conditions. Environ. Toxicol. Chem. 2011;30:239–246. © 2010 SETAC
A regional mass balance of methylmercury in San Francisco Bay, California, USA
Authors: Yee Donald , McKee Lester J , Oram John J
Published: September 2010

The San Francisco Bay (California, USA) is a water body listed as impaired because of Hg contamination in sport fish for human consumption, as well as possible effects on resident wildlife. A legacy of Hg mining in local watersheds and Hg used in Au mining in the Sierra Nevada (USA) has contributed to contamination seen in the bay, with additional more recent and ongoing inputs from various sources. Methylmercury is the species of Hg most directly responsible for contamination in biota, so better understanding of its sources, loads, and processes was sought to identify the best means to reduce impacts. A regional scale model of San Francisco Bay was developed to characterize major methylmercury inputs and processes. The model was used to evaluate the potential impact of uncertainties in estimates for methylmercury loading pathways and environmental processes, identify major data gaps, and explore management prospects for reducing methylmercury contamination. External loading pathways considered in the mass balance include methylmercury loads entering via atmospheric deposition to the bay surface, and discharges from the Sacramento/San Joaquin Delta, local watersheds, municipal wastewater, and fringing wetlands. Internal processes considered include exchange between bed and suspended sediments and the water column, in situ production and demethylation, biological uptake, and losses via hydrologic transport to the ocean through the Golden Gate. In situ sediment methylation and demethylation were dominant sources and losses determining ambient steady-state concentrations in the model, with changes in external loads and export causing smaller changes. Better information on methylation and demethylation is thus most critical to improving understanding of methylmercury balances and management. Environ. Toxicol. Chem. 2011;30:88–96. © 2010 SETAC
Assessment of field-related influences on polychlorinated biphenyl exposures and sorbent amendment using polychaete bioassays and passive sampler measurements
Authors: Janssen Elisabeth M.-L , Oen Amy M.P , Luoma Samuel N , Luthy Richard G
Published: September 2010

Field-related influences on polychlorinated biphenyl (PCB) exposure were evaluated by employing caged deposit-feeders, Neanthes arenaceodentata, along with polyoxymethylene (POM) samplers using parallel in situ and ex situ bioassays with homogenized untreated or activated carbon (AC) amended sediment. The AC amendment achieved a remedial efficiency in reducing bioaccumulation by 90% in the laboratory and by 44% in the field transplants. In situ measurements showed that PCB uptake by POM samplers was greater for POM placed in the surface sediment compared with the underlying AC amendment, suggesting that tidal exchange of surrounding material with similar PCB availability as untreated sediment was redeposited in the cages. Polychlorinated biphenyls bioaccumulation with caged polychaetes from untreated sediment was half as large under field conditions compared with laboratory conditions. A biodynamic model was used to confirm and quantify the different processes that could have influenced these results. Three factors appeared most influential in the bioassays: AC amendment significantly reduces bioavailability under laboratory and field conditions; sediment deposition within test cages in the field partially masks the remedial benefit of underlying AC-amended sediment; and deposit-feeders exhibit less PCB uptake from untreated sediment when feeding is reduced. Ex situ and in situ experiments inevitably show some differences that are associated with measurement methods and effects of the environment. Parallel ex situ and in situ bioassays, passive sampler measurements, and quantifying important processes with a model can tease apart these field influences. Environ. Toxicol. Chem. 2011;30:173–180. © 2010 SETAC
Two Early Cretaceous fishes discovered from the most northern area of China: implications for the palaeobiogeography of the Jehol Biota
Authors: Xiao‐Bo Li , Mei‐Sheng Zhang , Yi‐Ni Wang
Published: September 2010

From a newly discovered Early Cretaceous fossil site at the Sanlianhe Coal Mine in Tahe County, Heilongjiang Province, the most northern area in China, two freshwater fossil fish had been recovered. This paper reports their classifications and implications regarding the palaeobiogeography of the Jehol Biota. The fish assemblage consists of Yanosteus sp. (Acipenseriforms) and Sinamia sp. (Amiiformes). Both are important members of the well known Jehol Biota, and their occurrence supports the correlation of the Yiliekede Formation at Sanlianhe Coal Mine site with the Jiufotang Formation of West Liaoning. The remains of the Yanosteus sp. from this locality is the first known record of the genus other than in the Yan‐Liao area of China, and the specimens of Sinamia sp. is quite similar to what may be a new species of Sinamia from West Liaoning. The new fossil site represents the most northern site that is undoubtedly part of the extent of the Jehol Biota as currently understood. The northern Great Xing'an Range area is an important region that may link correlations between the Early Cretaceous continental biotas of China, Mongolia and Russia. Copyright © 2010 John Wiley & Sons, Ltd.
Synthesis of new types of N,N‐disubstituted aminomethylspirophosphoranes
Authors: Prishchenko Andrey A. , Livantsov Mikhail V. , Novikova Olga P. , Livantsova Ludmila I. , Petrosyan Valery S.
Published: September 2010

Aminomethylation of several hydrospirophosphoranes and their derivatives, using chloro‐, alkoxy‐, and amino‐substituted methylamines of various structures, is proposed as the convenient method for the synthesis of new N,N‐disubstituted aminomethylspirophosphoranes. The unique reaction of aminomethylphosphonites with ethylene glycol also resulted in the aminomethylspirophosphoranes via the transesterification followed by the redox process. © 2010 Wiley Periodicals, Inc. Heteroatom Chem 21:515–520, 2010; View this article online at wileyonlinelibrary.com. DOI 10.1002/hc.20642