DOE Office of Scientific and Technical Information (OSTI.GOV)
Kaczmarski, Krzysztof; Guiochon, Georges A
2011-01-01
In supercritical fluid chromatography (SFC), the significant expansion of the mobile phase along the column causes the formation of axial and radial gradients of temperature. Due to these gradients, the mobile phase density, its viscosity, its velocity, its diffusion coefficients, etc. are not constant throughout the column. This results in a nonuniform flow velocity distribution, itself causing a loss of column efficiency in certain cases, even at low flow rates, as they do in HPLC. At high flow rates, an important deformation of the elution profiles of the sample components may occur. The model previously used to account satisfactorily formore » the retention of an unsorbed solute in SFC is applied to the modeling of the elution peak profiles of retained compounds. The numerical solution of the combined heat and mass balance equations provides the temperature and the pressure profiles inside the column and values of the retention time and the band profiles of retained compounds that are in excellent agreement with independent experimental data for large value of mobile phase reduced density. At low reduced densities, the band profiles can strongly depend on the column axial distribution of porosity.« less
Patil, Nitin S; Mendhe, Rakesh B; Sankar, Ajeet A; Iyer, Harish
2008-01-11
In preparative chromatography, often the solubility of the sample in the mobile phase is limited, making the mobile phase unsuitable as a solvent for preparation of load. Generally, solvents that have high solubility for the sample also have higher elution strengths than the mobile phase. Additionally, at high loading volumes, these strong sample solvents are known to adversely affect the band profiles leading to poor chromatographic performance. Here, we show that controlling the mobile phase strength during loading and post-load elution resulted in improved band profiles when the sample solvent was stronger than the mobile phase. Such an approach improves performance in preparative chromatography by allowing either higher sample loading or higher organic content in mobile phase (without loss of yield). Alternately, the approach can be used for improvement in performance by increase in yield or product purity.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Kmak, Kelly N.; Despotopulos, John D.; Shaughnessy, Dawn A.
In this paper, a separation of 209Po, 207Bi and 212Pb using AG 50Wx8 and AG MP 50 cation exchange resins in an HCl medium was developed. A procedure in which Po(IV) elutes first in 0.2 M HCl, followed by Bi(III) in 0.4 M HCl and finally Pb(II) in 2 M HCl was established. The separation using AG 50Wx8 provides a much better elution profile than that of AG MP 50 with no overlap between the elution bands. Finally, this separation has the potential to be used as an isotope generator for producing 210Po from 210Pb.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Gritti, Fabrice; Guiochon, Georges A
2008-01-01
The parameters that affect the shape of the band profiles of acido-basic compounds under moderately overloaded conditions (sample size less than 500 nmol for a conventional column) in RPLC are discussed. Only analytes that have a single pK{sub a} are considered. In the buffer mobile phase used for their elution, their dissociation may, under certain conditions, cause a significant pH perturbation during the passage of the band. Two consecutive injections (3.3 and 10 {micro}L) of each one of three sample solutions (0.5, 5, and 50 mM) of ten compounds were injected on five C{sub 18}-bonded packing materials, including the 5more » {micro}m Xterra-C{sub 18} (121 {angstrom}), 5 {micro}m Gemini-C{sub 18} (110 {angstrom}), 5 {micro}m Luna-C{sub 18}(2) (93 {angstrom}), 3.5 {micro}m Extend-C{sub 18} (80 {angstrom}), and 2.7 {micro}m Halo-C{sub 18} (90 {angstrom}). The mobile phase was an aqueous solution of methanol buffered at a constant {sub W}{sup W}pH of 6, with a phosphate buffer. The total concentration of the phosphate groups was constant at 50 mM. The methanol concentration was adjusted to keep all the retention factors between 1 and 10. The compounds injected were phenol, caffeine, 3-phenyl 1-propanol, 2-phenyl butyric acid, amphetamine, aniline, benzylamine, p-toluidine, procainamidium chloride, and propranololium chloride. Depending on the relative values of the analyte pK{sub a} and the buffer solution pH, these analytes elute as the neutral, the cationic, or the anionic species. The influence of structural parameters such as the charge, the size, and the hydrophobicity of the analytes on the shape of its overloaded band profile is discussed. Simple but general rules predict these shapes. An original adsorption model is proposed that accounts for the unusual peak shapes observed when the analyte is partially dissociated in the buffer solution during its elution.« less
Separation of Pb, Bi and Po by cation exchange resin
Kmak, Kelly N.; Despotopulos, John D.; Shaughnessy, Dawn A.
2017-09-27
In this paper, a separation of 209Po, 207Bi and 212Pb using AG 50Wx8 and AG MP 50 cation exchange resins in an HCl medium was developed. A procedure in which Po(IV) elutes first in 0.2 M HCl, followed by Bi(III) in 0.4 M HCl and finally Pb(II) in 2 M HCl was established. The separation using AG 50Wx8 provides a much better elution profile than that of AG MP 50 with no overlap between the elution bands. Finally, this separation has the potential to be used as an isotope generator for producing 210Po from 210Pb.
Evaluation of the electroosmotic medium pump system for preparative disk gel electrophoresis.
Hayakawa, M; Hosogi, Y; Takiguchi, H; Saito, S; Shiroza, T; Shibata, Y; Hiratsuka, K; Kiyama-Kishikawa, M; Abiko, Y
2001-01-15
This paper describes an improved electroosmotic elution system for preparative sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) based on the epochal idea of H. V. Tan et al. (Nucleic Acids Res. 1988, 16, 1921-1930). In this elution system, a semipermeable membrane, mounted under the gel terminal end, works as the elution pump as well as the partition of the elution chamber. We refer to this system as the "electroosmotic medium pump system." Operation of the constructed apparatus (3.6 cm i.d. disk gel column) and resolution of the protein bands were examined by separation of the model protein mixture (bovine serum albumin (BSA), ovalbumin, bovine carbonic anhydrase, soybean trypsin inhibitor) and purification of the membrane protein, dipeptidyl peptidase IV (DPP IV). The Spectra/Por 7 dialysis membrane provided a better flow profile for the elution buffer. The four model proteins of the protein mixture were able to be completely separated from each other and recovered without dilution. The maximum protein concentration of eluate achieved was 93 mg/ml, when applying a single component, BSA fraction V, as a sample. Furthermore, the multifunctional ectoenzyme, DPP IV, was purified in a single step. Copyright 2001 Academic Press.
[Optimized isolation and purification of non-typeable Haemophilus influenzae Haps protein].
Li, Wan-yi; Kuang, Yu; Li, Ming-yuan; Yang, Yuan; Jiang, Zhong-hua; Yao, Feng; Chen, Chang-chun
2007-12-01
To optimize the isolation and purification conditions for Hap(s) protein of non-typeable Haemophilus influenzae. Hap(s) protein was purified by ammonium sulfate precipitation, dialysis desalting and Hitrap weak cation exchange columns of CM Sepharose Fast Flow. The condition of the elution was optimized for pH and ionic strength, the absorbance at 280 nm of the elution samples were detected, and the targeted protein band in the collected samples was observed by SDS-PAGE electrophoresis. The Hitrap ion exchange column was eluted with buffer 1, which resulted in a baseline distribution of absorbance at 280 nm. Buffer 2 elution of the column resulted in the presence of peak absorbance with trails, which was identified to be constituted by some low molecular weight bands by subsequent SDS-PAGE. In serial column elution with buffer 3 with different ionic strength, a peak absorbance was observed with the ionic strength of 100 mmol/L NaCl, and SDS-PAGE confirmed that the peak was generated by the target protein. No obvious peaks or bands in SDS-PAGE occurred with the other ionic strengths. The pH of the buffer only affect the elution of the irrelevant proteins rather than the Hap(s) protein, and elution with the buffer containing 100 mmol/L NaCl can be optimal for eluting the Hap(s) protein.
NASA Astrophysics Data System (ADS)
Klein, R.; Adler, A.; Beanlands, R. S.; de Kemp, R. A.
2007-02-01
A rubidium-82 (82Rb) elution system is described for use with positron emission tomography. Due to the short half-life of 82Rb (76 s), the system physics must be modelled precisely to account for transport delay and the associated activity decay and dispersion. Saline flow is switched between a 82Sr/82Rb generator and a bypass line to achieve a constant-activity elution of 82Rb. Pulse width modulation (PWM) of a solenoid valve is compared to simple threshold control as a means to simulate a proportional valve. A predictive-corrective control (PCC) algorithm is developed which produces a constant-activity elution within the constraints of long feedback delay and short elution time. The system model parameters are adjusted through a self-tuning algorithm to minimize error versus the requested time-activity profile. The system is self-calibrating with 2.5% repeatability, independent of generator activity and elution flow rate. Accurate 30 s constant-activity elutions of 10-70% of the total generator activity are achieved using both control methods. The combined PWM-PCC method provides significant improvement in precision and accuracy of the requested elution profiles. The 82Rb elution system produces accurate and reproducible constant-activity elution profiles of 82Rb activity, independent of parent 82Sr activity in the generator. More reproducible elution profiles may improve the quality of clinical and research PET perfusion studies using 82Rb.
Klein, R; Adler, A; Beanlands, R S; Dekemp, R A
2007-02-07
A rubidium-82 ((82)Rb) elution system is described for use with positron emission tomography. Due to the short half-life of (82)Rb (76 s), the system physics must be modelled precisely to account for transport delay and the associated activity decay and dispersion. Saline flow is switched between a (82)Sr/(82)Rb generator and a bypass line to achieve a constant-activity elution of (82)Rb. Pulse width modulation (PWM) of a solenoid valve is compared to simple threshold control as a means to simulate a proportional valve. A predictive-corrective control (PCC) algorithm is developed which produces a constant-activity elution within the constraints of long feedback delay and short elution time. The system model parameters are adjusted through a self-tuning algorithm to minimize error versus the requested time-activity profile. The system is self-calibrating with 2.5% repeatability, independent of generator activity and elution flow rate. Accurate 30 s constant-activity elutions of 10-70% of the total generator activity are achieved using both control methods. The combined PWM-PCC method provides significant improvement in precision and accuracy of the requested elution profiles. The (82)Rb elution system produces accurate and reproducible constant-activity elution profiles of (82)Rb activity, independent of parent (82)Sr activity in the generator. More reproducible elution profiles may improve the quality of clinical and research PET perfusion studies using (82)Rb.
Kamarei, Fahimeh; Vajda, Péter; Guiochon, Georges
2013-09-20
This paper compares two methods used for the preparative purification of a mixture of (S)-, and (R)-naproxen on a Whelk-O1 column, using either high performance liquid chromatography or supercritical fluid chromatography. The adsorption properties of both enantiomers were measured by frontal analysis, using methanol-water and methanol-supercritical carbon dioxide mixtures as the mobile phases. The measured adsorption data were modeled, providing the adsorption isotherms and their parameters, which were derived from the nonlinear fit of the isotherm models to the experimental data points. The model used was a Bi-Langmuir isotherm, similar to the model used in many enantiomeric separations. These isotherms were used to calculate the elution profiles of overloaded elution bands, assuming competitive Bi-Langmuir behavior of the two enantiomers. The analysis of these profiles provides the basis for a comparison between supercritical fluid chromatographic and high performance liquid chromatographic preparative scale separations. It permits an illustration of the advantages and disadvantages of these methods and a discussion of their potential performance. Copyright © 2013 Elsevier B.V. All rights reserved.
Abia, Jude A; Mriziq, Khaled S; Guiochon, Georges A
2009-04-01
Using an on-column local electrochemical microdetector operated in the amperometric mode, band elution profiles were recorded at different radial locations at the exit of a 10 mm id, 100 mm long silica-based monolithic column. HETP plots were then acquired at each of these locations, and all these results were fitted to the Knox equation. This provided a spatial distribution of the values of the eddy diffusion (A), the molecular diffusion (B), and the resistance to the kinetics of mass transfer (C) terms. Results obtained indicate that the wall region yields higher A values and smaller C values than the central core region. Significant radial fluctuations of these contributions to band broadening occur throughout the exit column cross-section. This phenomenon is due to the structural radial heterogeneity of the column.
Effect of Nanoparticle Surface on the HPLC Elution Profile of Liposomal Nanoparticles.
Itoh, Naoki; Yamamoto, Eiichi; Santa, Tomofumi; Funatsu, Takashi; Kato, Masaru
2016-06-01
Nanoparticles have been used in diverse areas, and even broader applications are expected in the future. Since surface modification can influence the configuration and toxicity of nanoparticles, a rapid screening method is important to ensure nanoparticle quality. We examined the effect of the nanoparticle surface morphology on the HPLC elution profile using two types of 100-nm liposomal nanoparticles (AmBisome(Ⓡ) and DOXIL(Ⓡ)). These 100-nm-sized nanoparticles eluted before the holdup time (about 4 min), even when a column packed with particles with a relatively large pore size (30 nm) was used. The elution time of the nanoparticles increased with pegylation of the nanoparticles and protein adsorption to the nanoparticles; however, the nanoparticles still eluted before the holdup time. The results of this study indicate that HPLC is a suitable tool for rapid evaluation of the surface of liposomal nanoparticles.
Radial distribution of the flow velocity, efficiency and concentration in a wide HPLC column
DOE Office of Scientific and Technical Information (OSTI.GOV)
Farkas, T.; Sepaniak, M.J.; Guiochon, G.
1997-08-01
The use of optical fibers in a fluorescence-detection scheme permits the accurate determination of the radial distribution of the transit time, the column efficiency, and the analyte concentration at the exit of a chromatographic axial-compression column (50 mmID). The results obtained demonstrate that the column is not homogeneous, but suggest a nearly cylindrical distribution of the packing density. The average velocity close to the column wall is 7% lower than along its axis and the HETP 25% higher. The lack of homogeneity of the column packing is another source of band broadening not taken into account in chromatography so far.more » It causes the apparent HETP derived from the conventional elution chromatogram recorded on the bulk eluent to be larger than the local HETP and the band profile to be unsymmetrical with a slight tail reminiscent of kinetic tailing.« less
Highly porous drug-eluting structures
Elsner, Jonathan J.; Kraitzer, Amir; Grinberg, Orly; Zilberman, Meital
2012-01-01
For many biomedical applications, there is need for porous implant materials. The current article focuses on a method for preparation of drug-eluting porous structures for various biomedical applications, based on freeze drying of inverted emulsions. This fabrication process enables the incorporation of any drug, to obtain an “active implant” that releases drugs to the surrounding tissue in a controlled desired manner. Examples for porous implants based on this technique are antibiotic-eluting mesh/matrix structures used for wound healing applications, antiproliferative drug-eluting composite fibers for stent applications and local cancer treatment, and protein-eluting films for tissue regeneration applications. In the current review we focus on these systems. We show that the release profiles of both types of drugs, water-soluble and water-insoluble, are affected by the emulsion's formulation parameters. The former's release profile is affected mainly through the emulsion stability and the resulting porous microstructure, whereas the latter's release mechanism occurs via water uptake and degradation of the host polymer. Hence, appropriate selection of the formulation parameters enables to obtain desired controllable release profile of any bioactive agent, water-soluble or water-insoluble, and also fit its physical properties to the application. PMID:23507890
Nikitas, P; Pappa-Louisi, A
2005-09-01
The original work carried out by Freiling and Drake in gradient liquid chromatography is rewritten in the current language of reversed-phase liquid chromatography. This allows for the rigorous derivation of the fundamental equation for gradient elution and the development of two alternative expressions of this equation, one of which is free from the constraint that the holdup time must be constant. In addition, the above derivation results in a very simple numerical solution of the various equations of gradient elution under any gradient profile. The theory was tested using eight catechol-related solutes in mobile phases modified with methanol, acetonitrile, or 2-propanol. It was found to be a satisfactory prediction of solute gradient retention behavior even if we used a simple linear description for the isocratic elution of these solutes.
Recursion equations in predicting band width under gradient elution.
Liang, Heng; Liu, Ying
2004-06-18
The evolution of solute zone under gradient elution is a typical problem of non-linear continuity equation since the local diffusion coefficient and local migration velocity of the mass cells of solute zones are the functions of position and time due to space- and time-variable mobile phase composition. In this paper, based on the mesoscopic approaches (Lagrangian description, the continuity theory and the local equilibrium assumption), the evolution of solute zones in space- and time-dependent fields is described by the iterative addition of local probability density of the mass cells of solute zones. Furthermore, on macroscopic levels, the recursion equations have been proposed to simulate zone migration and spreading in reversed-phase high-performance liquid chromatography (RP-HPLC) through directly relating local retention factor and local diffusion coefficient to local mobile phase concentration. This new approach differs entirely from the traditional theories on plate concept with Eulerian description, since band width recursion equation is actually the accumulation of local diffusion coefficients of solute zones to discrete-time slices. Recursion equations and literature equations were used in dealing with same experimental data in RP-HPLC, and the comparison results show that the recursion equations can accurately predict band width under gradient elution.
Kaczmarski, Krzysztof; Poe, Donald P; Guiochon, Georges
2010-10-15
When chromatography is carried out with high-density carbon dioxide as the main component of the mobile phase (a method generally known as "supercritical fluid chromatography" or SFC), the required pressure gradient along the column is moderate. However, this mobile phase is highly compressible and, under certain experimental conditions, its density may decrease significantly along the column. Such an expansion absorbs heat, cooling the column, which absorbs heat from the outside. The resulting heat transfer causes the formation of axial and radial gradients of temperature that may become large under certain conditions. Due to these gradients, the mobile phase velocity and most physico-chemical parameters of the system (viscosity, diffusion coefficients, etc.) are no longer constant throughout the column, resulting in a loss of column efficiency, even at low flow rates. At high flow rates and in serious cases, systematic variations of the retention factors and the separation factors with increasing flow rates and important deformations of the elution profiles of all sample components may occur. The model previously used to account satisfactorily for the effects of the viscous friction heating of the mobile phase in HPLC is adapted here to account for the expansion cooling of the mobile phase in SFC and is applied to the modeling of the elution peak profiles of an unretained compound in SFC. The numerical solution of the combined heat and mass balance equations provides temperature and pressure profiles inside the column, and values of the retention time and efficiency for elution of this unretained compound that are in excellent agreement with independent experimental data. Copyright © 2010 Elsevier B.V. All rights reserved.
Aluminum elution and precipitation in glass vials: effect of pH and buffer species.
Ogawa, Toru; Miyajima, Makoto; Wakiyama, Naoki; Terada, Katsuhide
2015-02-01
Inorganic extractables from glass vials may cause particle formation in the drug solution. In this study, the ability of eluting Al ion from borosilicate glass vials, and tendencies of precipitation containing Al were investigated using various pHs of phosphate, citrate, acetate and histidine buffer. Through heating, all of the buffers showed that Si and Al were eluted from glass vials in ratios almost the same as the composition of borosilicate glass, and the amounts of Al and Si from various buffer solutions at pH 7 were in the following order: citrate > phosphate > acetate > histidine. In addition, during storage after heating, the Al concentration at certain pHs of phosphate and acetate buffer solution decreased, suggesting the formation of particles containing Al. In citrate buffer, Al did not decrease in spite of the high elution amount. Considering that the solubility profile of aluminum oxide and the Al eluting profile of borosilicate glass were different, it is speculated that Al ion may be forced to leach into the buffer solution according to Si elution on the surface of glass vials. When Al ions were added to the buffer solutions, phosphate, acetate and histidine buffer showed a decrease of Al concentration during storage at a neutral range of pHs, indicating the formation of particles containing Al. In conclusion, it is suggested that phosphate buffer solution has higher possibility of forming particles containing Al than other buffer solutions.
De Santo, Ilaria; Sanguigno, Luigi; Causa, Filippo; Monetta, Tullio; Netti, Paolo A
2012-11-07
Drug elution properties of TiO(2) nanotube arrays have been largely investigated by means of solely macroscopic observations. Controversial elution performances have been reported so far and a clear comprehension of these phenomena is still missing as a consequence of a lack of molecular investigation methods. Here we propose a way to discern drug elution properties of nanotubes through the evaluation of drug localization by Fluorescence Correlation Spectroscopy (FCS) analysis. We verified this method upon doxorubicin elution from differently loaded TiO(2) nanotubes. Diverse elution profiles were obtained from nanotubes filled by soaking and wet vacuum impregnation methods. Impregnated nanotubes controlled drug diffusion up to thirty days, while soaked samples completed elution in seven days. FCS analysis of doxorubicin motion in loaded nanotubes clarified that more than 90% of drugs dwell preferentially in inter-nanotube spaces in soaked samples due to decorrelation in a 2D fashion, while a 97% fraction of molecules showed 1D mobility ascribable to displacements along the nanotube vertical axis of wet vacuum impregnated nanotubes. The diverse drug localizations inferred from FCS measurements, together with distinct drug-surface interaction strengths resulting from diverse drug filling techniques, could explain the variability in elution kinetics.
NASA Astrophysics Data System (ADS)
Han, Bin; Lob, Silvia; Sablier, Michel
2018-06-01
In this study, we report the use of pyrolysis-GCxGC/MS profiles for an optimized treatment of data issued from pyrolysis-GC/MS combined with the automatic deconvolution software Automated Mass Spectral Deconvolution and Identification System (AMDIS). The method was illustrated by the characterization of marker compounds of East Asian handmade papers through the examination of pyrolysis-GCxGC/MS data to get information which was used for manually identifying low concentrated and co-eluting compounds in 1D GC/MS data. The results showed that the merits of a higher separation power for co-eluting compounds and a better sensitivity for low concentration compounds offered by a GCxGC system can be used effectively for AMDIS 1D GC/MS data treatment: (i) the compound distribution in pyrolysis-GCxGC/MS profiles can be used as "peak finder" for manual check of low concentration and co-eluting compound identification in 1D GC/MS data, and (ii) pyrolysis-GCxGC/MS profiles can provide better quality mass spectra with observed higher match factors in the AMDIS automatic match process. The combination of 2D profile with AMDIS was shown to contribute efficiently to a better characterization of compound profiles in the chromatograms obtained by 1D analysis in focusing on the mass spectral identification. [Figure not available: see fulltext.
Current manufacturing processes of drug-eluting sutures.
Champeau, Mathilde; Thomassin, Jean-Michel; Tassaing, Thierry; Jérôme, Christine
2017-11-01
Drug-eluting sutures represent the next generation of surgical sutures since they fulfill their mechanical functions but also deliver the drug in their vicinity after implantation. These implants are produced by a variety of manufacturing processes. Drug-eluting sutures represent the next generation of surgical sutures since they fulfill their mechanical functions but also deliver the drug in their vicinity after implantation. These implants are produced by a variety of manufacturing processes. Two general approaches can be followed: (i) the ones that add the API into the material during the manufacturing process of the suture and (ii) the ones that load the API to an already manufactured suture. Areas covered: This review provides an overview of the current manufacturing processes for drug-eluting suture production and discusses their benefits and drawbacks depending on the type of drugs. The mechanical properties and the drug delivery profile of drug-eluting sutures are highlighted since these implants must fulfill both criteria. Expert opinion: For limited drug contents, melt extrusion and electrospinning are the emerging processes since the drug is added during the suture manufacture process. Advantageously, the drug release profile can be tuned by controlling the processing parameters specific to each process and the composition of the drug-containing polymer. If high drug content is targeted, the coating or grafting of a drug layer on a pre-manufactured suture allows for preservation of the tensile strength requirements of the suture.
HPLC-Chip/MS Technology in Proteomic Profiling
NASA Astrophysics Data System (ADS)
Vollmer, Martin; van de Goor, Tom
HPLC-chip/MS is a novel nanoflow analytical technology conducted on a microfabricated chip that allows for highly efficient HPLC separation and superior sensitive MS detection of complex proteomic mixtures. This is possible through on-chip preconcentration and separation with fluidic connection made automatically in a leak-tight fashion. Minimum precolumn and postcolumn peak dispersion and uncompromised ease of use result in compounds eluting in bands of only a few nanoliters. The chip is fabricated out of bio-inert polyimide-containing channels and integrated chip structures, such as an electrospray emitter, columns, and frits manufactured by laser ablation technology. Meanwhile, a variety of HPLC-chips differing in design and stationary phase are commercially available, which provide a comprehensive solution for applications in proteomics, glycomics, biomarker, and pharmaceutical discovery. The HPLC-chip can also be easily integrated into a multidimensional separation workflow where different orthogonal separation techniques are combined to solve a highly complex separation problems. In this chapter, we describe in detail the methodological chip usage and functionality and its application in the elucidation of the protein profile of human nucleoli.
Size-exclusion chromatography system for macromolecular interaction analysis
Stevens, Fred J.
1988-01-01
A low pressure, microcomputer controlled system employing high performance liquid chromatography (HPLC) allows for precise analysis of the interaction of two reversibly associating macromolecules such as proteins. Since a macromolecular complex migrates faster than its components during size-exclusion chromatography, the difference between the elution profile of a mixture of two macromolecules and the summation of the elution profiles of the two components provides a quantifiable indication of the degree of molecular interaction. This delta profile is used to qualitatively reveal the presence or absence of significant interaction or to rank the relative degree of interaction in comparing samples and, in combination with a computer simulation, is further used to quantify the magnitude of the interaction in an arrangement wherein a microcomputer is coupled to analytical instrumentation in a novel manner.
Purification and identification of the fusicoccin binding protein from oat root plasma membrane
NASA Technical Reports Server (NTRS)
de Boer, A. H.; Watson, B. A.; Cleland, R. E.
1989-01-01
Fusicoccin (FC), a fungal phytotoxin, stimulates the H(+) -ATPase located in the plasma membrane (PM) of higher plants. The first event in the reaction chain leading to enhanced H(+) -efflux seems to be the binding of FC to a FC-binding protein (FCBP) in the PM. We solubilized 90% of the FCBP from oat (Avena sativa L. cv Victory) root PM in an active form with 1% octyl-glucoside. The FCBP was stabilized by the presence of protease inhibitors. The FCBP was purified by affinity chromatography using FC-linked adipic acid dihydrazide agarose (FC-AADA). Upon elution with 8 molar urea, two major protein bands on sodium dodecyl sulfate-polyaerylamide gel electrophoresis with molecular weights of 29,700 and 31,000 were obtained. Successive chromatography on BBAB Bio-Gel A, hexyl agarose, and FC-AADA resulted in the same two bands when the FC-AADA was eluted with sodium dodecyl sulfate. A direct correlation was made between 3H-FC-binding activity and the presence of the two protein bands. The stoichiometry of the 29,700 and 31,000 molecular weight bands was 1:2. This suggests that the FCBP occurs in the native form as a heterotrimer with an apparent molecular weight of approximately 92,000.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Choi, Megan; Nordmeyer, Robert A.; Cornell, Earl
2009-10-02
To facilitate a direct interface between protein separation by PAGE and protein identification by mass spectrometry, we developed a multichannel system that continuously collects fractions as protein bands migrate off the bottom of gel electrophoresis columns. The device was constructed using several short linear gel columns, each of a different percent acrylamide, to achieve a separation power similar to that of a long gradient gel. A Counter Free-Flow elution technique then allows continuous and simultaneous fraction collection from multiple channels at low cost. We demonstrate that rapid, high-resolution separation of a complex protein mixture can be achieved on this systemmore » using SDS-PAGE. In a 2.5 h electrophoresis run, for example, each sample was separated and eluted into 48-96 fractions over a mass range of 10-150 kDa; sample recovery rates were 50percent or higher; each channel was loaded with up to 0.3 mg of protein in 0.4 mL; and a purified band was eluted in two to three fractions (200 L/fraction). Similar results were obtained when running native gel electrophoresis, but protein aggregation limited the loading capacity to about 50 g per channel and reduced resolution.« less
A rapid and accurate approach for prediction of interactomes from co-elution data (PrInCE).
Stacey, R Greg; Skinnider, Michael A; Scott, Nichollas E; Foster, Leonard J
2017-10-23
An organism's protein interactome, or complete network of protein-protein interactions, defines the protein complexes that drive cellular processes. Techniques for studying protein complexes have traditionally applied targeted strategies such as yeast two-hybrid or affinity purification-mass spectrometry to assess protein interactions. However, given the vast number of protein complexes, more scalable methods are necessary to accelerate interaction discovery and to construct whole interactomes. We recently developed a complementary technique based on the use of protein correlation profiling (PCP) and stable isotope labeling in amino acids in cell culture (SILAC) to assess chromatographic co-elution as evidence of interacting proteins. Importantly, PCP-SILAC is also capable of measuring protein interactions simultaneously under multiple biological conditions, allowing the detection of treatment-specific changes to an interactome. Given the uniqueness and high dimensionality of co-elution data, new tools are needed to compare protein elution profiles, control false discovery rates, and construct an accurate interactome. Here we describe a freely available bioinformatics pipeline, PrInCE, for the analysis of co-elution data. PrInCE is a modular, open-source library that is computationally inexpensive, able to use label and label-free data, and capable of detecting tens of thousands of protein-protein interactions. Using a machine learning approach, PrInCE offers greatly reduced run time, more predicted interactions at the same stringency, prediction of protein complexes, and greater ease of use over previous bioinformatics tools for co-elution data. PrInCE is implemented in Matlab (version R2017a). Source code and standalone executable programs for Windows and Mac OSX are available at https://github.com/fosterlab/PrInCE , where usage instructions can be found. An example dataset and output are also provided for testing purposes. PrInCE is the first fast and easy-to-use data analysis pipeline that predicts interactomes and protein complexes from co-elution data. PrInCE allows researchers without bioinformatics expertise to analyze high-throughput co-elution datasets.
Shin, Geewook; Lee, Hyungjun; Palaksha, K. J.; Kim, Youngrim; Lee, Eunyoung; Shin, Yongseung; Lee, Eunggoo; Park, Kyungdae
2006-01-01
The present study was undertaken to produce monoclonal antibodies (MAbs) against immunoglobulin (Ig) purified from black rockfish (Sebastes schlegeli Higendorf) serum using protein A, mannan binding protein, and goat IgG affinity columns. These three different ligands were found to possess high affinity for black rockfish serum Ig. All of the Igs purified eluted at only 0.46 M NaCl concentration in anion exchange column chromatography and consisted of two bands at 70 kDa and 25 kDa in SDS-PAGE; they also had similar antigenicity for MAbs to Ig heavy chain in immunoblot assays. Therefore, black rockfish Ig is believed to exist as a single isotype within serum. The MAbs produced against Ig heavy chain reacted specifically with spots distributed over the pI range from 4.8 to 5.6 with a molecular weight of 70 kDa on two dimensional gel electrophoresis immunoblot profiles. PMID:16871026
Siemens, I R; Yee, D K; Reagan, L P; Fluharty, S J
1994-01-01
The murine neuroblastoma N1E-115 cell line possesses type 1 and type 2 angiotensin II (AngII) receptor subtypes. In vitro differentiation of these cells substantially increases the density of the AT2-receptor subtype, whereas the density of the AT1 receptors remains unchanged. In the present study, we report that the zwitterionic detergent 3-[(3-cholamidopropyl)dimethylammonio]-1-propanesulfonate (CHAPS) selectively solubilized AT2 receptors from N1E-115 cell membranes and that these receptors could be purified further to near homogeneity by affinity chromatography. More specifically, the presence of an agonist (AngII) during affinity purification of AT2 receptors resulted in the elution of high (110-kDa) and low (66-kDa) molecular mass proteins as determined by gel electrophoresis under nonreducing conditions. In contrast, when the nonselective antagonist Sar1,Ile8-AngII was used during purification, only the lower 66-kDa protein was observed. Affinity purification in the presence of the peptide and nonpeptide AT2-receptor antagonists CGP42112A and PD123319 also resulted in elution of the same 66-kDa protein, but unlike that in the presence of Sar1,Ile8-AngII, some of the high molecular weight site was observed as well. On the other hand, Losartan, an AT1-receptor antagonist, was completely ineffective in eluting any AngII receptors from the affinity column, further confirming their AT2 identity. After agonist elution, the 110-kDa band dissociated into two low molecular mass bands of 66 kDa and 54 kDa when sodium dodecyl sulfate-gel electrophoresis was run under reducing conditions.(ABSTRACT TRUNCATED AT 250 WORDS)
Effect of modulator sorption on gradient shape in ion-exchange chromatography
NASA Technical Reports Server (NTRS)
Velayudhan, A.; Ladisch, M. R.; Mitchell, C. A. (Principal Investigator)
1995-01-01
Mobile phase additives, or modulators, are used in gradient elution chromatography to facilitate separation and reduce separation time. The modulators are usually assumed to be linearly adsorbed or unadsorbed. Here, the consequences of nonlinear modulator adsorption are examined for ion-exchange gradient elution through a series of simulations. Even when the buffer salt is identical to the modulator salt, gradient deformation is observed; the extent of deformation increases as the volume of the feed is increased. When the modulator salt is different from the buffer salt, unusual effects are observed, and the chromatograms are quite different from those predicted by classical gradient elution theory. In particular, local increases in the buffer concentration are found between feed bands, and serve to improve the separation. These effects become more pronounced as the feed volume increases, and could therefore prove valuable in preparative applications.
Gruendling, Till; Guilhaus, Michael; Barner-Kowollik, Christopher
2008-09-15
We report on the successful application of size exclusion chromatography (SEC) combined with electrospray ionization mass spectrometry (ESI-MS) and refractive index (RI) detection for the determination of accurate molecular weight distributions of synthetic polymers, corrected for chromatographic band broadening. The presented method makes use of the ability of ESI-MS to accurately depict the peak profiles and retention volumes of individual oligomers eluting from the SEC column, whereas quantitative information on the absolute concentration of oligomers is obtained from the RI-detector only. A sophisticated computational algorithm based on the maximum entropy principle is used to process the data gained by both detectors, yielding an accurate molecular weight distribution, corrected for chromatographic band broadening. Poly(methyl methacrylate) standards with molecular weights up to 10 kDa serve as model compounds. Molecular weight distributions (MWDs) obtained by the maximum entropy procedure are compared to MWDs, which were calculated by a conventional calibration of the SEC-retention time axis with peak retention data obtained from the mass spectrometer. Comparison showed that for the employed chromatographic system, distributions below 7 kDa were only weakly influenced by chromatographic band broadening. However, the maximum entropy algorithm could successfully correct the MWD of a 10 kDa standard for band broadening effects. Molecular weight averages were between 5 and 14% lower than the manufacturer stated data obtained by classical means of calibration. The presented method demonstrates a consistent approach for analyzing data obtained by coupling mass spectrometric detectors and concentration sensitive detectors to polymer liquid chromatography.
Jeliazkova, Ekaterina; Zheljazkov, Valtcho D; Kačániova, Miroslava; Astatkie, Tess; Tekwani, Babu L
2018-06-07
The profile and bioactivity of hops (Humulus lupulus L.) essential oil, a complex natural product extracted from cones via steam distillation, depends on genetic and environmental factors, and may also depend on extraction process. We hypothesized that compound mixtures eluted sequentially and captured at different timeframes during the steam distillation process of whole hop cones would have differential chemical and bioactivity profiles. The essential oil was collected sequentially at 8 distillation time (DT) intervals: 0-2, 2-5, 5-10, 10-30, 30-60, 60-120, 120-180, and 180-240 min. The control was a 4-h non-interrupted distillation. Nonlinear regression models described the DT and essential oil compounds relationship. Fractions yielded 0.035 to 0.313% essential oil, while control yielded 1.47%. The oil eluted during the first hour was 83.2%, 9.6% during the second hour, and only 7.2% during the second half of the distillation. Essential oil (EO) fractions had different chemical profile. Monoterpenes were eluted early, while sequiterpenes were eluted late. Myrcene and linalool were the highest in 0-2 min fraction, β-caryophyllene, β-copaene, β-farnesene, and α-humulene were highest in fractions from middle of distillation, whereas α- bergamotene, γ-muurolene, β- and α-selinene, γ- and δ-cadinene, caryophyllene oxide, humulne epoxide II, τ-cadinol, and 6-pentadecen-2-one were highest in 120-180 or 180-240 min fractions. The Gram-negative Escherichia coli was strongly inhibited by essential oil fractions from 2-5 min and 10-30 min, followed by oil fraction from 0-2 min. The strongest inhibition activity against Gram-negative Yersinia enterocolitica, and Gram-positive Clostridium perfringens, Enterococcus faecalis, and Staphylococcus aureus subs. aureus was observed with the control essential oil. This is the first study to describe significant activity of hops essential oils against Trypanosoma brucei, a parasitic protozoan that causes African trypanosomiasis (sleeping sickness in humans and nagana in other animals). Hops essential oil fractions or whole oil may be used as antimicrobial agents or for the development of new drugs.
Ma, Hongyan; Delafield, Daniel G; Wang, Zhe; You, Jianlan; Wu, Si
2017-04-01
The microbial secretome, known as a pool of biomass (i.e., plant-based materials) degrading enzymes, can be utilized to discover industrial enzyme candidates for biofuel production. Proteomics approaches have been applied to discover novel enzyme candidates through comparing protein expression profiles with enzyme activity of the whole secretome under different growth conditions. However, the activity measurement of each enzyme candidate is needed for confident "active" enzyme assignments, which remains to be elucidated. To address this challenge, we have developed an Activity-Correlated Quantitative Proteomics Platform (ACPP) that systematically correlates protein-level enzymatic activity patterns and protein elution profiles using a label-free quantitative proteomics approach. The ACPP optimized a high performance anion exchange separation for efficiently fractionating complex protein samples while preserving enzymatic activities. The detected enzymatic activity patterns in sequential fractions using microplate-based assays were cross-correlated with protein elution profiles using a customized pattern-matching algorithm with a correlation R-score. The ACPP has been successfully applied to the identification of two types of "active" biomass-degrading enzymes (i.e., starch hydrolysis enzymes and cellulose hydrolysis enzymes) from Aspergillus niger secretome in a multiplexed fashion. By determining protein elution profiles of 156 proteins in A. niger secretome, we confidently identified the 1,4-α-glucosidase as the major "active" starch hydrolysis enzyme (R = 0.96) and the endoglucanase as the major "active" cellulose hydrolysis enzyme (R = 0.97). The results demonstrated that the ACPP facilitated the discovery of bioactive enzymes from complex protein samples in a high-throughput, multiplexing, and untargeted fashion. Graphical Abstract ᅟ.
NASA Astrophysics Data System (ADS)
Ma, Hongyan; Delafield, Daniel G.; Wang, Zhe; You, Jianlan; Wu, Si
2017-04-01
The microbial secretome, known as a pool of biomass (i.e., plant-based materials) degrading enzymes, can be utilized to discover industrial enzyme candidates for biofuel production. Proteomics approaches have been applied to discover novel enzyme candidates through comparing protein expression profiles with enzyme activity of the whole secretome under different growth conditions. However, the activity measurement of each enzyme candidate is needed for confident "active" enzyme assignments, which remains to be elucidated. To address this challenge, we have developed an Activity-Correlated Quantitative Proteomics Platform (ACPP) that systematically correlates protein-level enzymatic activity patterns and protein elution profiles using a label-free quantitative proteomics approach. The ACPP optimized a high performance anion exchange separation for efficiently fractionating complex protein samples while preserving enzymatic activities. The detected enzymatic activity patterns in sequential fractions using microplate-based assays were cross-correlated with protein elution profiles using a customized pattern-matching algorithm with a correlation R-score. The ACPP has been successfully applied to the identification of two types of "active" biomass-degrading enzymes (i.e., starch hydrolysis enzymes and cellulose hydrolysis enzymes) from Aspergillus niger secretome in a multiplexed fashion. By determining protein elution profiles of 156 proteins in A. niger secretome, we confidently identified the 1,4-α-glucosidase as the major "active" starch hydrolysis enzyme (R = 0.96) and the endoglucanase as the major "active" cellulose hydrolysis enzyme (R = 0.97). The results demonstrated that the ACPP facilitated the discovery of bioactive enzymes from complex protein samples in a high-throughput, multiplexing, and untargeted fashion.
Glenne, Emelie; Leek, Hanna; Klarqvist, Magnus; Samuelsson, Jörgen; Fornstedt, Torgny
2017-05-05
Strangely shaped overloaded bands were recently reported using a standard supercritical fluid chromatographic system comprising a diol column as the stationary phase and carbon dioxide with methanol as the mobile phase. Some of these overloaded elution profiles appeared strongly deformed and even had "anti-Langmuirian" shapes although their solute compounds had "Langmuirian" adsorption. To obtain a more complete understanding of the generality of these effects, the investigation was expanded to cover also other common co-solvents, such as ethanol, 2-propanol, and acetonitrile, as well as various stationary phase materials, such as silica, and 2-ethylpyridine. From this expanded study it could be confirmed that the effects of deformed overloaded solute band shapes, due to co-solvent adsorption, is general phenomena in supercritical fluid chromatographic. It could also be concluded that these effects as well as previously observed "solvent effects" or "plug effects" are entirely due to competition between the solute and solvent molecules for the adsorption sites on the stationary phase surface. Finally, guidelines were given for how to evaluate the risk of deformations occurring for a given solvent-column combination, based simply on testing retention times of solutes and co-solvent. Copyright © 2017 Elsevier B.V. All rights reserved.
Omar, Jone; Olivares, Maitane; Amigo, José Manuel; Etxebarria, Nestor
2014-04-01
Comprehensive Two Dimensional Gas Chromatography - Mass Spectrometry (GC × GC/qMS) analysis of Cannabis sativa extracts shows a high complexity due to the large variety of terpenes and cannabinoids and to the fact that the complete resolution of the peaks is not straightforwardly achieved. In order to support the resolution of the co-eluted peaks in the sesquiterpene and the cannabinoid chromatographic region the combination of Multivariate Curve Resolution and Alternating Least Squares algorithms was satisfactorily applied. As a result, four co-eluting areas were totally resolved in the sesquiterpene region and one in the cannabinoid region in different samples of Cannabis sativa. The comparison of the mass spectral profiles obtained for each resolved peak with theoretical mass spectra allowed the identification of some of the co-eluted peaks. Finally, the classification of the studied samples was achieved based on the relative concentrations of the resolved peaks. Copyright © 2014 Elsevier B.V. All rights reserved.
Ontogeny of a novel pituitary protein (7B2) in the human fetal intestine.
Suzuki, H; Christofides, N D; Adrian, T E; Chretien, M; Seidah, N G; Polak, J M; Bloom, S R
1985-11-28
The developmental profile of the concentration of a novel pituitary protein (7B2) was studied immunochemically in the human gastrointestinal tract from 12 weeks of gestation to 4 months after birth and was compared to the distribution in the adult. 7B2-like immunoreactivity (IR-7B2) was detected in all segments studied, but no gross changes were seen through fetal life. At term higher concentrations of IR-7B2 were found in the duodenum and the antrum, which is similar to the distribution of adult man. Gel permeation chromatography revealed that the main peak of 7B2 immunoreactivity in the fetal intestinal extract eluted with a Kav of 0.3. Similar elution profiles were also observed in extracts of human adult intestine.
NASA Astrophysics Data System (ADS)
Mahoney, Christine M.; Patwardhan, Dinesh V.; Ken McDermott, M.
2006-07-01
Secondary ion mass spectrometry (SIMS) employing an SF 5+ polyatomic primary ion source was utilized to analyze several materials commonly used in drug-eluting stents (DES). Poly(ethylene- co-vinyl acetate) (PEVA), poly(lactic- co-glycolic acid) (PLGA) and various poly(urethanes) were successfully depth profiled using SF 5+ bombardment. The resultant molecular depth profiles obtained from these polymeric films showed very little degradation in molecular signal as a function of increasing SF 5+ primary ion dose when experiments were performed at low temperatures (signal was maintained for doses up to ˜5 × 10 15 ions/cm 2). Temperature was determined to be an important parameter in both the success of the depth profiles and the mass spectral analysis of the polymers. In addition to the pristine polymer films, paclitaxel (drug released in Taxus™ stent) containing PLGA films were also characterized, where it was confirmed that both drug and polymer signals could be monitored as a function of depth at lower paclitaxel concentrations (10 wt%).
Cornelius, Rena M.; Shankar, Sucharita P.; Brash, John L.; Babensee, Julia E.
2011-01-01
Intact and fragmented proteins, eluted from self assembled monolayer (SAM) surfaces of alkanethiols of different chemistries (-CH3, -OH, -COOH, -NH2 ), following exposure to human plasma (HP) or human serum (HS), were examined using sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) and immunoblotting techniques. The SAM surfaces were incubated for 1 hour with 10% (v/v) sterile-filtered heat-inactivated (h.i.) HS or 1% (v/v) sterile-filtered h.i. HP preparations [both in phosphate buffered saline (PBS)]. Adsorbed proteins were eluted using 10% SDS/2.3% dithioerythritol for characterization of protein profiles. The type of incubating medium may be an important determinant of adsorbed protein profiles, since some variations were observed in eluates from filtered versus control unfiltered h.i. 10% HS or 1% HP. Albumin and apolipoprotein A1 were consistently detected in both filtered h.i 10% HS and 1% HP eluates from all SAM surfaces and from control tissue culture-treated polystyrene (TCPS). Interestingly, Factor H and Factor I, antithrombin, prothrombin, high molecular weight kininogen (HMWK) and IgG were present in eluates from OH, COOH and NH2 SAM surfaces and in eluates from TCPS, but not in eluates from CH3 SAM surfaces, following exposure to filtered h.i. 10% HS. These results suggest that CH3 SAM surfaces were the least pro-inflammatory of all SAM surfaces. Overall, similar trends were observed in the profiles of proteins eluted from surfaces exposed to filtered 10% HS or 1% HP. However the unique profiles of adsorbed proteins on different SAM surface chemistries may be related to their differential interactions with cells, including immune/inflammatory cells. PMID:21509932
Singh, Manoj; Metwal, Mamta; Kumar, Vandana A; Kumar, Anil
2016-01-30
Attempts were made to identify and characterize the calcium binding proteins (CaBPs) in grain filling stages of finger millet using proteomics, bioinformatics and molecular approaches. A distinctly observed blue color band of 48 kDa stained by Stains-all was eluted and analyzed as calreticulin (CRT) using nano liquid chromatography-tandem mass spectrometry (nano LC-MS). Based on the top hits of peptide mass fingerprinting results, conserved primers were designed for isolation of the CRT gene from finger millet using calreticulin sequences of different cereals. The deduced nucleotide sequence analysis of 600 bp amplicon showed up to 91% similarity with CRT gene(s) of rice and other plant species and designated as EcCRT1. Transcript profiling of EcCRT1 showed different levels of relative expression at different stages of developing spikes. The higher expression of EcCRT1 transcripts and protein were observed in later stages of developing spikes which might be due to greater translational synthesis of EcCRT1 protein during seed maturation in finger millet. Preferentially higher synthesis of this CaBP during later stages of grain filling may be responsible for the sequestration of calcium in endoplasmic reticulum of finger millet grains. © 2015 Society of Chemical Industry.
Partial purification of coriolus versicolor's extracellular polyphenol oxidase (PPO)
DOE Office of Scientific and Technical Information (OSTI.GOV)
Moore, N.L.; Dashek, W.V.
1993-05-01
Coriolus versicolor, a white-rot basidiomycete, secretes ligno-celluloytic enzymes. Because these are valuable to paper-pulp agricultural industries, trials are in progress to substrate induce these enzymes enhance their secretions. Reported are attempts to develop an extracellular PPO (o-diphenols to 0-diquinones) purification protocol applicable to [open quote]batch-cultured[close quote] C. versicolor. Whereas dialysis (MW [open quote]cut-off[close quote], 14,000) of 13 day growth medium (GM) resulted in 2.17 fold PPO spc. act. increase, dialysis plus a 0-30% (NH[sub 4])[sub 2]SO[sub 4] [open quote]cut[close quote] yielded a 3.27 fold enhancement. Subsequent GM chromatography on DEAE CM-Sephadexes revealed that PPO exchanged with DEAE's counterion without enhancingmore » spc. act. Gel filtration of GM commercial PPOs on G-150 resulted in similar elutions indicating a substitute for ion exchange chromatography. Time-dependent fungal growth in liquid medium followed by viscometry utilizing CMC revealed a GM endocellulase 2 days after inoculation an activity rise to day 12. Filteration of Onozuka cellulase on G-150 yielded an elution profile similar to those of GM authentic PPO's compounding C. versicolor's PPO purification. SDS-PAGE of dialyzed GM revealed 4 proteins, one of which was removed by the (NH[sub 4])[sub 2]SO[sub 4]. The m[sub TS] of commercial Sigma's PPO Onozuka cellulase were 0.76 0.59, respectively, for comparison to C. versicolor's PPO. Affinity, hydroxylapatite hydrophobic interaction chromatographies may yield a single SDS-PAGE PPO band.« less
The impact of column connection on band broadening in very high pressure liquid chromatography.
Stankovich, Joseph J; Gritti, Fabrice; Stevenson, Paul G; Guiochon, Georges
2013-09-01
A series of experiments was conducted to evaluate the degree of band broadening in very high pressure LC due to column connections. Different column manufacturers use slightly different designs for their column fittings. If the same column connections are repeatedly used to attach columns of different origins, different void volumes form between capillary tubes and column inlets. An Agilent Ultra Low Dispersion Kit (tubing id 75 μm) was installed on an Agilent Infinity 1290 ultra HPLC and used to connect successively an Agilent, a Phenomenex, and a Waters column. A series of uracil (unretained) samples were injected and eluted at a wide range of flow rates with a water/acetonitrile mixture as eluent. In order to determine the variance contribution from column connections as accurately as possible a nonretained probe compound was selected because the variance contribution from the column is the smallest for analytes, which have very low k values. Yet, this effect still has an impact on the resolution for moderately retained compounds (k > 2) for narrow-bore columns packed with fine particles, since variance contributions are additive for linear chromatographic systems. Each injection was replicated five times under the same experimental conditions. Then NanoViper column connections (tubing id 75 μm) were used and the same injections were made. This system was designed to minimize connection void volumes for any column. Band variances were calculated as the second central moment of elution peaks and used to assess the degree of band broadening due to the column connections. Band broadening may increase from 3.8 to 53.9% when conventional metal ferrules were used to join columns to connection sites. The results show that the variance contribution from improper connections can generate as much as 60.5% of the total variance observed. This demonstrates that column connections can play a larger role than the column packing with respect to band dispersion. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Atrial natriuretic-like peptide and its prohormone within metasequoia.
Yang, Q; Gower, W R; Li, C; Chen, P; Vesely, D L
1999-07-01
Metasequoia glyptostroboides was one of the dominant conifers in North America, Asia, and Europe for more than 100 million years since the late Cretaceous Albian Age, but Quaternary glaciations drove the Metasequoia population to apparent extinction. A small pocket of Metasequoia, however, was found in central China in the 1940s representing the only surviving population of this "living fossil" species. Atrial natriuretic peptide, a 28-amino-acid peptide hormone that causes sodium and water excretion in animals, has been found to be part of the first peptide hormonal system in lower plants. The existence of this hormonal system has never been examined within trees of any genus. High-performance gel permeation chromatography of the leaves and stems (i.e., branches) of Metasequoia followed by atrial natriuretic peptide radioimmunoassay revealed an ANP-like peptide and its prohormone (i.e., approximately 13,000 mol wt) were present in both leaves and stems of this conifer. The elution profile of ANP-like peptide in stems of Metasequoia had a shoulder to the left of where pure synthetic ANP elutes suggesting the possibility of a slightly larger peptide eluting within this shoulder secondary to alternate processing of the ANP-like prohormone and similar to what occurs with the kidney of animals. The elution profile of ANP-like peptide in the leaves of Metasequoia revealed two peaks; one where ANP elutes and a second peak suggesting a smaller peptide that has been metabolically processed. The presence of the ANP-like prohormone strongly suggests that ANP-like gene expression is occurring in both leaves and stems of Metasequoia since this prohormone is the gene product of this hormonal system. The presence of the ANP-like hormonal system in trees implies that this hormonal system may have been present early in land plant evolution to allow trees to reach heights of greater than 30 feet where a water flow-enhancing substance is absolutely necessary for water flow to occur to these heights.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Heo, Sung; College of Information and Communication Engineering, Sungkyunkwan University, Cheoncheon-dong 300, Jangan-gu, Suwon 440-746; Lee, Hyung-Ik
2015-06-29
To investigate the band gap profile of Cu(In{sub 1−x},Ga{sub x})(Se{sub 1−y}S{sub y}){sub 2} of various compositions, we measured the band gap profile directly as a function of in-depth using high-resolution reflection energy loss spectroscopy (HR-REELS), which was compared with the band gap profile calculated based on the auger depth profile. The band gap profile is a double-graded band gap as a function of in-depth. The calculated band gap obtained from the auger depth profile seems to be larger than that by HR-REELS. Calculated band gaps are to measure the average band gap of the spatially different varying compositions with respectmore » to considering its void fraction. But, the results obtained using HR-REELS are to be affected by the low band gap (i.e., out of void) rather than large one (i.e., near void). Our findings suggest an analytical method to directly determine the band gap profile as function of in-depth.« less
Chen, Apeng; Lynch, Kyle B; Wang, Xiaochun; Lu, Joann J; Gu, Congying; Liu, Shaorong
2014-09-24
We integrate a high-pressure electroosmotic pump (EOP), a nanoflow gradient generator, and a capillary column into a miniaturized liquid chromatographic system that can be directly coupled with a mass spectrometer for proteomic analysis. We have recently developed a low-cost high-pressure EOP capable of generating pressure of tens of thousands psi, ideal for uses in miniaturized HPLC. The pump worked smoothly when it was used for isocratic elutions. When it was used for gradient elutions, generating reproducible gradient profiles was challenging; because the pump rate fluctuated when the pump was used to pump high-content organic solvents. This presents an issue for separating proteins/peptides since high-content organic solvents are often utilized. In this work, we solve this problem by incorporating our high-pressure EOP with a nano-flow gradient generator so that the EOP needs only to pump an aqueous solution. With this combination, we develop a capillary-based nano-HPLC system capable of performing nano-flow gradient elution; the pump rate is stable, and the gradient profiles are reproducible and can be conveniently tuned. To demonstrate its utility, we couple it with either a UV absorbance detector or a mass spectrometer for peptide separations. Copyright © 2014. Published by Elsevier B.V.
Paclitaxel Drug-eluting Tracheal Stent Could Reduce Granulation Tissue Formation in a Canine Model
Wang, Ting; Zhang, Jie; Wang, Juan; Pei, Ying-Hua; Qiu, Xiao-Jian; Wang, Yu-Ling
2016-01-01
Background: Currently available silicone and metallic stents for tracheal stenosis are associated with many problems. Granulation proliferation is one of the main complications. The present study aimed to evaluate the efficacy of paclitaxel drug-eluting tracheal stent in reducing granulation tissue formation in a canine model, as well as the pharmacokinetic features and safety profiles of the coated drug. Methods: Eight beagles were randomly divided into a control group (bare-metal stent group, n = 4) and an experimental group (paclitaxel-eluting stent group, n = 4). The observation period was 5 months. One beagle in both groups was sacrificed at the end of the 1st and 3rd months, respectively. The last two beagles in both groups were sacrificed at the end of 5th month. The proliferation of granulation tissue and changes in tracheal mucosa were compared between the two groups. Blood routine and liver and kidney function were monitored to evaluate the safety of the paclitaxel-eluting stent. The elution method and high-performance liquid chromatography were used to characterize the rate of in vivo release of paclitaxel from the stent. Results: Compared with the control group, the proliferation of granulation tissue in the experimental group was significantly reduced. The drug release of paclitaxel-eluting stent was the fastest in the 1st month after implantation (up to 70.9%). Then, the release slowed down gradually. By the 5th month, the release reached up to 98.5%. During the observation period, a high concentration of the drug in the trachea (in the stented and adjacent unstented areas) and lung tissue was not noted, and the blood test showed no side effect. Conclusions: The paclitaxel-eluting stent could safely reduce the granulation tissue formation after stent implantation in vivo, suggesting that the paclitaxel-eluting tracheal stent might be considered for potential use in humans in the future. PMID:27824004
Zarghani, Maryam; Parastar, Hadi
2017-11-17
The objective of the present work is development of joint approximate diagonalization of eigenmatrices (JADE) as a member of independent component analysis (ICA) family, for the analysis of gas chromatography-mass spectrometry (GC-MS) and comprehensive two-dimensional gas chromatography-mass spectrometry (GC×GC-MS) data to address incomplete separation problem occurred during the analysis of complex sample matrices. In this regard, simulated GC-MS and GC×GC-MS data sets with different number of components, different degree of overlap and noise were evaluated. In the case of simultaneous analysis of multiple samples, column-wise augmentation for GC-MS and column-wise super-augmentation for GC×GC-MS was used before JADE analysis. The performance of JADE was evaluated in terms of statistical parameters of lack of fit (LOF), mutual information (MI) and Amari index as well as analytical figures of merit (AFOMs) obtained from calibration curves. In addition, the area of feasible solutions (AFSs) was calculated by two different approaches of MCR-BANDs and polygon inflation algorithm (FACPACK). Furthermore, JADE performance was compared with multivariate curve resolution-alternating least squares (MCR-ALS) and other ICA algorithms of mean-field ICA (MFICA) and mutual information least dependent component analysis (MILCA). In all cases, JADE could successfully resolve the elution and spectral profiles in GC-MS and GC×GC-MS data with acceptable statistical and calibration parameters and their solutions were in AFSs. To check the applicability of JADE in real cases, JADE was used for resolution and quantification of phenanthrene and anthracene in aromatic fraction of heavy fuel oil (HFO) analyzed by GC×GC-MS. Surprisingly, pure elution and spectral profiles of target compounds were properly resolved in the presence of baseline and interferences using JADE. Once more, the performance of JADE was compared with MCR-ALS in real case. On this matter, the mutual information (MI) values were 1.01 and 1.13 for resolved profiles by JADE and MCR-ALS, respectively. In addition, LOD values (μg/mL) were respectively 1.36 and 1.24 for phenanthrene and 1.26 and 1.09 for anthracene using MCR-ALS and JADE which showed outperformance of JADE over MCR-ALS. Copyright © 2017 Elsevier B.V. All rights reserved.
Analysis of the multiple forms of Gaucher spleen sphingolipid activator protein 2.
Paton, B C; Poulos, A
1988-01-01
Gaucher spleen sphingolipid activator protein 2 was fractionated into concanavalin A binding- and non-binding fractions. These fractions each contained several bands on non-denaturing polyacrylamide gel electrophoresis (PAGE). The two fractions were further fractionated by electroblotting the proteins from preparative gels onto nitrocellulose, staining with Ponceau S to locate the bands of protein and then eluting the protein components from the nitrocellulose. A total of ten fractions, each containing only one or two major components, was collected. All of these subfractions activated beta-glucocerebrosidase and sphingomyelinase and most subfractions also activated beta-galactocerebrosidase. The structural relationship of the bands was investigated using endoglycosidase digestions. The results indicated that the two bands with the fastest mobility on non-denaturing PAGE did not contain any carbohydrate. The remaining bands showed only limited or partial digestion with endoglycosidase H and endoglycosidase D, but were readily hydrolysed with endoglycosidase F. The products of these digestions included bands with similar mobilities to the non-carbohydrate containing bands. Images Fig. 1. Fig. 2. Fig. 3. PMID:3178760
Wolf, William M; Vlachos, Helen A; Marroquin, Oscar C; Lee, Joon S; Smith, Conrad; Anderson, William D; Schindler, John T; Holper, Elizabeth M; Abbott, J Dawn; Williams, David O; Laskey, Warren K; Kip, Kevin E; Kelsey, Sheryl F; Mulukutla, Suresh R
2010-02-01
Diabetes is a powerful predictor of adverse events in patients undergoing percutaneous coronary intervention. Drug-eluting stents reduce restenosis rates compared with bare metal stents; however, controversy remains regarding which drug-eluting stents provides greater benefit in patients with diabetes. Accordingly, we compared the safety and efficacy of sirolimus-eluting stents (SES) with paclitaxel-eluting stents (PES) among diabetic patients in a contemporary registry. Using the National Heart, Lung, and Blood Institute Dynamic Registry, we evaluated 2-year outcomes of diabetic patients undergoing percutaneous coronary interventions with SES (n=677) and PES (n=328). Clinical and demographic characteristics, including age, body mass index, insulin use, left ventricular function, and aspirin/clopidogrel use postprocedure, did not differ significantly between the groups except that PES-treated patients had a greater frequency of hypertension and hyperlipidemia. At the 2-year follow-up, no significant differences were observed between PES and SES with regard to safety or efficacy end points. PES- and SES-treated patients had similar rates of death (10.7% versus 8.2%, P=0.20), death and myocardial infarction (14.9% versus 13.6%, P=0.55), repeat revascularization (14.8% versus 17.8%, P=0.36), and stent thrombosis (1.3% versus 1.3%, P=0.95). After adjustment, no significant differences between the 2 stent types in any outcome were observed. PES and SES are equally efficacious and have similar safety profiles in diabetic patients undergoing percutaneous coronary interventions in clinical practice.
Stone, Orrin J; Biette, Kelly M; Murphy, Patrick J M
2014-01-01
Hydrophobic interaction chromatography (HIC) most commonly requires experimental determination (i.e., scouting) in order to select an optimal chromatographic medium for purifying a given target protein. Neither a two-step purification of untagged green fluorescent protein (GFP) from crude bacterial lysate using sequential HIC and size exclusion chromatography (SEC), nor HIC column scouting elution profiles of GFP, have been previously reported. Bacterial lysate expressing recombinant GFP was sequentially adsorbed to commercially available HIC columns containing butyl, octyl, and phenyl-based HIC ligands coupled to matrices of varying bead size. The lysate was fractionated using a linear ammonium phosphate salt gradient at constant pH. Collected HIC eluate fractions containing retained GFP were then pooled and further purified using high-resolution preparative SEC. Significant differences in presumptive GFP elution profiles were observed using in-line absorption spectrophotometry (A395) and post-run fluorimetry. SDS-PAGE and western blot demonstrated that fluorometric detection was the more accurate indicator of GFP elution in both HIC and SEC purification steps. Comparison of composite HIC column scouting data indicated that a phenyl ligand coupled to a 34 µm matrix produced the highest degree of target protein capture and separation. Conducting two-step protein purification using the preferred HIC medium followed by SEC resulted in a final, concentrated product with >98% protein purity. In-line absorbance spectrophotometry was not as precise of an indicator of GFP elution as post-run fluorimetry. These findings demonstrate the importance of utilizing a combination of detection methods when evaluating purification strategies. GFP is a well-characterized model protein, used heavily in educational settings and by researchers with limited protein purification experience, and the data and strategies presented here may aid in development other of HIC-compatible protein purification schemes.
Improvement of band gap profile in Cu(InGa)Se{sub 2} solar cells through rapid thermal annealing
DOE Office of Scientific and Technical Information (OSTI.GOV)
Chen, D.S.; College of Mathematics and Physics, Shanghai University of Electric Power, Shanghai, 200090; Yang, J.
Highlights: • Proper RTA treatment can effectively optimize band gap profile to more expected level. • Inter-diffusion of atoms account for the improvement of the graded band gap profile. • The variation of the band gap profile created an absolute gain in the efficiency by 1.22%. - Abstract: In the paper, the effect of rapid thermal annealing on non-optimal double-graded band gap profiles was investigated by using X-ray photoelectron spectroscopy and capacitance–voltage measurement techniques. Experimental results revealed that proper rapid thermal annealing treatment can effectively improve band gap profile to more optimal level. The annealing treatment could not only reducemore » the values of front band gap and minimum band gap, but also shift the position of the minimum band gap toward front electrode and enter into space charge region. In addition, the thickness of Cu(InGa)Se{sub 2} thin film decreased by 25 nm after rapid thermal annealing treatment. All of these modifications were attributed to the inter-diffusion of atoms during thermal treatment process. Simultaneously, the variation of the band gap profile created an absolute gain in the efficiency by 1.22%, short-circuit current density by 2.16 mA/cm{sup 2} and filled factor by 3.57%.« less
Identification of proteinaceous material in the bone of the dinosaur Iguanodon.
Embery, Graham; Milner, Angela C; Waddington, Rachel J; Hall, Rachel C; Langley, Martin S; Milan, Anna M
2003-01-01
This study has directed attention at the search for bone-related proteins in an extract of demineralized rib bone of the 120 mya Iguanodon. The inner compact bone was demineralized and the GuCl extract resolved into 11 fractions using anion exchange chromatography, which all contained silver-reactive proteins with various amino acid profiles. Two specific fractions, iv and xi, revealed characteristics typical of contemporary phosphoproteins and proteoglycans, respectively. Fraction iv, 43-57 kDa, contained a high ratio of aspartate and serine, although no phosphate was discernable. Fraction xi contained a band of 41-47 kDa and was rich in chondroitin sulphate and hyaluronan. In addition an early eluting fraction was immunoreactive with an antibody against osteocalcin. A cancellous bone fraction from the same bone sample was also analyzed using N-terminal sequencing and revealed potential similarities with cystatin. While we do not claim to have identified the presence of intact proteins, this study has value in demonstrating that extruded extracellular matrix is protected by its capacity to induce mineralization, which subsequently is important in conserving detectable protein products in ancient skeletal tissues.
Ion exchange purification of scandium
Herchenroeder, Laurie A.; Burkholder, Harvey R.
1990-10-23
An improvement in purification of scandium through ion exchange chromatography is disclosed in which the oxidation potential of the eluting solution is altered by the addition of potassium chlorate or ammonium chloride so that removal of contaminants is encouraged. The temperature, pH and concentration of the eluent HEDTA are controlled in order to maintain the scandium in the column while minimizing dilution of the scandium band. Recovery of scandium is improved by pumping dilute scandium over the column prior to stripping the scandium and precipitation. This eliminates the HEDTA ion and other monovalent cations contaminating the scandium band. This method maximizes recovery of scandium while maintaining purity.
Ion exchange purification of scandium
Herchenroeder, L.A.; Burkholder, H.R.
1990-10-23
An improvement in purification of scandium through ion exchange chromatography is disclosed in which the oxidation potential of the eluting solution is altered by the addition of potassium chlorate or ammonium chloride so that removal of contaminants is encouraged. The temperature, pH and concentration of the eluent HEDTA are controlled in order to maintain the scandium in the column while minimizing dilution of the scandium band. Recovery of scandium is improved by pumping dilute scandium over the column prior to stripping the scandium and precipitation. This eliminates the HEDTA ion and other monovalent cations contaminating the scandium band. This method maximizes recovery of scandium while maintaining purity. 2 figs.
Stoll, Dwight R; Sajulga, Ray W; Voigt, Bryan N; Larson, Eli J; Jeong, Lena N; Rutan, Sarah C
2017-11-10
An important research direction in the continued development of two-dimensional liquid chromatography (2D-LC) is to improve the detection sensitivity of the method. This is especially important in applications where injection of large volumes of effluent from the first dimension ( 1 D) column into the second dimension ( 2 D) column leads to severe 2 D peak broadening and peak shape distortion. For example, this is common when coupling two reversed-phase columns and the organic solvent content of the 1 D mobile phase overwhelms the 2 D column with each injection of 1 D effluent, leading to low resolution in the second dimension. In a previous study we validated a simulation approach based on the Craig distribution model and adapted from the work of Czok and Guiochon [1] that enabled accurate simulation of simple isocratic and gradient separations with very small injection volumes, and isocratic separations with mismatched injection and mobile phase solvents [2]. In the present study we have extended this simulation approach to simulate separations relevant to 2D-LC. Specifically, we have focused on simulating 2 D separations where gradient elution conditions are used, there is mismatch between the sample solvent and the starting point in the gradient elution program, injection volumes approach or even exceed the dead volume of the 2 D column, and the extent of sample loop filling is varied. To validate this simulation we have compared results from simulations and experiments for 101 different conditions, including variation in injection volume (0.4-80μL), loop filling level (25-100%), and degree of mismatch between sample organic solvent and the starting point in the gradient elution program (-20 to +20% ACN). We find that that the simulation is accurate enough (median errors in retention time and peak width of -1.0 and -4.9%, without corrections for extra-column dispersion) to be useful in guiding optimization of 2D-LC separations. However, this requires that real injection profiles obtained from 2D-LC interface valves are used to simulate the introduction of samples into the 2 D column. These profiles are highly asymmetric - simulation using simple rectangular pulses leads to peak widths that are far too narrow under many conditions. We believe the simulation approach developed here will be useful for addressing practical questions in the development of 2D-LC methods. Copyright © 2017 Elsevier B.V. All rights reserved.
Moreno, Raul; Martin-Reyes, Roberto; Jimenez-Valero, Santiago; Sanchez-Recalde, Angel; Galeote, Guillermo; Calvo, Luis; Plaza, Ignacio; Lopez-Sendon, Jose-Luis
2011-04-01
The use of drug-eluting stents (DES) in unfavourable patients has been associated with higher rates of clinical complications and stent thrombosis, and because of that concerns about the use of DES in high-risk settings have been raised. This study sought to demonstrate that the clinical benefit of DES increases as the risk profile of the patients increases. A meta-regression analysis from 31 randomized trials that compared DES and bare-metal stents, including overall 12,035 patients, was performed. The relationship between the clinical benefit of using DES (number of patients to treat [NNT] to prevent one episode of target lesion revascularization [TLR]), and the risk profile of the population (rate of TLR in patients allocated to bare-metal stents) in each trial was evaluated. The clinical benefit of DES increased as the risk profile of each study population increased: NNT for TLR=31.1-1.2 (TLR for bare-metal stents); p<0.001. The use of DES was safe regardless of the risk profile of each study population, since the effect of DES in mortality, myocardial infarction, and stent thrombosis, was not adversely affected by the risk profile of each study population (95% confidence interval for β value 0.09 to 0.11, -0.12 to 0.19, and -0.03 to-0.15 for mortality, myocardial infarction, and stent thrombosis, respectively). The clinical benefit of DES increases as the risk profile of the patients increases, without affecting safety. Copyright © 2009 Elsevier Ireland Ltd. All rights reserved.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Gritti, Fabrice; Guiochon, Georges A
2009-01-01
We measured overloaded band profiles for a series of nine compounds (phenol, caffeine, 3-phenyl 1-propanol, 2-phenylbutyric acid, amphetamine, aniline, benzylamine, p-toluidine, and procainamidium chloride) on columns packed with four different C{sub 18}-bonded packing materials: XTerra-C{sub 18}, Gemini-C{sub 18}, Luna-C{sub 18}(2), and Halo-C{sub 18}, using buffered methanol-water mobile phases. The {sub W}{sup S}pH of the mobile phase was increased from 2.6 to 11.3. The buffer concentration (either phosphate, acetate, or carbonate buffers) was set constant at values below the maximum concentration of the sample in the band. The influence of the surface chemistry of the packing material on the retention andmore » the shape of the peaks was investigated. Adsorbents having a hybrid inorganic/organic structure tend to give peaks exhibiting moderate or little tailing. The retention and the shape of the band profiles can easily be interpreted at {sub W}{sup S}pHs that are well above or well below the {sub W}{sup S}pK{sub a} of the compound studied. In contrast, the peak shapes in the intermediary pH range (i.e., close to the compound {sub W}{sup S}pK{sub a}) have rarely been studied. These shapes reveal the complexity of the competitive adsorption behavior of couples of acido-basic conjugated compounds at {sub W}{sup S}pHs that are close to their {sub W}{sup S}pK{sub a}. They also reveal the role of the buffer capacity on the resulting peak shape. With increasing {sub W}{sup S}pH, the overloaded profiles are first langmuirian (isotherm type I) at low {sub W}{sup S}pHs, they become S-shaped (isotherm type II), then anti-langmuirian (isotherm type III), S-shaped again at intermediate {sub W}{sup S}pHs, and finally return to a langmuirian shape at high {sub W}{sup S}pHs. A new general adsorption isotherm model that takes into account the dissociation equilibrium of conjugated acidic and basic species in the bulk mobile phase accounts for these transient band shapes. An excellent agreement was achieved between experimental profiles and those calculated with a two-sites adsorption isotherm model at all {sub W}{sup S}pHs. The neutral species adsorbs strongly on a first type of sites that have a high density while the ionic species adsorb preferentially on a second type of sites that have a very low density. The evolution of the peak shape when the {sub W}{sup S}pH changes from acidic to basic is well explained by the weak buffer capacity of the mobile phase used compared to the concentration of the eluted compounds.« less
Measurements and Simulations of Nadir-Viewing Radar Returns from the Melting Layer at X- and W-Bands
NASA Technical Reports Server (NTRS)
Liao, Liang; Meneghini, Robert; Tian, Lin; Heymsfield, Gerald M.
2010-01-01
Simulated radar signatures within the melting layer in stratiform rain, namely the radar bright band, are checked by means of comparisons with simultaneous measurements of the bright band made by the EDOP (X-band) and CRS (W-band) airborne Doppler radars during the CRYSTAL-FACE campaign in 2002. A stratified-sphere model, allowing the fractional water content to vary along the radius of the particle, is used to compute the scattering properties of individual melting snowflakes. Using the effective dielectric constants computed by the conjugate gradient-fast Fourier transform (CGFFT) numerical method for X and W bands, and expressing the fractional water content of melting particle as an exponential function in particle radius, it is found that at X band the simulated radar bright-band profiles are in an excellent agreement with the measured profiles. It is also found that the simulated W-band profiles usually resemble the shapes of the measured bright-band profiles even though persistent offsets between them are present. These offsets, however, can be explained by the attenuation caused by cloud water and water vapor at W band. This is confirmed by the comparisons of the radar profiles made in the rain regions where the un-attenuated W-band reflectivity profiles can be estimated through the X- and W band Doppler velocity measurements. The bright-band model described in this paper has the potential to be used effectively for both radar and radiometer algorithms relevant to the TRMM and GPM satellite missions.
Trapp, Oliver
2010-02-12
Highly efficient and sophisticated separation techniques are available to analyze complex compound mixtures with superior sensitivities and selectivities often enhanced by a 2nd dimension, e.g. a separation technique or spectroscopic and spectrometric techniques. For enantioselective separations numerous chiral stationary phases (CSPs) exist to cover a broad range of chiral compounds. Despite these advances enantioselective separations can become very challenging for mixtures of stereolabile constitutional isomers, because the on-column interconversion can lead to completely overlapping peak profiles. Typically, multidimensional separation techniques, e.g. multidimensional GC (MDGC), using an achiral 1st separation dimension and transferring selected analytes to a chiral 2nd separation are the method of choice to approach such problems. However, this procedure is very time consuming and only predefined sections of peaks can be transferred by column switching to the second dimension. Here we demonstrate for stereolabile 1,2-dialkylated diaziridines a technique to experimentally deconvolute overlapping gas chromatographic elution profiles of constitutional isomers based on multiple-reaction-monitoring MS (MRM-MS). The here presented technique takes advantage of different fragmentation probabilities and pathways to isolate the elution profile of configurational isomers. Copyright 2009 Elsevier B.V. All rights reserved.
Soares, Rafael Dutra; Welke, Juliane Elisa; Nicolli, Karine Primieri; Zanus, Mauro; Caramão, Elina Bastos; Manfroi, Vitor; Zini, Cláudia Alcaraz
2015-09-15
This study reports, for the first time, the main changes that occur with some important aroma compounds of Moscatel sparkling wines during winemaking, measured using headspace solid-phase microextraction, one-dimensional and comprehensive two-dimensional gas chromatography (GC×GC) with mass spectrometry detection (MS). The best conditions of volatile extraction included the use of PDMS/DVB fibre, 2mL of wine, 30% of NaCl, 40°C for 30min. The chromatographic profile of sparkling wines showed decreasing amounts of monoterpenes (limonene, 4-terpineol, terpinolene, citronellol, α-terpineol, linalool, hotrienol, and nerol oxide), increasing amounts of esters (terpenyl esters, ethyl octanoate, ethyl decanoate and hexyl acetate) and alcohols (1-nonanol and 2-phenylethanol). Sixty-nine compounds co-eluted in the first dimension; only six co-eluted in the second dimension. GC×GC/TOFMS allows more detailed study of the volatile profile of sparkling wines. Copyright © 2015 Elsevier Ltd. All rights reserved.
Ravald, L; Fornstedt, T
2001-01-26
The bi-Langmuir equation has recently been proven essential to describe chiral chromatographic surfaces and we therefore investigated the accuracy of the elution by characteristic points method (ECP) for estimation of bi-Langmuir isotherm parameters. The ECP calculations was done on elution profiles generated by the equilibrium-dispersive model of chromatography for five different sets of bi-Langmuir parameters. The ECP method generates two different errors; (i) the error of the ECP calculated isotherm and (ii) the model error of the fitting to the ECP isotherm. Both errors decreased with increasing column efficiency. Moreover, the model error was strongly affected by the weight of the bi-Langmuir function fitted. For some bi-Langmuir compositions the error of the ECP calculated isotherm is too large even at high column efficiencies. Guidelines will be given on surface types to be avoided and on column efficiencies and loading factors required for adequate parameter estimations with ECP.
Coriolano, Marília Cavalcanti; Silva, Cynarha Daysy Cardoso da; Melo, Cristiane Moutinho Lagos de; Bezerra, Ranilson de Souza; Santos, Athiê Jorge Guerra; Pereira, Valéria Rêgo Alves; Coelho, Luana Cassandra Breitenbach Barroso
2012-11-01
This work reports the isolation of a serum lectin from cobia fish (Rachycentron canadum) named RcaL. Immunomodulatory activity on mice splenocyte experimental cultures through cytotoxic assays and cytokine production were also performed. RcaL was obtained through precipitation with ammonium sulphate and affinity chromatography on a Concanavalin A-Sepharose 4B column. The ammonium sulphate fraction F3 showed the highest specific hemagglutinating activity and was applied to affinity chromatography. The lectin was eluted with methyl-α-D-mannopyranoside. RcaL showed highest affinity for methyl-α-D-mannopyranoside and D-mannose; eluted fractions of RcaL agglutinated rabbit erythrocytes (titre, 128(-1)) retained 66 % of chromatographed lectin activity, and the obtained purification factor was 1.14. Under reducing conditions, a polypeptide band of 19.2 kDa was revealed in sodium dodecyl sulphate polyacrylamide gel electrophoresis (PAGE). PAGE confirmed RcaL as an acidic protein revealed in a single band. Cytotoxic and immunomodulatory assays with RcaL in mice splenocyte cultures showed that the lectin was not cytotoxic and induced higher interferon gamma and nitric oxide production in splenocyte cultures. Purified RcaL induced preferential Th1 response, suggesting that it acts as an immunomodulatory compound.
Aryal, Uma K.; Olson, Douglas J.H.; Ross, Andrew R.S.
2008-01-01
Although widely used in proteomics research for the selective enrichment of phosphopeptides from protein digests, immobilized metal-ion affinity chromatography (IMAC) often suffers from low specificity and differential recovery of peptides carrying different numbers of phosphate groups. By systematically evaluating and optimizing different loading, washing, and elution conditions, we have developed an efficient and highly selective procedure for the enrichment of phosphopeptides using a commercially available gallium(III)-IMAC column (PhosphoProfile, Sigma). Phosphopeptide enrichment using the reagents supplied with the column is incomplete and biased toward the recovery and/or detection of smaller, singly phosphorylated peptides. In contrast, elution with base (0.4 M ammonium hydroxide) gives efficient and balanced recovery of both singly and multiply phosphorylated peptides, while loading peptides in a strong acidic solution (1% trifluoracetic acid) further increases selectivity toward phosphopeptides, with minimal carryover of nonphosphorylated peptides. 2,5-Dihydroxybenzoic acid, a matrix commonly used when analyzing phosphopeptides by matrix-assisted laser desorption/ionization mass spectrometry was also evaluated as an additive in loading and eluting solvents. Elution with 50% acetonitrile containing 20 mg/mL dihydroxybenzoic acid and 1% phosphoric acid gave results similar to those obtained using ammonium hydroxide as the eluent, although the latter showed the highest specificity for phosphorylated peptides. PMID:19183793
Discontinuous pH gradient-mediated separation of TiO2-enriched phosphopeptides
Park, Sung-Soo; Maudsley, Stuart
2010-01-01
Global profiling of phosphoproteomes has proven a great challenge due to the relatively low stoichiometry of protein phosphorylation and poor ionization efficiency in mass spectrometers. Effective, physiologically-relevant, phosphoproteome research relies on the efficient phosphopeptide enrichment from complex samples. Immobilized metal affinity chromatography and titanium dioxide chromatography (TOC) can greatly assist selective phosphopeptide enrichment. However, the complexity of resultant enriched samples is often still high, suggesting that further separation of enriched phosphopeptides is required. We have developed a pH-gradient elution technique for enhanced phosphopeptide identification in conjunction with TOC. Using this process, we have demonstrated its superiority to the traditional ‘one-pot’ strategies for differential protein identification. Our technique generated a highly specific separation of phosphopeptides by an applied pH-gradient between 9.2 and 11.3. The most efficient elution range for high-resolution phosphopeptide separation was between pH 9.2 and 9.4. High-resolution separation of multiply-phosphorylated peptides was primarily achieved using elution ranges > pH 9.4. Investigation of phosphopeptide sequences identified in each pH fraction indicated that phosphopeptides with phosphorylated residues proximal to acidic residues, including glutamic acid, aspartic acid, and other phosphorylated residues, were preferentially eluted at higher pH values. PMID:20946866
Renkoğlu, Pelin; Çelebier, Mustafa; Arıca-Yegin, Betül
2015-05-01
Cocrystals have recently gained importance in the pharmaceutical industry. In this study, olanzapine and carbamazepine cocrystals were synthesized by using nicotinamide as cocrystal forming agent to achieve improvements in the physicochemical characteristics of the active ingredients. An HPLC method was developed to determine the amount, thus, the stoichiometric ratios of olanzapine and carbamazepine in the synthesized cocrystals. Olanzapine:nicotinamide and olanzapine tablet formulations were prepared and the developed HPLC method was applied successfully in order to compare the dissolution profiles of these formulations. An ACE 5 CN, 25 cm × 4.6 mm, 5 µm column was used and a gradient elution program was performed for simultaneous determination of olanzapine, carbamazepine and nicotinamide. Phosphate buffer (pH 5.0, 25 mM) and methanol was used in a ratio from 80:20 to 70:30 while the flow rate was 1 mL min(-1) for the elution of the compounds within 12 min. In conclusion, two different aims were achieved, the first one was to indicate the stoichiometric ratios of the active ingredients olanzapine and carbamazepine with nicotinamide in their cocrystals, and the second one was the comparison of the dissolution profiles of the olanzapine and olanzapine:nicotinamide cocrystal formulations. It was found that the cocrystal formulation with nicotinamide improved the dissolution profile of olanzapine.
Miswan, Zulaika; Lukman, Siti Khadijah; Abd Majid, Fadzilah Adibah; Loke, Mun Fai; Saidin, Syafiqah; Hermawan, Hendra
2016-12-30
Active ingredients of ginsenoside, Rg1 and Re, are able to inhibit the proliferation of vascular smooth muscle cells and promote the growth of vascular endothelial cells. These capabilities are of interest for developing a novel drug-eluting stent to potentially solve the current problem of late-stent thrombosis and poor endotheliazation. Therefore, this study was aimed to incorporate ginsenoside into degradable coating of poly(lactic-co-glycolic acid) (PLGA). Drug mixture composed of ginseng extract and 10% to 50% of PLGA (xPLGA/g) was coated on electropolished stainless steel 316L substrate by using a dip coating technique. The coating was characterized principally by using attenuated total reflectance-Fourier transform infrared spectroscopy, scanning electron microscopy and contact angle analysis, while the drug release profile of ginsenosides Rg1 and Re was determined by using mass spectrometry at a one month immersion period. Full and homogenous coating coverage with acceptable wettability was found on the 30PLGA/g specimen. All specimens underwent initial burst release dependent on their composition. The 30PLGA/g and 50PLGA/g specimens demonstrated a controlled drug release profile having a combination of diffusion- and swelling-controlled mechanisms of PLGA. The study suggests that the 30PLGA/g coated specimen expresses an optimum composition which is seen as practicable for developing a controlled release drug-eluting stent. Copyright © 2016 Elsevier B.V. All rights reserved.
Antibiotic eluting clay mineral (Laponite®) for wound healing application: an in vitro study.
Ghadiri, M; Chrzanowski, W; Rohanizadeh, R
2014-11-01
Different materials in form of sponge, hydrogel and film have been developed and formulated for treating and dressing burn wounds. In this study, the potential of Laponite, a gel forming clay, in combination with an antimicrobial agent (mafenide), as a wound dressing material was tested in vitro. Laponite/mafenide (Lap/Maf) hydrogel was formulated in three different ratios of Lap/Maf 1:1, 1:2, 1:3. Laponite/mafenide/alginate (Lap/Maf/Alg) film was also formulated by combining Lap/Maf gel (1:1) with alginate. Intercalation rate of mafenide into the layers of Laponite nanoparticles and physico-chemical properties, including wound dressing characteristics of materials were studied using various analytical methods. Furthermore, the degradation of materials and the release profile of mafenide were investigated in simulated wound exudates fluid and antibacterial effectiveness of the eluted mafenide was tested on a range of bacterial species. The cytotoxicity of materials was also evaluated in skin fibroblast culture. The results showed that mafenide molecules were intercalated between the nano-sized layers of Laponite. The eluted mafenide showed active antibacterial effects against all three tested bacteria. All intercalated mafenide released from Lap/Maf 1:1 and 1:2 gel formulations and nearly 80% release from 1:3 formulation during test period. No significant difference was observed in release profile of mafenide between Lap/Maf/Alg film and Lap/Maf formulations. Wound dressing tests on Lap/Maf/Alg film showed it is a breathable dressing and has capacity to absorb wound exudates. The study showed that prepared Lap/Maf composite has the potential to be used as an antibiotic eluting gel or film for wound healing application. Additionally, Laponite has shown benefits in wound healing processes by releasing Mg(2+) ions and thereby reducing the cytotoxic effect of mafenide on fibroblast cells.
Murphy, Patrick J. M.
2014-01-01
Background Hydrophobic interaction chromatography (HIC) most commonly requires experimental determination (i.e., scouting) in order to select an optimal chromatographic medium for purifying a given target protein. Neither a two-step purification of untagged green fluorescent protein (GFP) from crude bacterial lysate using sequential HIC and size exclusion chromatography (SEC), nor HIC column scouting elution profiles of GFP, have been previously reported. Methods and Results Bacterial lysate expressing recombinant GFP was sequentially adsorbed to commercially available HIC columns containing butyl, octyl, and phenyl-based HIC ligands coupled to matrices of varying bead size. The lysate was fractionated using a linear ammonium phosphate salt gradient at constant pH. Collected HIC eluate fractions containing retained GFP were then pooled and further purified using high-resolution preparative SEC. Significant differences in presumptive GFP elution profiles were observed using in-line absorption spectrophotometry (A395) and post-run fluorimetry. SDS-PAGE and western blot demonstrated that fluorometric detection was the more accurate indicator of GFP elution in both HIC and SEC purification steps. Comparison of composite HIC column scouting data indicated that a phenyl ligand coupled to a 34 µm matrix produced the highest degree of target protein capture and separation. Conclusions Conducting two-step protein purification using the preferred HIC medium followed by SEC resulted in a final, concentrated product with >98% protein purity. In-line absorbance spectrophotometry was not as precise of an indicator of GFP elution as post-run fluorimetry. These findings demonstrate the importance of utilizing a combination of detection methods when evaluating purification strategies. GFP is a well-characterized model protein, used heavily in educational settings and by researchers with limited protein purification experience, and the data and strategies presented here may aid in development other of HIC-compatible protein purification schemes. PMID:25254496
Titanium-nitride-oxide-coated coronary stents: insights from the available evidence.
Karjalainen, Pasi P; Nammas, Wail
2017-06-01
Coating of stent surface with a biocompatible material is suggested to improve stent safety profile. A proprietary process was developed to coat titanium-nitride-oxide on the stent surface, based on plasma technology that uses the nano-synthesis of gas and metal. Preclinical in vitro and in vivo investigation confirmed blood compatibility of titanium (nitride-) oxide films. Titanium-nitride-oxide-coated stents demonstrated a better angiographic outcome, compared with bare-metal stents at mid-term follow-up; however, they failed to achieve non-inferiority for angiographic outcome versus second-generation drug-eluting stents. Observational studies showed adequate clinical outcome at mid-term follow-up. Non-randomized studies showed an outcome of titanium-nitride-oxide-coated stents comparable to - or better than - first-generation drug-eluting stents at long-term follow-up. Two randomized controlled trials demonstrated comparable efficacy outcome, and a better safety outcome of titanium-nitride-oxide-coated stents versus drug-eluting stents at long-term follow-up. Evaluation by optical coherence tomography at mid-term follow-up revealed better neointimal strut coverage associated with titanium-nitride-oxide-coated stents versus drug-eluting stents; yet, neointimal hyperplasia thickness was greater. Key messages Stents coated with titanium-nitride-oxide demonstrated biocompatibility in preclinical studies: they inhibit platelet and fibrin deposition, and reduce neointimal growth. In observational and non-randomized studies, titanium-nitride-oxide-coated stents were associated with adequate safety and efficacy outcome. In randomized trials of patients with acute coronary syndrome, titanium-nitride-oxide-coated stents were associated with a better safety outcome, compared with drug-eluting stents; efficacy outcome was comparable.
Gonçalves, Tatiana Siqueira; de Menezes, Luciane Macedo; Ribeiro, Luciele Gonzaga; Lindholz, Catieli Gobetti; Medina-Silva, Renata
2014-01-01
The aim of this study was to evaluate the cytotoxicity induced by orthodontic bands through survival tests on Saccharomyces cerevisiae, a microorganism that presents several genetic and biochemical characteristics similar to human cells. Three groups of bands were evaluated: silver soldered (SSB), laser soldered (LSB), and bands without any solder (WSB). Yeast cells were directly exposed to the bands and indirectly, when a previous elution of the metals in artificial saliva was performed. The negative control was composed of yeast cells or artificial saliva not exposed to any kind of metal. In the direct exposure experiments, all tested groups of bands induced a slight reduction in yeast viability compared to the control. This effect was more intense for the SSB, although not statistically significant. For the indirect exposure experiments, the SSB induced a statistically significant decrease in cell viability compared to the LSB. There were no significant differences between the survival rates of the negative control and the LSB group in both direct and saliva tests. SSBs were cytotoxic, whilst LSBs were not, confirming that laser soldering may be a more biocompatible alternative for use in connecting wires to orthodontic appliances. PMID:24511527
Wharton, Christopher W.
1974-01-01
1. Purified stem bromelain (EC 3.4.22.4) was eluted from Sephadex G-100 as a single peak. The specific activity across the elution peak was approximately constant towards p-nitrophenyl hippurate but increased with elution volume with N2-benzoyl-l-arginine ethyl ester as substrate. 2. The apparent molecular weight, determined by elution analysis on Sephadex G-100, is 22500±1500, an anomalously low value. 3. Purified stem bromelain was eluted from CM-cellulose CM-32 as a single peak and behaved as a single species during column electrophoresis on Sephadex G-100. 4. Purified stem bromelain migrates as a single band during polyacrylamide-gel electrophoresis under a wide variety of conditions. 5. The molecular weight determined by polyacrylamide-gel electrophoresis in the presence of sodium dodecyl sulphate is 28500±1000. 6. Sedimentation-velocity and equilibrium-ultracentrifugation experiments, under a variety of conditions, indicate that bromelain is an apparently homogeneous single peptide chain of mol.wt. 28400±1400. 7. The N-terminal amino acid composition is 0.64±0.04mol of valine and 0.36±0.04mol of alanine per mol of enzyme of mol.wt. 28500. (The amino acid recovery of the cyanate N-terminal amino acid analysis was standardized by inclusion of carbamoyl-norleucine at the cyclization stage.) 8. The pH-dependence of the Michaelis parameters of the bromelain-catalysed hydrolysis of N-benzyloxycarbonyl-l-phenylalanyl-l-serine methyl ester was determined. 9. The magnitude and pH-dependence of the Michaelis parameters have been interpreted in terms of the mechanism of the enzyme. 10. The enzyme is able to bind N-benzyloxycarbonyl-l-phenylalanyl-l-serine methyl ester relatively strongly but seems unable to make use of the binding energy to promote catalysis. PMID:4462742
Thomas, M P; Topham, C M; Kowlessur, D; Mellor, G W; Thomas, E W; Whitford, D; Brocklehurst, K
1994-01-01
Chymopapain M, the monothiol cysteine proteinase component of the chymopapain band eluted after chymopapains A and B in cation-exchange chromatography, was isolated from the dried latex of Carica papaya and characterized by kinetic and chromatographic analysis. This late-eluted chymopapain is probably a component of the cysteine proteinase fraction of papaya latex discovered by Schack [(1967) Compt. Rend. Trav. Lab. Carlsberg 36, 67-83], named papaya peptidase B by Lynn [(1979) Biochim. Biophys. Acta 569, 193-201] and partially characterized by Polgár [(1981) Biochim. Biophys. Acta 658, 262-269] and is the enzyme with unusual specificity characteristics (papaya proteinase IV) that Buttle, Kembhavi, Sharp, Shute, Rich and Barrett [Biochem. J. (1989) 261, 469-476] claimed to be a previously undetected cysteine proteinase eluted from a cation-exchange column near to the early-eluted chymopapains. A study of the time-dependent chromatographic consequences of thiol-dependent proteolysis of the components of papaya latex is reported. Chymopapain M was isolated by (i) affinity chromatography followed by separation from papain using cation-exchange f.p.l.c. on a Mono S HR5/5 column and (ii) cation-exchange chromatography followed by an unusual variant of covalent chromatography by thiol-disulphide interchange. The existence in chymopapain M of a nucleophilic interactive Cys/His catalytic-site system analogous to those in papain (EC 3.4.22.2) and other cysteine proteinases was deduced from the characteristics shape of the pH-second-order rate constant (k) profiles for its reactions with 2,2'-dipyridyl disulphide and ethyl 2-pyridyl disulphide. Analysis of the pH-k data for the reactions of chymopapain M with the 2-pyridyl disulphides and with 4,4'-dipyridyl disulphide permits the assignment of molecular pKa values of 3.4 and 8.7 to the formation and subsequent dehydronation of the Cys-S-/His-Im+H state of the catalytic site and reveals three other kinetically influential ionizations with pKa values 3.4, 4.3 and 5.6. The pH-dependences of kcat./Km for the hydrolysis of N-acetyl-L-Phe-Gly-4-nitroanilide at 25.0 degrees C and I0.1 M catalysed by chymopapain M and papain were determined. For both enzymes, little catalytic activity (5-7% of the maximal) develops consequent on formation of the catalytic site Cys-S-/His-Im+H ion-pair state (across pKa 3.4 for both enzymes). For papain, full expression of Kcat./Km for the uncharged substrate requires only the additional hydronic dissociation with pKa 4.2. By contrast, full expression of kcat./Km for chymopapain M requires additional hydronic dissociation with pKa values of 4.3 and 5.6.(ABSTRACT TRUNCATED AT 400 WORDS) Images Figure 6 Figure 7 PMID:8010964
Williams, Christopher
2012-11-06
This data was collected by the NOAA 449-MHz and 2.8-GHz profilers in support of the Department of Energy (DOE) and NASA sponsored Mid-latitude Continental Convective Cloud Experiment (MC3E). The profiling radars were deployed in Northern Oklahoma at the DOE Atmospheric Radiation Mission (ARM) Southern Great Plans (SGP) Central Facility from 22 April through 6 June 2011. NOAA deployed three instruments: a Parsivel disdrometer, a 2.8-GHz profiler, and a 449-MHz profiler. The parasivel provided surface estimates of the raindrop size distribution and is the reference used to absolutely calibrate the 2.8 GHz profiler. The 2.8-GHz profiler provided unattenuated reflectivity profiles of the precipitation. The 449-MHz profiler provided estimates of the vertical air motion during precipitation from near the surface to just below the freezing level. By using the combination of 2.8-GHz and 449-MHz profiler observations, vertical profiles of raindrop size distributions can be retrieved. The profilers are often reference by their frequency band: the 2.8-GHz profiler operates in the S-band and the 449-MHz profiler operates in the UHF band. The raw observations are available as well as calibrated spectra and moments. This document describes how the instruments were deployed, how the data was collected, and the format of the archived data.
Low-resolution structure of Drosophila translin
Kumar, Vinay; Gupta, Gagan D.
2012-01-01
Crystals of native Drosophila melanogaster translin diffracted to 7 Å resolution. Reductive methylation of the protein improved crystal quality. The native and methylated proteins showed similar profiles in size-exclusion chromatography analyses but the methylated protein displayed reduced DNA-binding activity. Crystals of the methylated protein diffracted to 4.2 Å resolution at BM14 of the ESRF synchrotron. Crystals with 49% solvent content belonged to monoclinic space group P21 with eight protomers in the asymmetric unit. Only 2% of low-resolution structures with similar low percentage solvent content were found in the PDB. The crystal structure, solved by molecular replacement method, refined to Rwork (Rfree) of 0.24 (0.29) with excellent stereochemistry. The crystal structure clearly shows that drosophila protein exists as an octamer, and not as a decamer as expected from gel-filtration elution profiles. The similar octameric quaternary fold in translin orthologs and in translin–TRAX complexes suggests an up-down dimer as the basic structural subunit of translin-like proteins. The drosophila oligomer displays asymmetric assembly and increased radius of gyration that accounts for the observed differences between the elution profiles of human and drosophila proteins on gel-filtration columns. This study demonstrates clearly that low-resolution X-ray structure can be useful in understanding complex biological oligomers. PMID:23650579
Kabir, S
1995-02-01
Jackfruit extracts contain a protein termed jacalin which possesses diverse biological properties. A detailed analysis of its charge properties has been lacking. The present investigation was initiated to study isoelectric properties of jacalin in detail and to isolate a single isoform of jacalin. Jacalin was isolated from jackfruit extracts by affinity chromatography on immunoglobulin-A immobilised to Sepharose 4B. Various techniques such as ion-exchange chromatography, isoelectric focusing (IEF) on polyacrylamide gels and preparative liquid IEF with the Rotofor cell were used. When analysed by IEF on thin layer polyacrylamide gels, jacalin was resolved into 35 bands over a pH range of 5.0-8.5. Upon SDS-PAGE in the second dimension all these charge species gave rise to only two-bands at 12 and 15.4 kDa. The lectin was mostly eluted with 50 and 100 mM sodium chloride when jackfruit extracts were fractionated on an anion-exchange column of DEAE-cellulose. In a single 6 hour run by preparative IEF with the Rotofor cell in the pH range of 3-9.5, it has been possible to isolate pure jacalin fractions containing fewer number of charged isomers. A single jacalin isoform was isolated by subjecting a Rotofor fraction containing fewer charged species to preparative IEF on thin layer polyacrylamide gel and eluting the band of interest from the gel. The isolated jacalin isoform was biologically active as it agglutinated erythrocytes. The study reveals the complexity of jacalin as it exists as multiple charge isomers over a broad pH range. By performing preparative IEF in solution as well as in thin layer polyacrylamide gels, it was possible to isolate a single jacalin isoform with the retention of biological activity.
Highly multiplexed targeted proteomics using precise control of peptide retention time.
Gallien, Sebastien; Peterman, Scott; Kiyonami, Reiko; Souady, Jamal; Duriez, Elodie; Schoen, Alan; Domon, Bruno
2012-04-01
Large-scale proteomics applications using SRM analysis on triple quadrupole mass spectrometers present new challenges to LC-MS/MS experimental design. Despite the automation of building large-scale LC-SRM methods, the increased numbers of targeted peptides can compromise the balance between sensitivity and selectivity. To facilitate large target numbers, time-scheduled SRM transition acquisition is performed. Previously published results have demonstrated incorporation of a well-characterized set of synthetic peptides enabled chromatographic characterization of the elution profile for most endogenous peptides. We have extended this application of peptide trainer kits to not only build SRM methods but to facilitate real-time elution profile characterization that enables automated adjustment of the scheduled detection windows. Incorporation of dynamic retention time adjustments better facilitate targeted assays lasting several days without the need for constant supervision. This paper provides an overview of how the dynamic retention correction approach identifies and corrects for commonly observed LC variations. This adjustment dramatically improves robustness in targeted discovery experiments as well as routine quantification experiments. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Identification and partial purification of pollen allergens from Artemisia princeps.
Park, H S; Hong, C S; Choi, H J; Hahm, K S
1989-12-01
The pollen of Artemisia has been considered as the main late summer-autumn allergen source in this country. To identify its allergenic components, Artemisia princeps pollen extracts were separated by 10% sodium dodecylsulfate polyacrylamide gel electrophoresis (SDS-PAGE), and transferred to nitrocellulose membrane, where IgE binding components were detected by the reaction with sera of twenty Artemisia-allergic patients and 125I-anti-human IgE, sixteen components in the molecular range of 10,000 and 85,000 daltons were detected. Twelve bands bound to IgE from 50% of the sera tested, and two bands (37,000, 23,000 daltons) showed the highest (85%) frequency of IgE-binding in twenty sera tested. When the gel of SDS-PAGE with Artemisia pollen extracts was sliced into 11 allergenic groups (AG) and the protein of each AG was obtained by the gel elution method, the wormwool-RAST inhibition test showed that the AG 10 demonstrated to be the most potent, and the AG 7 was the next. Six AGs showed significant responses (more than 100% of wheal size to histamine, 1 mg/ml) on the skin prick test in more than 50% of the patients tested. It is suggested that electrophoretic transfer analysis with SDS-PAGE may be a valuable method for Artemisia allergen identification, and the possibility of partial purification of allergens by employing gel elution is discussed.
An Empirical Study on Raman Peak Fitting and Its Application to Raman Quantitative Research.
Yuan, Xueyin; Mayanovic, Robert A
2017-10-01
Fitting experimentally measured Raman bands with theoretical model profiles is the basic operation for numerical determination of Raman peak parameters. In order to investigate the effects of peak modeling using various algorithms on peak fitting results, the representative Raman bands of mineral crystals, glass, fluids as well as the emission lines from a fluorescent lamp, some of which were measured under ambient light whereas others under elevated pressure and temperature conditions, were fitted using Gaussian, Lorentzian, Gaussian-Lorentzian, Voigtian, Pearson type IV, and beta profiles. From the fitting results of the Raman bands investigated in this study, the fitted peak position, intensity, area and full width at half-maximum (FWHM) values of the measured Raman bands can vary significantly depending upon which peak profile function is used in the fitting, and the most appropriate fitting profile should be selected depending upon the nature of the Raman bands. Specifically, the symmetric Raman bands of mineral crystals and non-aqueous fluids are best fit using Gaussian-Lorentzian or Voigtian profiles, whereas the asymmetric Raman bands are best fit using Pearson type IV profiles. The asymmetric O-H stretching vibrations of H 2 O and the Raman bands of soda-lime glass are best fit using several Gaussian profiles, whereas the emission lines from a florescent light are best fit using beta profiles. Multiple peaks that are not clearly separated can be fit simultaneously, provided the residuals in the fitting of one peak will not affect the fitting of the remaining peaks to a significant degree. Once the resolution of the Raman spectrometer has been properly accounted for, our findings show that the precision in peak position and intensity can be improved significantly by fitting the measured Raman peaks with appropriate profiles. Nevertheless, significant errors in peak position and intensity were still observed in the results from fitting of weak and wide Raman bands having unnormalized intensity/FWHM ratios lower than 200 counts/cm -1 .
Experimental study on neptunium migration under in situ geochemical conditions
NASA Astrophysics Data System (ADS)
Kumata, M.; Vandergraaf, T. T.
1998-12-01
Results are reported for migration experiments performed with Np under in situ geochemical conditions over a range of groundwater flow rates in columns of crushed rock in a specially designed facility at the 240-level of the Underground Research Laboratory (URL) near Pinawa, Manitoba, Canada. This laboratory is situated in an intrusive granitic rock formation, the Lac du Bonnet batholith. Highly altered granitic rock and groundwater were obtained from a major subhorizontal fracture zone at a depth of 250 m in the URL. The granite was wet-crushed and wet-sieved with groundwater from this fracture zone. The 180-850-μm size fraction was selected and packed in 20-cm long, 2.54-cm in diameter Teflon™-lined stainless steel columns. Approximately 30-ml vols of groundwater containing 3HHO and 237Np were injected into the columns at flow rates of 0.3, 1, and 3 ml/h, followed by elution with groundwater, obtained from the subhorizontal fracture, at the same flow rates, for a period of 95 days. Elution profiles for 3HHO were obtained, but no 237Np was detected in the eluted groundwater. After terminating the migration experiments, the columns were frozen, the column material was removed and cut into twenty 1-cm thick sections and each section was analyzed by gamma spectrometry. Profiles of 237Np were obtained for the three columns. A one-dimensional transport model was fitted to the 3HHO breakthrough curves to obtain flow parameters for this experiment. These flow parameters were in turn applied to the 237Np concentration profiles in the columns to produce sorption and dispersion coefficients for Np. The results show a strong dependence of retardation factors ( Rf) on flow rate. The decrease in the retarded velocity of the neptunium ( Vn) varied over one order of magnitude under the geochemical conditions for these experiments.
Valgimigli, Marco; Patialiakas, Athanasios; Thury, Attila; Colangelo, Salvatore; Campo, Gianluca; Tebaldi, Matteo; Ungi, Imre; Tondi, Stefano; Roffi, Marco; Menozzi, Alberto; de Cesare, Nicoletta; Garbo, Roberto; Meliga, Emanuele; Testa, Luca; Gabriel, Henrique M; Airoldi, Flavio; Ferlini, Marco; Liistro, Francesco; Dellavalle, Antonio; Vranckx, Pascal; Briguori, Carlo
2013-11-01
The use of drug-eluting stent (DES) instead of bare-metal stent (BMS) in patients at high stent thrombosis or bleeding risk as well as in those at low restenosis risk (ie, uncertain DES candidates) remains a matter of debate. Zotarolimus-Eluting Endeavor Sprint stent (E-ZES) (Santa Rosa, CA) is a hydrophilic polymer-based second-generation device with unique drug fast-release profile, which may allow for a shorter dual antiplatelet therapy (DAPT) duration without safety concerns. The primary objective is to assess whether E-ZES implantation followed by a shorter than currently recommended course of DAPT will decrease the incidence of 12-month major adverse cardiovascular events as compared with BMS in undefined DES recipients. Actual duration of DAPT regimen will be dictated by patients' characteristics and not by stent type and, as such, can be as short as 30 days after intervention in both stent groups. The ZEUS study is an open-label randomized clinical trial conducted at 20 clinical sites in Italy, Switzerland, Portugal, and Hungary. With 1,600 individuals, this study will have 85% power to detect a 33% difference in the primary end point consisting of the composite of death, nonfatal myocardial infarction, or target vessel revascularization. The ZEUS trial aims to assess whether the use of E-ZES, followed by a DAPT duration regimen based on patients' characteristics and not by stent type, is superior to conventional BMS implantation in undefined DES recipients who qualify for the presence of high thrombosis, bleeding, or low restenosis risk criteria. © 2013.
Optimization of doxorubicin loading for superabsorbent polymer microspheres: in vitro analysis.
Liu, David M; Kos, Sebastian; Buczkowski, Andrzej; Kee, Stephen; Munk, Peter L; Klass, Darren; Wasan, Ellen
2012-04-01
This study was designed to establish the ability of super-absorbent polymer microspheres (SAP) to actively uptake doxorubicin and to establish the proof of principle of SAP's ability to phase transfer doxorubicin onto the polymer matrix and to elute into buffer with a loading method that optimizes physical handling and elution characteristics. Phase I: 50-100 μm SAP subject to various prehydration methods (normal saline 10 cc, hypertonic saline 4 cc, iodinated contrast 10 cc) or left in their dry state, and combined with 50 mg of clinical grade lyophilized doxorubicin reconstituted with various methods (normal saline 10 cc and 25 cc, sterile water 4 cc, iodinated contrast 5 cc) were placed in buffer and assessed based on loading, handling, and elution utilizing high-performance liquid chromatography (HPLC). Phase II: top two performing methods were subject to loading of doxorubicin (50, 75, 100 mg) in a single bolus (group A) or as a serial loading method (group B) followed by measurement of loading vs. time and elution vs. time. Phase I revealed the most effective loading mechanisms and easiest handling to be dry (group A) vs. normal saline prehydrated (group B) SAP with normal saline reconstituted doxorubicin (10 mg/mL) with loading efficiencies of 83.1% and 88.4%. Phase II results revealed unstable behavior of SAP with 100 mg of doxorubicin and similar loading/elution profiles of dry and prehydrated SAP, with superior handling characteristics of group B SAP at 50 and 75 mg. SAP demonstrates the ability to load and bulk phase transfer doxorubicin at 50 and 75 mg with ease of handling and optimal efficiency through dry loading of SAP.
Optimization of Doxorubicin Loading for Superabsorbent Polymer Microspheres: in vitro Analysis
DOE Office of Scientific and Technical Information (OSTI.GOV)
Liu, David M., E-mail: dave.liu@vch.ca; Kos, Sebastian; Buczkowski, Andrzej
2012-04-15
Purpose: This study was designed to establish the ability of super-absorbent polymer microspheres (SAP) to actively uptake doxorubicin and to establish the proof of principle of SAP's ability to phase transfer doxorubicin onto the polymer matrix and to elute into buffer with a loading method that optimizes physical handling and elution characteristics. Methods: Phase I: 50-100 {mu}m SAP subject to various prehydration methods (normal saline 10 cc, hypertonic saline 4 cc, iodinated contrast 10 cc) or left in their dry state, and combined with 50 mg of clinical grade lyophilized doxorubicin reconstituted with various methods (normal saline 10 cc andmore » 25 cc, sterile water 4 cc, iodinated contrast 5 cc) were placed in buffer and assessed based on loading, handling, and elution utilizing high-performance liquid chromatography (HPLC). Phase II: top two performing methods were subject to loading of doxorubicin (50, 75, 100 mg) in a single bolus (group A) or as a serial loading method (group B) followed by measurement of loading vs. time and elution vs. time. Results: Phase I revealed the most effective loading mechanisms and easiest handling to be dry (group A) vs. normal saline prehydrated (group B) SAP with normal saline reconstituted doxorubicin (10 mg/mL) with loading efficiencies of 83.1% and 88.4%. Phase II results revealed unstable behavior of SAP with 100 mg of doxorubicin and similar loading/elution profiles of dry and prehydrated SAP, with superior handling characteristics of group B SAP at 50 and 75 mg. Conclusions: SAP demonstrates the ability to load and bulk phase transfer doxorubicin at 50 and 75 mg with ease of handling and optimal efficiency through dry loading of SAP.« less
Simple, high-yield purification of xanthine oxidase from bovine milk.
Ozer, N; Müftüoglu, M; Ataman, D; Ercan, A; Ogüs, I H
1999-05-13
Xanthine oxidase, a commercially important enzyme with a wide area of application, was extracted from fresh milk, without added preservatives, using toluene and heat. The short purification procedure, with high yield, consisted of extraction, ammonium sulfate fractionation, and DEAE-Sepharose (fast flow) column chromatography. Xanthine oxidase was eluted as a single activity peak from the column using a buffer gradient. The purification fold, specific activity and yield for the purified xanthine oxidase were 328, 10.161 U/mg and 69%, respectively. The enzyme was concentrated by ultrafiltration, although 31% of the activity was lost during concentration, no change in specific activity was observed. Activity and protein gave coincident staining bands on native polyacrylamide gels. The intensity and the number of bands were dependent on the oxidative state(s) of the enzyme; reduction by 2-mercaptoethanol decreased the intensity of the slow-moving bands and increased the intensity of the fastest-moving band. Following sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE), two major bands (molecular masses of 152 and 131 kDa) were observed, accounting for > or = 95% of xanthine oxidase. Native- and SDS-PAGE showed that the purified xanthine oxidase becomes a heterodimer due to endogenous proteases.
Ropero, M J Patiño; Fariñas, N Rodríguez; Krupp, E; Mateo, R; Nevado, J J Berzas; Martín-Doimeadios, R C Rodríguez
2016-06-01
Mercury (Hg) is likely bound to large biomolecules (e.g. proteins) in living organisms, and in order to assess Hg metabolic pathways and possible toxicological effects, it is essential to study these Hg containing biomolecules. However, the exact nature of most metal binding biomolecules is unknown. Such studies are still in their infancy and information on this topic is scarce because the analysis is challenging, mainly due to their lability upon digestion or extraction from the tissue. New analytical methods that allow complex Hg-biomolecules to be analysed intact are needed and only few very recent studies deal with this approach. Therefore, as an initial step towards the characterization of Hg containing biomolecules, an analytical procedure has been optimised using size-exclusion chromatography (SEC) with inductively coupled plasma mass spectrometry (ICP-MS) detection. We applied this technique to elucidate the distribution and elution profile of Hg and Se, and some physiological important elements such as Fe, Ni, Zn and Cu, to assess metal binding profiles in liver and kidney samples of red deer (Cervus elaphus) and wild boar (Sus scrofa) who roam freely within the largest Hg mining district on Earth, Almadén in Spain. Elemental fractionation profiles of the extracts from different tissues were obtained using two different SEC columns (BioSep-SEC-S2000 GL 300-1kDa and Superdex 75 10/300 GL 70-3kDa). Similar profiles of Hg were observed in red deer and wild boar; however, significant differences were evident for liver and kidney. Moreover, the profiles of Se showed a single peak at high-medium molecular weight in all investigated tissues, while co-elution of Hg with Fe, Ni, Zn and Cu was observed. Copyright © 2016 Elsevier B.V. All rights reserved.
Klein-Júnior, Luiz C; Viaene, Johan; Salton, Juliana; Koetz, Mariana; Gasper, André L; Henriques, Amélia T; Vander Heyden, Yvan
2016-09-09
Extraction methods evaluation to access plants metabolome is usually performed visually, lacking a truthful method of data handling. In the present study the major aim was developing reliable time- and solvent-saving extraction and fractionation methods to access alkaloid profiling of Psychotria nemorosa leaves. Ultrasound assisted extraction was selected as extraction method. Determined from a Fractional Factorial Design (FFD) approach, yield, sum of peak areas, and peak numbers were rather meaningless responses. However, Euclidean distance calculations between the UPLC-DAD metabolic profiles and the blank injection evidenced the extracts are highly diverse. Coupled with the calculation and plotting of effects per time point, it was possible to indicate thermolabile peaks. After screening, time and temperature were selected for optimization, while plant:solvent ratio was set at 1:50 (m/v), number of extractions at one and particle size at ≤180μm. From Central Composite Design (CCD) results modeling heights of important peaks, previously indicated by the FFD metabolic profile analysis, time was set at 65min and temperature at 45°C, thus avoiding degradation. For the fractionation step, a solid phase extraction method was optimized by a Box-Behnken Design (BBD) approach using the sum of peak areas as response. Sample concentration was consequently set at 150mg/mL, % acetonitrile in dichloromethane at 40% as eluting solvent, and eluting volume at 30mL. Summarized, the Euclidean distance and the metabolite profiles provided significant responses for accessing P. nemorosa alkaloids, allowing developing reliable extraction and fractionation methods, avoiding degradation and decreasing the required time and solvent volume. Copyright © 2016 Elsevier B.V. All rights reserved.
A search for diffuse band profile variations in the rho Ophiuchi cloud
NASA Technical Reports Server (NTRS)
Snow, T. P.; Timothy, J. G.; Sear, S.
1982-01-01
High signal-to-noise profiles of the broad diffuse interstellar band at 4430 A were obtained on the 2.2-m telescope at the Mauna Kea Observatory, using the newly-developed pulse-counting multi-anode microchannel array detector system in an effort to determine whether the band profile varies with mean grain size as expected if the band is produced by absorbers embedded in grain lattices. The lack of profile variability over several lines of sight where independent evidence indicates that the mean grain size varies shows that lambda 4430 is probably not formed by the same grains that are responsible for interstellar extinction at visible wavelengths. The possibility that this band is created by a population of very small ( approximately 100 A) grains is still viable, as is the hypothesis that it has a molecular origin.
Ultrawide bandgap pentamode metamaterials with an asymmetric double-cone outside profile
NASA Astrophysics Data System (ADS)
Chu, Yangyang; Li, Yucheng; Cai, Chengxin; Liu, Guangshuan; Wang, Zhaohong; Xu, Zhuo
2018-03-01
The band-gap characteristic is an important feature of acoustic metamaterials, which has important theoretical and practical significance in acoustic devices. Pentamode metamaterials (PMs) with phonon band-gap characteristics based on an asymmetric double-cone outside profile are presented and studied in this paper. The phonon band structures of these PMs are calculated by using the finite element method. In addition to the single-mode band-gaps, the complete 3D band-gaps are also obtained by changing the outside profile of the double-cone. Moreover, by adjusting the outside profile and the diameter of the double-cone to reduce the symmetry of the structure, the complete 3D band-gap can be widened. Further parametric analysis is presented to investigate the effect of geometrical parameters on the phonon band-gap property, the numerical simulations show that the maximum relative bandwidth is expanded by 15.14 times through reducing the symmetry of the structure. This study provides a possible way for PMs to control elastic wave propagation in the field of depressing vibration and noise, acoustic filtering and acoustic cloaking.
Kawai, Makoto; Hara, Yukichi
2006-02-01
Western blotting of aminopeptidase N (APN) detects a high-molecular-mass isoform (260 kDa) [M. Kawai, Y. Otake, Y. Hara High-molecular-mass isoform of aminopeptidase N/CD13 in serum from cholestatic patients. Clin Chim Acta 330 (2003) 141-149] in cholestatic patient serum but is time-consuming. Human sera were electrophoresed on polyacrylamide gel containing Triton-X100 (Triton-PAGE) and stained with leucine-B-naphthylamide (LAP-staining). The stained bands were eluted from the gel, treated with N- and O-glycosidase if necessary, and analyzed by Western blotting [M. Kawai, Y. Otake, Y. Hara High-molecular-mass isoform of aminopeptidase N/CD13 in serum from cholestatic patients. Clin Chim Acta 330 (2003) 141-149]. Triton-PAGE and LAP-staining clearly detected fast bands in all the sera examined. Almost parallel with leucine aminopeptidase activity, slow bands were strongly stained in all 11 cholestatic patients but clearly stained in 3 out of 14 patients with hepatobiliary diseases other than cholestasis. PAGE with various concentrations of Triton showed that Triton slows down slow bands but not fast bands. Western blotting showed that Triton-PAGE-slow bands of cholestasis contained 140 and 260-kDa APN and that fast bands were slightly smaller than monomer-size slow bands after glycosidase treatment. Less time-consuming than Western blotting, Triton-PAGE and LAP-staining detect novel APN bands slowed by Triton and partly composed of the high-molecular-mass isoform in cholestasis. The slow bands seem to be homodimers of APN with transmembrane anchors. The polypeptide of the fast band seems to be processed differently from that of the slow band.
Voigt deconvolution method and its applications to pure oxygen absorption spectrum at 1270 nm band.
Al-Jalali, Muhammad A; Aljghami, Issam F; Mahzia, Yahia M
2016-03-15
Experimental spectral lines of pure oxygen at 1270 nm band were analyzed by Voigt deconvolution method. The method gave a total Voigt profile, which arises from two overlapping bands. Deconvolution of total Voigt profile leads to two Voigt profiles, the first as a result of O2 dimol at 1264 nm band envelope, and the second from O2 monomer at 1268 nm band envelope. In addition, Voigt profile itself is the convolution of Lorentzian and Gaussian distributions. Competition between thermal and collisional effects was clearly observed through competition between Gaussian and Lorentzian width for each band envelope. Voigt full width at half-maximum height (Voigt FWHM) for each line, and the width ratio between Lorentzian and Gaussian width (ΓLΓG(-1)) have been investigated. The following applied pressures were at 1, 2, 3, 4, 5, and 8 bar, while the temperatures were at 298 K, 323 K, 348 K, and 373 K range. Copyright © 2015 Elsevier B.V. All rights reserved.
Forced degradation and impurity profiling: recent trends in analytical perspectives.
Jain, Deepti; Basniwal, Pawan Kumar
2013-12-01
This review describes an epigrammatic impression of the recent trends in analytical perspectives of degradation and impurities profiling of pharmaceuticals including active pharmaceutical ingredient (API) as well as drug products during 2008-2012. These recent trends in forced degradation and impurity profiling were discussed on the head of year of publication; columns, matrix (API and dosage forms) and type of elution in chromatography (isocratic and gradient); therapeutic categories of the drug which were used for analysis. It focuses distinctly on comprehensive update of various analytical methods including hyphenated techniques for the identification and quantification of thresholds of impurities and degradants in different pharmaceutical matrices. © 2013 Elsevier B.V. All rights reserved.
Bernevic, Bogdan; El-Khatib, Ahmed H; Jakubowski, Norbert; Weller, Michael G
2018-04-02
The human copper-protein ceruloplasmin (Cp) is the major copper-containing protein in the human body. The accurate determination of Cp is mandatory for the reliable diagnosis of several diseases. However, the analysis of Cp has proven to be difficult. The aim of our work was a proof of concept for the determination of a metalloprotein-based on online immunocapture ICP-MS. The immuno-affinity step is responsible for the enrichment and isolation of the analyte from serum, whereas the compound-independent quantitation with ICP-MS delivers the sensitivity, precision, and large dynamic range. Off-line ELISA (enzyme-linked immunosorbent assay) was used in parallel to confirm the elution profile of the analyte with a structure-selective method. The total protein elution was observed with the 32 S mass trace. The ICP-MS signals were normalized on a 59 Co signal. The human copper-protein Cp could be selectively determined. This was shown with pure Cp and with a sample of human serum. The good correlation with off-line ELISA shows that Cp could be captured and eluted selectively from the anti-Cp affinity column and subsequently determined by the copper signal of ICP-MS.
Balss, Karin M; Long, Frederick H; Veselov, Vladimir; Orana, Argjenta; Akerman-Revis, Eugena; Papandreou, George; Maryanoff, Cynthia A
2008-07-01
Multivariate data analysis was applied to confocal Raman measurements on stents coated with the polymers and drug used in the CYPHER Sirolimus-eluting Coronary Stents. Partial least-squares (PLS) regression was used to establish three independent calibration curves for the coating constituents: sirolimus, poly(n-butyl methacrylate) [PBMA], and poly(ethylene-co-vinyl acetate) [PEVA]. The PLS calibrations were based on average spectra generated from each spatial location profiled. The PLS models were tested on six unknown stent samples to assess accuracy and precision. The wt % difference between PLS predictions and laboratory assay values for sirolimus was less than 1 wt % for the composite of the six unknowns, while the polymer models were estimated to be less than 0.5 wt % difference for the combined samples. The linearity and specificity of the three PLS models were also demonstrated with the three PLS models. In contrast to earlier univariate models, the PLS models achieved mass balance with better accuracy. This analysis was extended to evaluate the spatial distribution of the three constituents. Quantitative bitmap images of drug-eluting stent coatings are presented for the first time to assess the local distribution of components.
Wernisch, Stefanie; Trapp, Oliver; Lindner, Wolfgang
2013-09-17
The interconversion of cis and trans isomers of dipeptides containing C-terminal proline was studied by dynamic chromatography on zwitterionic chiral stationary phases at temperatures ranging from -15°C to +45°C The cis-trans isomers could be separated below 0°C and above 0-10°C plateau formation and peak coalescence phenomena occurred, which is characteristic for a dynamic process at the time-scale of partitioning. At and above room temperature, full coalescence was observed, which allowed separations of enantiomers without interference from interconversion effects. Analysis of the dynamic elution profiles of the interconverting peptides allowed the determination of isomerization rate constants and thermodynamic activation parameters (isomerization enthalpy, entropy and activation energy). In accordance with established results, isomerization rates and thermodynamic parameters were found to depend on the nature of the N-terminal amino acid. Isomerization barriers were only slightly lower than values determined with other methods but significant differences in the relative contributions of the activation enthalpy and entropy as well as isomerization rates pointed toward selector-moderated isomerization dynamics. Copyright © 2013 Elsevier B.V. All rights reserved.
Hong, Chang-Sook; Funk, Sonja; Muller, Laurent; Boyiadzis, Michael; Whiteside, Theresa L
2016-01-01
Isolation from human plasma of exosomes that retain functional and morphological integrity for probing their protein, lipid and nucleic acid content is a priority for the future use of exosomes as biomarkers. A method that meets these criteria and can be scaled up for patient monitoring is thus desirable. Plasma specimens (1 mL) of patients with acute myeloid leukaemia (AML) or a head and neck squamous cell carcinoma (HNSCC) were differentially centrifuged, ultrafiltered and fractionated by size exclusion chromatography in small disposable columns (mini-SEC). Exosomes were eluted in phosphate-buffered saline and were evaluated by qNano for particle size and counts, morphology by transmission electron microscopy, protein content, molecular profiles by western blots, and for ability to modify functions of immune cells. Exosomes eluting in fractions #3-5 had a diameter ranging from 50 to 200 nm by qNano, with the fraction #4 containing the bulk of clean, unaggregated exosomes. The exosome elution profiles remained constant for repeated runs of the same plasma. Larger plasma volumes could be fractionated running multiple mini-SEC columns in parallel. Particle concentrations per millilitre of plasma in #4 fractions of AML and HNSCC were comparable and were higher (p<0.003) than those in normal controls. Isolated AML exosomes co-incubated with normal human NK cells inhibited NKG2D expression levels (p<0.004), and HNSCC exosomes suppressed activation (p<0.01) and proliferation of activated T lymphocytes (p<0.03). Mini-SEC allows for simple and reproducible isolation from human plasma of exosomes retaining structural integrity and functional activity. It enables molecular/functional analysis of the exosome content in serial specimens of human plasma for clinical applications.
Leaching of FGD Byproducts Using a CSTX
DOE Office of Scientific and Technical Information (OSTI.GOV)
Kairies, C.L.; Schroeder, K.T.; Cardone, C.R.
2005-09-01
Leaching studies of coal utilization byproducts (CUB) are often performed to determine the compatibility of the material in a particular end-use or disposal environment. Typically, these studies are conducted using either a batch or a fixed-bed column technique. Fixed-bed columns offer the advantage of a continuous flow of effluent that provides elution profiles with changing elution volume and pH. Unfortunately, clogs can form in fixed-bed leaching columns, either because of cementitious properties of the material itself, such as is seen for fluidized bed combustion (FBC) fly ash, or because of precipitate formation, such as can occur when a high-calcium ashmore » is subjected to sulfate-containing leachates. Also, very fine-grained materials, such as gypsum, do not provide sufficient permeability for study in a fixed-bed column. A continuous, stirred-tank extractor (CSTX) is being used as an alternative technique that can provide the elution profile of column leaching but without the low permeability problems. The CSTX has been successfully employed in the leaching of flue gas desulfurization products that would not be sufficiently permeable under traditional column leaching conditions. The results indicate that the leaching behavior depends on a number of factors, including (but not limited to) solubility and neutralization capacity of the mineral phases present, sorption properties of these phases, behavior of the solubilized material in the tank, and the type of species in solution. In addition, leaching to near-exhaustion of a wallboard produced from FGD gypsum has allowed the isolation of a highly adsorptive phase. This phase appears to be present in at least some FGD gypsums and accounts for the immobilization of trace metals such as arsenic, cobalt, lead, and mercury.« less
de la Torre Hernández, José M; Brugaletta, Salvatore; Gómez Hospital, Joan A; Baz, José A; Pérez de Prado, Armando; López Palop, Ramón; Cid, Belén; García Camarero, Tamara; Diego, Alejandro; Gimeno de Carlos, Federico; Fernández Díaz, José A; Sanchis, Juan; Alfonso, Fernando; Blanco, Roberto; Botas, Javier; Navarro Cuartero, Javier; Moreu, José; Bosa, Francisco; Vegas Valle, José M; Elízaga, Jaime; Arrebola, Antonio L; Ruiz Arroyo, José R; Hernández-Hernández, Felipe; Salvatella, Neus; Monteagudo, Marta; Gómez Jaume, Alfredo; Carrillo, Xavier; Martín Reyes, Roberto; Lozano, Fernando; Rumoroso, José R; Andraka, Leire; Domínguez, Antonio J
2017-02-01
The proportion of elderly patients undergoing primary angioplasty is growing. The present study describes the clinical profile, procedural characteristics, outcomes, and predictors of outcome. A 31-center registry of consecutive patients older than 75 years treated with primary angioplasty. Clinical and procedural data were collected, and the patients underwent clinical follow-up. The study included 3576 patients (39.3% women, 48.5% with renal failure, 11.5% in Killip III or IV, and 29.8% with>6hours of chest pain). Multivessel disease was present in 55.4% and nonculprit lesions were additionally treated in 24.8%. Radial access was used in 56.4%, bivalirudin in 11.8%, thromboaspiration in 55.9%, and drug-eluting stents in 26.6%. The 1-month and 2-year incidences of cardiovascular death were 10.1% and 14.7%, respectively. The 2-year rates of definite or probable thrombosis, repeat revascularization, and BARC bleeding>2 were 3.1%, 2.3%, and 4.2%, respectively. Predictive factors were diabetes mellitus, renal failure, atrial fibrillation, delay to reperfusion>6hours, ejection fraction<45%, Killip class III-IV, radial access, bivalirudin, drug-eluting stents, final TIMI flow of III, and incomplete revascularization at discharge. Notable registry findings include frequently delayed presentation and a high prevalence of adverse factors such as renal failure and multivessel disease. Positive procedure-related predictors include shorter delay, use of radial access, bivalirudin, drug-eluting stents, and complete revascularization before discharge. Copyright © 2016 Sociedad Española de Cardiología. Published by Elsevier España, S.L.U. All rights reserved.
[UPLC characteristic chromatographic profile of Poria].
Zhang, Qi; Wang, Zhenzhong; Xiao, Wei; Zhang, Liangqi; Bi, Kaishun; Jia, Ying
2012-04-01
To establish a UPLC characteristic chromatographic profile analysis method to quickly assess Poria quality and provide basis fro controlling Poria quality. The UPLC characteristic chromatographic profiles of fifteen batches of Poria were determined by ACQUITY UPLC, with HSS T3 Column (2.1 mm x 100 mm, 1.8 microm) eluted with the mobile phases of water containing 0.05% phosphoric acid and acetonitrile in gradient mode. The detection wavelength was set at 243 nm. The common mode of the UPLC characteristic chromatographic profile was set up. There were 20 common peaks, seven of which were identified, and the similar degrees of the fifteen samples to the common mode were between 0.787 and 0.974. The method was so time-saving that it can be used for the quality control of Poria.
Groskreutz, Stephen R.; Weber, Stephen G.
2016-01-01
In this work we characterize the development of a method to enhance temperature-assisted on-column solute focusing (TASF) called two-stage TASF. A new instrument was built to implement two-stage TASF consisting of a linear array of three independent, electronically controlled Peltier devices (thermoelectric coolers, TECs). Samples are loaded onto the chromatographic column with the first two TECs, TEC A and TEC B, cold. In the two-stage TASF approach TECs A and B are cooled during injection. TEC A is heated following sample loading. At some time following TEC A’s temperature rise, TEC B’s temperature is increased from the focusing temperature to a temperature matching that of TEC A. Injection bands are focused twice on-column, first on the initial TEC, e.g. single-stage TASF, then refocused on the second, cold TEC. Our goal is to understand the two-stage TASF approach in detail. We have developed a simple yet powerful digital simulation procedure to model the effect of changing temperature in the two focusing zones on retention, band shape and band spreading. The simulation can predict experimental chromatograms resulting from spatial and temporal temperature programs in combination with isocratic and solvent gradient elution. To assess the two-stage TASF method and the accuracy of the simulation well characterized solutes are needed. Thus, retention factors were measured at six temperatures (25–75 °C) at each of twelve mobile phases compositions (0.05–0.60 acetonitrile/water) for homologs of n-alkyl hydroxylbenzoate esters and n-alkyl p-hydroxyphenones. Simulations accurately reflect experimental results in showing that the two-stage approach improves separation quality. For example, two-stage TASF increased sensitivity for a low retention solute by a factor of 2.2 relative to single-stage TASF and 8.8 relative to isothermal conditions using isocratic elution. Gradient elution results for two-stage TASF were more encouraging. Application of two-stage TASF increased peak height for the least retained solute in the test mixture by a factor of 3.2 relative to single-stage TASF and 22.3 compared to isothermal conditions for an injection four-times the column volume. TASF improved resolution and increased peak capacity; for a 12-minute separation peak capacity increased from 75 under isothermal conditions to 146 using single-stage TASF, and 185 for two-stage TASF. PMID:27836226
Groskreutz, Stephen R; Weber, Stephen G
2016-11-25
In this work we characterize the development of a method to enhance temperature-assisted on-column solute focusing (TASF) called two-stage TASF. A new instrument was built to implement two-stage TASF consisting of a linear array of three independent, electronically controlled Peltier devices (thermoelectric coolers, TECs). Samples are loaded onto the chromatographic column with the first two TECs, TEC A and TEC B, cold. In the two-stage TASF approach TECs A and B are cooled during injection. TEC A is heated following sample loading. At some time following TEC A's temperature rise, TEC B's temperature is increased from the focusing temperature to a temperature matching that of TEC A. Injection bands are focused twice on-column, first on the initial TEC, e.g. single-stage TASF, then refocused on the second, cold TEC. Our goal is to understand the two-stage TASF approach in detail. We have developed a simple yet powerful digital simulation procedure to model the effect of changing temperature in the two focusing zones on retention, band shape and band spreading. The simulation can predict experimental chromatograms resulting from spatial and temporal temperature programs in combination with isocratic and solvent gradient elution. To assess the two-stage TASF method and the accuracy of the simulation well characterized solutes are needed. Thus, retention factors were measured at six temperatures (25-75°C) at each of twelve mobile phases compositions (0.05-0.60 acetonitrile/water) for homologs of n-alkyl hydroxylbenzoate esters and n-alkyl p-hydroxyphenones. Simulations accurately reflect experimental results in showing that the two-stage approach improves separation quality. For example, two-stage TASF increased sensitivity for a low retention solute by a factor of 2.2 relative to single-stage TASF and 8.8 relative to isothermal conditions using isocratic elution. Gradient elution results for two-stage TASF were more encouraging. Application of two-stage TASF increased peak height for the least retained solute in the test mixture by a factor of 3.2 relative to single-stage TASF and 22.3 compared to isothermal conditions for an injection four-times the column volume. TASF improved resolution and increased peak capacity; for a 12-min separation peak capacity increased from 75 under isothermal conditions to 146 using single-stage TASF, and 185 for two-stage TASF. Copyright © 2016 Elsevier B.V. All rights reserved.
Waksman, Ron; Ghali, Magdi; Goodroe, Randy; Ryan, Thomas; Turco, Mark; Ring, Michael; McGarry, Thomas; Dobies, David; Shammas, Nicolas; Steinberg, Daniel H; Swymelar, Stacy; Kaneshige, Kimberly; Torguson, Rebecca
2012-10-15
Registry Experience at the Washington Hospital Center, DES - Taxus Liberte Versus Xience V (REWARDS TLX) is a physician-initiated, retrospective, real-world, multicenter, observational study for all patients >18 years of age subjected to percutaneous coronary intervention with everolimus-eluting stents (EESs) or paclitaxel-eluting stents (PESs). Outcomes of patients receiving a TAXUS Liberté or XIENCE V drug-eluting stent were compared. Baseline clinical, procedural, and follow-up data at 12 months were collected from 10 clinical centers by an electronic data capture system. The study's primary end point was major adverse cardiac events: a composite of all-cause death, Q-wave myocardial infarction, target vessel revascularization, and stent thrombosis. The trial is registered with http://www.clinicaltrials.gov (NCT01134159). Data were entered for 1,195 patients (PES, n = 595; EES, n = 600). Baseline clinical characteristics were similar except for higher dyslipidemia, systemic hypertension, and family history of coronary artery disease in the EES group. In-hospital outcome was similar between groups, with an overall in-hospital stent thrombosis rate of 0.2%. The primary end point at 12 months was similar (EES 7.8% vs 10.8%, p = 0.082). Overall stent thrombosis rate was lower in the EES group (0.3% vs 1.2%, respectively, p = 0.107); however, target lesion revascularization was similar (PES, hazard ratio 1.46, 95% confidence interval 0.98 to 2.19, p = 0.064). There was no difference in overall mortality between groups. In conclusion, second-generation EESs and PESs demonstrated similar efficacy and safety profiles for broadened patient and lesion subsets compared to a selected population from the pivotal trials. However, for composite efficacy and safety end points, EESs outperformed second-generation PESs. Copyright © 2012 Elsevier Inc. All rights reserved.
Toklu, Bora; Amoroso, Nicholas; Fusaro, Mario; Kumar, Sunil; Hannan, Edward L; Faxon, David P; Feit, Frederick
2013-01-01
Objective To compare the efficacy and safety of biodegradable polymer drug eluting stents with those of bare metal stents and durable polymer drug eluting stents. Design Mixed treatment comparison meta-analysis of 258 544 patient years of follow-up from randomized trials. Data sources and study selection PubMed, Embase, and Central were searched for randomized trials comparing any of the Food and Drug Administration approved durable polymer drug eluting stents (sirolimus eluting, paclitaxel eluting, cobalt chromium everolimus eluting, platinum chromium everolimus eluting, zotarolimus eluting-Endeavor, and zotarolimus eluting-Resolute) or biodegradable polymer drug eluting stents, with each other or against bare metal stents. Outcomes Long term efficacy (target vessel revascularization, target lesion revascularization) and safety (death, myocardial infarction, stent thrombosis). Landmark analysis at more than one year was evaluated to assess the potential late benefit of biodegradable polymer drug eluting stents. Results From 126 randomized trials and 258 544 patient years of follow-up, for long term efficacy (target vessel revascularization), biodegradable polymer drug eluting stents were superior to paclitaxel eluting stents (rate ratio 0.66, 95% credibility interval 0.57 to 0.78) and zotarolimus eluting stent-Endeavor (0.69, 0.56 to 0.84) but not to newer generation durable polymer drug eluting stents (for example: 1.03, 0.89 to 1.21 versus cobalt chromium everolimus eluting stents). Similarly, biodegradable polymer drug eluting stents were superior to paclitaxel eluting stents (rate ratio 0.61, 0.37 to 0.89) but inferior to cobalt chromium everolimus eluting stents (2.04, 1.27 to 3.35) for long term safety (definite stent thrombosis). In the landmark analysis after one year, biodegradable polymer drug eluting stents were superior to sirolimus eluting stents for definite stent thrombosis (rate ratio 0.29, 0.10 to 0.82) but were associated with increased mortality compared with cobalt chromium everolimus eluting stents (1.52, 1.02 to 2.22). Overall, among all stent types, the newer generation durable polymer drug eluting stents (zotarolimus eluting stent-Resolute, cobalt chromium everolimus eluting stents, and platinum chromium everolimus eluting stents) were the most efficacious (lowest target vessel revascularization rate) stents, and cobalt chromium everolimus eluting stents were the safest with significant reductions in definite stent thrombosis (rate ratio 0.35, 0.21 to 0.53), myocardial infarction (0.65, 0.55 to 0.75), and death (0.72, 0.58 to 0.90) compared with bare metal stents. Conclusions Biodegradable polymer drug eluting stents are superior to first generation durable polymer drug eluting stents but not to newer generation durable polymer stents in reducing target vessel revascularization. Newer generation durable polymer stents, and especially cobalt chromium everolimus eluting stents, have the best combination of efficacy and safety. The utility of biodegradable polymer stents in the context of excellent clinical outcomes with newer generation durable polymer stents needs to be proven. PMID:24212107
Fasoula, S; Zisi, Ch; Gika, H; Pappa-Louisi, A; Nikitas, P
2015-05-22
A package of Excel VBA macros have been developed for modeling multilinear gradient retention data obtained in single or double gradient elution mode by changing organic modifier(s) content and/or eluent pH. For this purpose, ten chromatographic models were used and four methods were adopted for their application. The methods were based on (a) the analytical expression of the retention time, provided that this expression is available, (b) the retention times estimated using the Nikitas-Pappa approach, (c) the stepwise approximation, and (d) a simple numerical approximation involving the trapezoid rule for integration of the fundamental equation for gradient elution. For all these methods, Excel VBA macros have been written and implemented using two different platforms; the fitting and the optimization platform. The fitting platform calculates not only the adjustable parameters of the chromatographic models, but also the significance of these parameters and furthermore predicts the analyte elution times. The optimization platform determines the gradient conditions that lead to the optimum separation of a mixture of analytes by using the Solver evolutionary mode, provided that proper constraints are set in order to obtain the optimum gradient profile in the minimum gradient time. The performance of the two platforms was tested using experimental and artificial data. It was found that using the proposed spreadsheets, fitting, prediction, and optimization can be performed easily and effectively under all conditions. Overall, the best performance is exhibited by the analytical and Nikitas-Pappa's methods, although the former cannot be used under all circumstances. Copyright © 2015 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Walrath, Jenna Cherie
Low-dimensional semiconductor structures are important for a wide variety of applications, and recent advances in nanoscale fabrication are paving the way for increasingly precise nano-engineering of a wide range of materials. It is therefore essential that the physics of materials at the nanoscale are thoroughly understood to unleash the full potential of nanotechnology, requiring the development of increasingly sophisticated instrumentation and modeling. Of particular interest is the relationship between the local density of states (LDOS) of low-dimensional structures and the band structure and local electronic properties. This dissertation presents the investigation of the band structure, LDOS, and local electronic properties of nanostructures ranging from zero-dimensional (0D) quantum dots (QDs) to two-dimensional (2D) thin films, synthesizing computational and experimental approaches including Poisson-Schrodinger band structure calculations, scanning tunneling microscopy (STM), scanning tunneling spectroscopy (STS), and scanning thermoelectric microscopy (SThEM). A method is presented for quantifying the local Seebeck coefficient (S) with SThEM, using a quasi-3D conversion matrix approach to directly convert temperature gradient-induced voltages S. For a GaAs p-n junction, the resulting S-profile is consistent with that computed using the free carrier concentration profile. This combined computational-experimental approach is expected to enable nanoscale measurements of S across a wide variety of heterostructure interfaces. The local carrier concentration, n, is profiled across epitaxial InAs/GaAs QDs, where SThEM is used to profile the temperature gradient-induced voltage, which is converted to a profile of the local S and finally to an n profile. The S profile is converted to a conduction band-edge profile and compared with Poisson-Schrodinger band-edge simulations. The combined computational-experimental approach suggests a reduced n in the QD center in comparison to that of the 2D alloy layer. The surface composition and band structure of ordered horizontal Sb2Te3 nanowires induced by femtosecond laser irradiation of a thin film are investigated, revealing a band gap modulation between buried Sb2Te3 nanowires and the surrounding insulating material. Finally, STM and STS are used to investigate the band structure of BiSbTe alloys at room temperature, revealing both the Fermi level and Dirac point located inside the bulk bandgap, indicating bulk-like insulating behavior with accessible surface states.
Rogers, Geraint B; Daniels, Thomas WV; Tuck, Andrew; Carroll, Mary P; Connett, Gary J; David, Gondi JP; Bruce, Kenneth D
2009-01-01
Background Drawing from previous studies, the traditional routine diagnostic microbiology evaluation of samples from chronic respiratory conditions may provide an incomplete picture of the bacteria present in airways disease. Here, the aim was to determine the extent to which routine diagnostic microbiology gave a different assessment of the species present in sputa when analysed by using culture-independent assessment. Methods Six different media used in routine diagnostic microbiology were inoculated with sputum from twelve patients. Bacterial growth on these plates was harvested and both RNA and DNA extracted. DNA and RNA were also extracted directly from the same sample of sputum. All nucleic acids served as templates for PCR and reverse transcriptase-PCR amplification of "broad range" bacterial 16S rRNA gene regions. The regions amplified were separated by Terminal Restriction Fragment Length Polymorphism (T-RFLP) profiling and compared to assess the degree of overlap between approaches. Results A mean of 16.3 (SD 10.0) separate T-RF band lengths in the profiles from each sputum sample by Direct Molecular Analysis, with a mean of 8.8 (SD 5.8) resolved by DNA profiling and 13.3 (SD 8.0) resolved by RNA profiling. In comparison, 8.8 (SD 4.4) T-RF bands were resolved in profiles generated by Culture-derived Molecular Analysis. There were a total of 184 instances of T-RF bands detected in the direct sputum profiles but not in the corresponding culture-derived profiles, representing 83 different T-RF band lengths. Amongst these were fifteen instances where the T-RF band represented more than 10% of the total band volume (with a mean value of 23.6%). Eight different T-RF band lengths were resolved as the dominant band in profiles generated directly from sputum. Of these, only three were detected in profiles generated from the corresponding set of cultures. Conclusion Due to their focus on isolation of a small group of recognised pathogens, the use of culture-dependent methods to analyse samples from chronic respiratory infections can provide a restricted understanding of the bacterial species present. The use of a culture-independent molecular approach here identifies that there are many bacterial species in samples from CF and COPD patients that may be clinically relevant. PMID:19368727
Inducible immune proteins in the dampwood termite Zootermopsis angusticollis
NASA Astrophysics Data System (ADS)
Rosengaus, Rebeca B.; Cornelisse, Tara; Guschanski, Katerina; Traniello, James F. A.
2007-01-01
Dampwood termites, Zootermopsis angusticollis (Isoptera: Termopsidae), mount an immune response to resist microbial infection. Here we report on results of a novel analysis that allowed us to electrophoretically assess changes in hemolymph proteins in the same individual before and after exposure to a pathogen. We demonstrate that contact with a sublethal concentration of the entomopathogenic fungus Metarhizium anisopliae (Deuteromycotina:Hypomycetes) induces the production of protective proteins in nymphs, pseudergates (false workers), and soldiers. Termites exposed to an immunizing dosage of fungal conidia consistently showed an enhancement of constitutive proteins (62-85 kDa) in the hemolymph as well as an induction of novel proteins (28-48 kDa) relative to preimmunization levels. No significant differences in protein banding patterns relative to baseline levels in control and naïve termites were observed. Incubating excised and eluted induced proteins produced by immunized pseudergates or immunized soldiers with conidia significantly reduced the germination of the fungus. The fungistatic effect of eluted proteins differed significantly among five colonies examined. Our results show that the upregulation of protective proteins in the hemolymph underscores the in vivo immune response we previously recorded in Z. angusticollis.
Chen, Yong; Li, Yang; Liu, Peng; Sun, Qun; Liu, Zhu
2014-04-01
A weakness of using immobilized metal affinity chromatography (IMAC) to purify recombinant proteins expressed in Pichia pastoris is the co-purification of native proteins that exhibit high affinities for Ni-IMAC. We have determined the elution profiles of P. pastoris proteins and have examined the native proteins that co-purify when eluting with 100 mM imidazole. Four major contaminants were identified: mitochondrial alcohol dehydrogenase isozyme III (mADH), nucleotide excision repair endonuclease, and the hypothetical proteins TPHA_0L01390 and TDEL_0B02190 which are homologous proteins derived from Tetrapisispora phaffii and Torulaspora delbrueckii, respectively. A new P. pastoris expression strain was engineered that eliminated the predominant contaminant, mADH, by gene disruption. The total amount of protein contaminants was reduced by 55 % without effecting cell growth. The present study demonstrates the feasibility of using a proteomic approach to facilitate bioprocess optimization.
NASA Technical Reports Server (NTRS)
Wang, Zuwei; Vaksman, Zalman; Putcha, Lakshmi
2008-01-01
Intranasal scopolamine is a choice drug for the treatment of motion sickness during space flight because of its quick onset of action, short half-life and favorable sideeffects profile. The dose administered usually ranges between 0.1 and 0.4 mg. Such small doses make it difficult to detect concentrations of scopolamine in biological fluids using existing sensitive LC/MS/MS method, especially when the biological sample volumes are limited. To measure scopolamine in human plasma to facilitate pharmacokinetic evaluation of the drug, we developed a sensitive LC/MS/MS method using 96 well micro elution plates for solid phase extraction (SPE) of scopolamine in human plasma. Human plasma (100-250 micro L) were loaded onto Waters Oasis HLB 96 well micro elution plate and eluted with 50 L of organic solvent without evaporation and reconstitution. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 3 minutes. The mobile phase for separation was 80:20 (v/v) methanol: ammonium acetate (30 mM) in water. Concentrations of scopolamine were determined using a Micromass Quattro Micro(TM) mass spectrometer with electrospray ionization (ESI). ESI mass spectra were acquired in positive ion mode with multiple reaction monitoring for the determination of scopolamine m/z = 304.2 right arrow 138.1 and internal standard hyoscyamine m/z = 290.2 right arrow 124.1. The method is rapid, reproducible, specific and has the following parameters: scopolamine and the IS are eluted at about 1.1 and 1.7 min respectively. The linear range is 25-10000 pg/mL for scopolamine in human plasma with correlation coefficients greater than 0.99 and CV less than 0.5%. The intra-day and inter-day CVs are less than 15% for quality control samples with concentrations of 75,300, and 750 pg/mL of scopolamine in human plasma. SPE using 96 well micro elution plates allows rapid sample preparation and enhanced sensitivity for the LC/MS/MS determination of scopolamine in a small volume of biological samples. The new method is also cost effective since it uses a small volume of organic solvents compared to the methods using SPE cartridges or regular 96 well SPE plates. This method can be successfully used for bioavailability and pharmacokinetic evaluations of scopolamine, especially when volumes of biological samples are limited. Further investigation to use automated SPE system with 96 well micro elution plates is planned.
Zhang, Tian-Tian; Lu, Chuan-Li; Jiang, Jian-Guo; Wang, Min; Wang, Dong-Mei; Zhu, Wei
2015-10-05
Polysaccharides of Rubus chingii Hu fruit and leaf were extracted to compare their antioxidant, anti-inflammatory, and anticancer activities against breast cancer cells MCF-7 and liver cancer cells Bel-7402. Results showed that all the tested bioactivities of polysaccharides from leaf (L-Ps) were better than those of polysaccharides from fruit (F-Ps). Response surface methodology was then used to optimize the extraction conditions of polysaccharides from leaf. Additionally, polysaccharides from fruit and leaf were characterized and their contents of total sugars, proteins and uronic acid were compared. It was found that polysaccharides from fruit and leaf were similar in IR and UV absorption, but significantly different in contents of total sugars, protein and uronic acid. Their elution profiles of DEAE-Sepharose fast flow column were different too. The main peak of polysaccharides from fruit was eluted with 0.3 mol/l NaCl solution and the main peak of polysaccharides from leaf was eluted with deionized water. The differences between the two polysaccharides may be responsible for their differences in bioactivities. Further studies are required to explore their complete structural characteristics, structure-activity relationship and the mechanism of their activities. Copyright © 2015 Elsevier Ltd. All rights reserved.
Jin, Gaowa; Guo, Zhimou; Xiao, Yuansheng; Yan, Jingyu; Dong, Xuefang; Shen, Aijin; Wang, Chaoran; Liang, Xinmiao
2016-10-01
A practical method was established for the definition of chromatographic parameters in preparative liquid chromatography. The parameters contained both the peak broadening level under different amounts of sample loading and the concentration distribution of the target compound in the elution. The parameters of the peak broadening level were defined and expressed as a matrix, which consisted of sample loading, the forward broadening and the backward broadening levels. The concentration distribution of the target compound was described by the heat map of the elution profile. The most suitable stationary phase should exhibit the narrower peak broadening and it was best to broaden to both sides to compare to the peak under analytical conditions. Besides, the concentration distribution of the target compounds should be focused on the middle of the elution. The guiding principles were validated by purification of amitriptyline from the mixture of desipramine and amitriptyline. On the selected column, when the content of the impurity desipramine was lower than 0.1%, the recovery of target compound was much higher than the other columns even when the sample loading was as high as 8.03 mg/cm 3 . The parameters and methods could be used for the evaluation and selection of stationary phases in preparative chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
D'Archivio, Angelo Antonio; Maggi, Maria Anna; Ruggieri, Fabrizio
2014-08-01
In this paper, a multilayer artificial neural network is used to model simultaneously the effect of solute structure and eluent concentration profile on the retention of s-triazines in reversed-phase high-performance liquid chromatography under linear gradient elution. The retention data of 24 triazines, including common herbicides and their metabolites, are collected under 13 different elution modes, covering the following experimental domain: starting acetonitrile volume fraction ranging between 40 and 60% and gradient slope ranging between 0 and 1% acetonitrile/min. The gradient parameters together with five selected molecular descriptors, identified by quantitative structure-retention relationship modelling applied to individual separation conditions, are the network inputs. Predictive performance of this model is evaluated on six external triazines and four unseen separation conditions. For comparison, retention of triazines is modelled by both quantitative structure-retention relationships and response surface methodology, which describe separately the effect of molecular structure and gradient parameters on the retention. Although applied to a wider variable domain, the network provides a performance comparable to that of the above "local" models and retention times of triazines are modelled with accuracy generally better than 7%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Reflectivity retrieval in a networked radar environment
NASA Astrophysics Data System (ADS)
Lim, Sanghun
Monitoring of precipitation using a high-frequency radar system such as X-band is becoming increasingly popular due to its lower cost compared to its counterpart at S-band. Networks of meteorological radar systems at higher frequencies are being pursued for targeted applications such as coverage over a city or a small basin. However, at higher frequencies, the impact of attenuation due to precipitation needs to be resolved for successful implementation. In this research, new attenuation correction algorithms are introduced to compensate the attenuation impact due to rain medium. In order to design X-band radar systems as well as evaluate algorithm development, it is useful to have simultaneous X-band observation with and without the impact of path attenuation. One way to obtain that data set is through theoretical models. Methodologies for generating realistic range profiles of radar variables at attenuating frequencies such as X-band for rain medium are presented here. Fundamental microphysical properties of precipitation, namely size and shape distribution information, are used to generate realistic profiles of X-band starting with S-band observations. Conditioning the simulation from S-band radar measurements maintains the natural distribution of microphysical parameters associated with rainfall. In this research, data taken by the CSU-CHILL radar and the National Center for Atmospheric Research S-POL radar are used to simulate X-band radar variables. Three procedures to simulate the radar variables at X-band and sample applications are presented. A new attenuation correction algorithm based on profiles of reflectivity, differential reflectivity, and differential propagation phase shift is presented. A solution for specific attenuation retrieval in rain medium is proposed that solves the integral equations for reflectivity and differential reflectivity with cumulative differential propagation phase shift constraint. The conventional rain profiling algorithms that connect reflectivity and specific attenuation can retrieve specific attenuation values along the radar path assuming a constant intercept parameter of the normalized drop size distribution. However, in convective storms, the drop size distribution parameters can have significant variation along the path. In this research, a dual-polarization rain profiling algorithm for horizontal-looking radars incorporating reflectivity as well as differential reflectivity profiles is developed. The dual-polarization rain profiling algorithm has been evaluated with X-band radar observations simulated from drop size distribution derived from high-resolution S-band measurements collected by the CSU-CHILL radar. The analysis shows that the dual-polarization rain profiling algorithm provides significant improvement over the current algorithms. A methodology for reflectivity and attenuation retrieval for rain medium in a networked radar environment is described. Electromagnetic waves backscattered from a common volume in networked radar systems are attenuated differently along the different paths. A solution for the specific attenuation distribution is proposed by solving the integral equation for reflectivity. The set of governing integral equations describing the backscatter and propagation of common resolution volume are solved simultaneously with constraints on total path attenuation. The proposed algorithm is evaluated based on simulated X-band radar observations synthesized from S-band measurements collected by the CSU-CHILL radar. Retrieved reflectivity and specific attenuation using the proposed method show good agreement with simulated reflectivity and specific attenuation.
NASA Astrophysics Data System (ADS)
Shinsuke, T.; Yasumi, A.; Takashi, K.
2003-05-01
To investigate whether trace metals bind to metallothioneins (MTs) in the hepatocytosol of green turtles (Chelonia mydas) and hawksbill turtles (Eretmochelys imbricata), MT fraction was obtained by ultracentrifugation and gel filtration methods. MTs separated from hepatocytosol were further purified and characterized by high performance liquid chromatography/inductively coupled plasma-mass spectrometry. In addition, the involvement of MTs in the accumulation of trace metals in the liver of sea turtle was examine. Gel filtration analysis showed that significant amounts of Cu, Zn, Ag and Cd were bound to MT in the cytosol of sea turtles, suggesting that such trace metals were primarily detoxified by interaction with MTs in the liver. Elution profiles of these trace metals by anion-exchange chromatography were different between green turtles and hawksbill turtles. These results suggest the presence of multiple isoforms of MT in the liver of both sea turtles; however, constituents of isoforms were different between green and hawksbill turtles. In both species, we observed the elevation of the height of a specific peak in elution profile with an increase in Cu concentration in hepatocytosol. This result suggests the presence of a novel MT isoform related to copper accumulation in the liver of sea turtles.
Zakaria, Philip; Dicinoski, Greg W; Ng, Boon Khing; Shellie, Robert A; Hanna-Brown, Melissa; Haddad, Paul R
2009-09-18
The ion-exchange separation of organic anions of varying molecular mass has been demonstrated using ion chromatography with isocratic, gradient and multi-step eluent profiles on commercially available columns with UV detection. A retention model derived previously for inorganic ions and based solely on electrostatic interactions between the analytes and the stationary phase was applied. This model was found to accurately describe the observed elution of all the anions under isocratic, gradient and multi-step eluent conditions. Hydrophobic interactions, although likely to be present to varying degrees, did not limit the applicability of the ion-exchange retention model. Various instrumental configurations were investigated to overcome problems associated with the use of organic modifiers in the eluent which caused compatibility issues with the electrolytically derived, and subsequently suppressed, eluent. The preferred configuration allowed the organic modifier stream to bypass the eluent generator, followed by subsequent mixing before entering the injection valve and column. Accurate elution prediction was achieved even when using 5-step eluent profiles with errors in retention time generally being less than 1% relative standard deviation (RSD) and all being less than 5% RSD. Peak widths for linear gradient separations were also modelled and showed good agreement with experimentally determined values.
Kumar, Sunil; Fusaro, Mario; Amoroso, Nicholas; Kirtane, Ajay J; Byrne, Robert A; Williams, David O; Slater, James; Cutlip, Donald E; Feit, Frederick
2012-01-01
Objectives To evaluate the efficacy and safety of currently used drug eluting stents compared with each other and compared with bare metal stents in patients with diabetes. Design Mixed treatment comparison meta-analysis. Data sources and study selection PubMed, Embase, and CENTRAL were searched for randomised clinical trials, until April 2012, of four durable polymer drug eluting stents (sirolimus eluting stents, paclitaxel eluting stents, everolimus eluting stents, and zotarolimus eluting stents) compared with each other or with bare metal stents for the treatment of de novo coronary lesions and enrolling at least 50 patients with diabetes. Primary outcomes Efficacy (target vessel revascularisation) and safety (death, myocardial infarction, stent thrombosis). Results From 42 trials with 22 844 patient years of follow-up, when compared with bare metal stents (reference rate ratio 1) all of the currently used drug eluting stents were associated with a significant reduction in target vessel revascularisation (37% to 69%), though the efficacy varied with the type of stent (everolimus eluting stents∼sirolimus eluting stents>paclitaxel eluting stents∼zotarolimus eluting stent>bare metal stents). There was about an 87% probability that everolimus eluting stents were the most efficacious compared with all others, though there were limited usable data for the zotarolimus eluting Resolute stent in patients with diabetes. Moreover, there was no increased risk of any safety outcome (including very late stent thrombosis) with any drug eluting stents compared with bare metal stents. There was about a 62% probability that the everolimus eluting stent was the safest stent for the outcome of “any” stent thrombosis. Conclusions Among patients with diabetes treated with coronary stents all currently available drug eluting stents were efficacious without compromising safety compared with bare metal stents. There were relative differences among the drug eluting stents, such that the everolimus eluting stent was the most efficacious and safe. PMID:22885395
Partial purification of the mu opioid receptor irreversibly labeled with (/sup 3/H)b-funaltrexamine
DOE Office of Scientific and Technical Information (OSTI.GOV)
Liu-Chen, L.Y.; Phillips, C.A.; Tam, S.W.
1986-03-01
The mu opioid receptor in bovine striatal membranes was specifically and irreversibly labeled by incubation with 5 nM (/sup 3/H)..beta..-funaltrexamine (approx.-FNA) at 37/sup 0/C for 90 min in the presence of 100 mM NaCl. The specific and irreversible binding of (/sup 3/H)..beta..-FNA as defined by that blocked by 1 /sup +/M naloxone was about 60% of total irreversible binding. The specific irreversible binding was saturable, stereospecific, time-, temperature, and tissue-dependent. Mu opioid ligands were much more potent than delta or kappa ligands in inhibiting the specific irreversible labeling. SDS polyacrylamide gel electrophoresis of solubilized membranes in the presence of 2-mercaptoethanolmore » yielded a major radiolabeled broad band of MW 68-97K daltons, characteristic of a glycoprotein band. This band was not observed in membranes labeled in the presence of excess unlabeled naloxone. The glycoprotein nature of the (/sup 3/H)..beta..-FNA-labeled opioid receptor was confirmed by its binding to a wheat germ agglutinin-Sepharose column and its elution with N-acetylglucosamine.« less
Mobile Three Frequency Radar as Research Platform for Precipitation Profiling
NASA Astrophysics Data System (ADS)
Schmidt, Walter; Rautiainen, Kimmo; Harri, Ari-Matti
2014-05-01
Precipitation profiling at the frequency bands of Ku, Ka and W bands are becoming increasingly popular in the studies of atmospheric microphysics. Ever since the introduction of Ku / Ka pair of frequencies for the Global Precipitation Measurement mission (GPM) and the success of W band in Cloudsat, the interest in precipitation profiling using these frequencies has increased. The profiling observations will also serve as ground validation instruments for several space missions such as GPM and EarthCARE [1]. In order to get better information to retrieve ice microphysics as well as to enhance sensitivity, we need to move from the standard S- and C-band weather radars to higher frequencies [2]. As was recently shown, the use of multi- frequency profiling yields important additional information compared to single-frequency radar mapping [3]. During the past four years a consortium of research, academic and private industries in Finland has been developing a flexible low-cost mobile three-band radar system for precipitation profiling. The feasibility of the concept is being demonstrated by implementing the Ku- and Ka-band part of the system. The antenna structure with antennas for Ku-, Ka- and W-band is completed allowing the pointing of all three antenna systems into the same direction during an azimuth and elevation scan. Using a freely programmable digital waveform generator and decoding electronics for the received data, the implementation of different wave form generation, compression and decoding schemes and their influence on the radar performance in the different bands can be evaluated and optimized. The modular design allows the connection of different transmitter control and receiver decoding units to any of the three band front-end electronics to evaluate the performance of different approaches in the various bands simultaneously. A real-time analysis software supports the data interpretation and system optimization during field tests. Via mobile internet connection and standard data formats the collected data can be made available for operative use. The mechanical integration on a standard car trailer allows the fast deployment to different locations. References [1] V. Chandrasekar, D. Moisseev, W. Schmidt, K. Rautiainen and A.-M Harri, "Scientific and engineering overview of the three frequency precipitation profiling radar at Helsinki" The 9th International Symposium on Advanced Environmental Monitoring and Modeling Helsinki, 2012. [2] V. Chandrasekar, H. Fukatsu and K. Mubarak, "Global mapping of attenuation at Ku- and Ka-band", IEEE Transactions on Geoscience and Remote Sensing, vol. 41, pp. 2166-2176, 2003 [3] J.Leinonen, D. Moisseev, V. Chandrasekar, J. Koskinen, "Mapping Radar Reflectivity Values of Snowfall Between Frequency Bands", IEEE Transactions on Geoscience and Remote Sensing, vol. 49, no.8, pp. 3047-3058, 2011 doi: 10.1109/TGRS.2011.2117432
Compton scattering studies and electronic properties of BaTiO3
NASA Astrophysics Data System (ADS)
Meena, Seema Kumari; Bapna, Komal; Heda, N. L.; Ahuja, B. L.
2018-04-01
We present the experimental momentum density of BaTiO3 measured using 20 Ci 137Cs Compton spectrometer. The experimental Compton profile (CP) has been compared with the linear combination of atomic orbitals (LCAO) based theoretical profiles for various exchange-correlation potentials. It is found that LCAO-B3PW based CP gives a better agreement with experiment than other theoretical profiles. We have also deduced the energy bands and density of states (DOS) for BaTiO3 using LCAO-B3PW scheme. The energy bands and DOS suggest an indirect band gap in the system arising due to O-2p states of valence band and Ti-3d states of conduction band. Peculiar electronic response of this system is found to be mainly due to hybridized states of Ba-5p/5s and O-2p orbitals.
Zone, J J; Taylor, T B; Kadunce, D P; Meyer, L J
1990-01-01
Linear IgA bullous dermatosis (LABD) is a rare blistering skin disease characterized by basement membrane zone deposition of IgA. This study identifies a tissue antigen detected by patient serum and then isolates the autoantibody using epidermis and protein bands blotted on nitrocellulose as immunoabsorbents. Sera from 10 patients (9 with cutaneous disease and 1 with cicatrizing conjunctivitis) were evaluated. Indirect immunofluorescence revealed an IgA anti-basement membrane antibody in 6 of 10 sera with monkey esophagus substrate and 9 of 10 sera with human epidermal substrate. Immunoblotting was performed on epidermal and dermal extracts prepared from skin separated at the basement membrane zone with either sodium chloride or EDTA. Saline-separated skin expressed a 97-kD band in dermal extract alone that was recognized by 4 of 10 sera. EDTA-separated skin expressed the 97-kD band in both epidermal (4 of 10 sera) and dermal (6 of 10 sera) extract. Immunoabsorption of positive sera with epidermis purified an IgA antibody that reacted uniquely with the 97-kD band. In addition, IgA antibody bound to nitrocellulose was eluted from the 97-kD band and found to uniquely bind basement membrane zone. It is likely that the 97-kD protein identified by these techniques is responsible for basement membrane binding of IgA in LABD. Images PMID:2107211
Sheng, Ning; Zheng, Hao; Xiao, Yao; Wang, Zhe; Li, Menglin; Zhang, Jinlan
2017-09-29
Chemical profile for Chinese medicine formulas composed of several herbs is always a challenge due to a big array of small molecules with high chemical diversity so much as isomers. The present paper develops a feasible strategy to characterize and identify complex chemical constituents of a four-herb traditional Chinese medicine formula, Denzhan Shenmai (DZSM) by integrating comprehensive two-dimensional liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC×LC-qTOF-MS) with multiple heart-cutting two-dimensional liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (MHC-qTOF-MS). DZSM was separated by C8×C18 HPLC column system for comprehensive two-dimensional liquid chromatography system and 283 compounds most of which belonged to phenolic acid, flavonoid, saponin and lignan families were characterized and identified within 75min. Some isomers and compounds at low level were analyzed on C8×Chiral HPLC column system for multiple heart-cutting two-dimensional liquid chromatography system with 1D and 2D optimized gradient elution program. These 1D cutting fractions were successively separated on 2D chiral chromatographic column under extended the 2D gradient elution time from 30s to 5.0min. 12 pairs of isomer compounds were separated with good resolution. The combination of LC×LC and MHC system provides a powerful technique for global chemical profiling of DZSM and provided feasible strategy for other complex systems. Copyright © 2017 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Strak, Pawel; Kempisty, Pawel; Sakowski, Konrad; Krukowski, Stanislaw
2014-09-01
Density functional theory studies were conducted to determine an influence of the carrier concentration on the optical and electronic properties of InN/GaN superlattice system. The oscillator strength values, energy gaps and the band profiles were obtained. The band profiles were found to be strongly affected for technically possible heavy n-type doping while for p-type doping the carrier influence, both screening and band shift, is negligible. Blue shift of the transition energy between conduction band minima and valence band maxima was observed for high concentrations of both type carriers.
A PROFILE ANALYSIS OF RAMAN-SCATTERED O VI BANDS AT 6825 Å AND 7082 Å IN SANDULEAK’S STAR
DOE Office of Scientific and Technical Information (OSTI.GOV)
Heo, Jeong-Eun; Lee, Hee-Won; Angeloni, Rodolfo
2016-12-20
We present a detailed modeling of the two broad bands observed at 6825 and 7082 Å in Sanduleak’s star, a controversial object in the Large Magellanic Cloud. These bands are known to originate from Raman scattering of O vi λ λ 1032 and 1038 photons with atomic hydrogen and are only observed in bona fide symbiotic stars. Our high-resolution spectrum obtained with the Magellan Inamori Kyocera Echelle spectrograph at the Magellan-Clay Telescope reveals, quite surprisingly, that the profiles of the two bands look very different: while the Raman 6825 Å band shows a single broad profile with a redward extendedmore » bump, the Raman 7082 Å band exhibits a distinct triple-peak profile. Our model suggests that the O vi emission nebula can be decomposed into a red, blue, and central emission region from an accretion disk, a bipolar outflow, and a further compact, optically thick region. We also perform Monte Carlo simulations with the aim of fitting the observed flux ratio F (6825)/ F (7082) ∼ 4.5, which indicates that the neutral region in Sanduleak’s star is characterized by the column density N{sub Hi} ∼ 1 × 10{sup 23} cm{sup −2}.« less
Cheng, Yanping; Gasior, Pawel; Shibuya, Masahiko; Ramzipoor, Kamal; Lee, Chang; Estrada, Edward A; Dokko, Daniell; McGregor, Jenn C; Conditt, Gerard B; Kaluza, Greg L; Granada, Juan F
2016-10-01
Clinically available bioresorbable scaffolds (BRS) rely on polymer crystallinity to achieve mechanical strength resulting in limited overexpansion capabilities and structural integrity when exposed to high-loading conditions. We aimed to evaluate the biomechanical behavior and vascular healing profile of a novel, sirolimus-eluting, high-molecular-weight, amorphous poly-l-lactic acid-based BRS (Amaranth BRS). In vitro biomechanical testing was performed under static and cyclic conditions. A total of 99 devices (65 Amaranth BRS versus 34 Absorb bioresorbable vascular scaffold [BVS]) were implanted in 99 coronary arteries of 37 swine for pharmacokinetics and healing evaluation at various time points. In the Absorb BVS, the number of fractures per scaffold seen on light microscopy was 6.0 (5.0-10.5) when overexpanded 1.0 mm above nominal values (≈34%). No fractures were observed in the Amaranth BRS group at 1.3 mm above nominal values (≈48% overexpansion). The number of fractures was higher in the Absorb BVS on accelerated cycle testing over time (at 24K cycles=5.0 [5.0-9.0] Absorb BVS versus 0.0 [0.0-0.5] Amaranth BRS). Approximately 90% of sirolimus was found to be eluted by 90 days. Optical coherence tomography analysis demonstrated lower percentages of late scaffold recoil in the Amaranth BRS at 3 months (Amaranth BRS=-10±16.1% versus Absorb BVS=10.7±13.2%; P=0.004). Histopathology analysis revealed comparable levels of vascular healing and inflammatory responses between both BRSs up to 6 months. New-generation high-molecular-weight amorphous poly-l-lactic acid scaffolds have the potential to improve the clinical performance of BRS and provide the ideal platform for the future miniaturization of the technology. © 2016 American Heart Association, Inc.
Williams, Christopher; Jensen, Mike
2012-11-06
This data was collected by the NOAA 449-MHz and 2.8-GHz profilers in support of the Department of Energy (DOE) and NASA sponsored Mid-latitude Continental Convective Cloud Experiment (MC3E). The profiling radars were deployed in Northern Oklahoma at the DOE Atmospheric Radiation Mission (ARM) Southern Great Plans (SGP) Central Facility from 22 April through 6 June 2011. NOAA deployed three instruments: a Parsivel disdrometer, a 2.8-GHz profiler, and a 449-MHz profiler. The parasivel provided surface estimates of the raindrop size distribution and is the reference used to absolutely calibrate the 2.8 GHz profiler. The 2.8-GHz profiler provided unattenuated reflectivity profiles of the precipitation. The 449-MHz profiler provided estimates of the vertical air motion during precipitation from near the surface to just below the freezing level. By using the combination of 2.8-GHz and 449-MHz profiler observations, vertical profiles of raindrop size distributions can be retrieved. The profilers are often reference by their frequency band: the 2.8-GHz profiler operates in the S-band and the 449-MHz profiler operates in the UHF band. The raw observations are available as well as calibrated spectra and moments. This document describes how the instruments were deployed, how the data was collected, and the format of the archived data.
Mori, Tadashi; Tanaka, Takayuki; Higashino, Tomohiro; Yoshida, Kota; Osuka, Atsuhiro
2016-06-23
Intrinsically chiral Möbius aromatic [28]hexaphyrin monophosphorus(V) and Möbius antiaromatic [30]hexaphyrin bisphosphorus(V) complexes have been optically resolved and their absolute configurations (ACs) were determined by combined experimental and theoretical investigations on their circular dichroisms (CDs). First elutes in chiral HPLC exhibited strong positive Cotton effects (CEs) at the B-band, characteristic for the ML configurations in their Möbius strips. Weak CEs at the Q-band, if attainable, complemented their AC assignment. The whole CD pattern and intensity were well reproduced by time-dependent approximate coupled cluster theory using model systems that omit five outward meso-aryl substituents (inward-meso-retained model), providing a solid basis for AC assignment. The cost efficient TD-DFT method with appropriate functionals for fully substituted (nontruncated) complexes well reproduced CEs around the B-band (but less satisfactory at the Q-band), also allows the rapid AC estimation for their Möbius strips. Observed difference in CDs between aromatic and antiaromatic hexaphyrins were better interpreted by their shifts in energy levels and altered interactions of relevant molecular orbitals, rather than small differences in Möbius geometries nor aromatic/antiaromatic character, despite the correlations recently claimed in planar π-systems.
Azadniya, Ebrahim; Morlock, Gertrud E
2018-01-19
An affordable bioanalytical workflow supports the collection of data on active ingredients, required for the understanding of health-related food, superfood and traditional medicines. Targeted effect-directed responses of single compounds in a complex sample highlight this powerful bioanalytical hyphenation of planar chromatography with (bio)assays. Among many reports about biological properties of Salvia miltiorrhiza Bunge root (Danshen) and their analytical methods, the highly efficient direct bioautography (DB) workflow has not been considered so far. There was just one TLC-acetylcholinesterase (AChE) method with a poor zone resolution apart from our two HPTLC-DB studies, however, all methods were focused on the nonpolar extracts of Danshen (tanshinones) only. The current study on HPTLC-UV/Vis/FLD-(bio)assay-HRMS, followed by streamlined scale-up to preparative layer chromatography (PLC)- 1 H-NMR, aimed at an even more streamlined, yet comprehensive bioanalytical workflow. It comprised effect-directed screening of both, its polar (containing phenolics) and nonpolar extracts (containing tanshinones) on the same HPTLC plate, the biochemical and biological profiling with four different (bio)assays and elucidation of structures of known and unidentified active compounds. The five AChE inhibitors, salvianolic acid B (SAB), lithiospermic acid (LSA) and rosmarinic acid (RA) as well as cryptotanshinone (CT) and 15,16-dihydrotanshinone I (DHTI) were confirmed, but also unidentified inhibitors were observed. In the polar extracts, SAB, LSA and RA exhibited free radical scavenging properties in the 2,2-diphenyl-1-picrylhydrazyl assay. CT, DHTI and some unidentified nonpolar compounds were found active against Gram-positive Bacillus subtilis and Gram-negative Aliivibrio fischeri (LOD 12 ng/band for CT, and 5 ng/band for DHTI). For the first time, the most multipotent unidentified active compound zone in the B. subtilis, A. fischeri and AChE fingerprints of the nonpolar Danshen extract was identified as co-eluted band of 1,2-dihydrotanshinone and methylenetanshinquinone in the ratio of 2:1. Copyright © 2017 Elsevier B.V. All rights reserved.
Gritti, Fabrice; Guiochon, Georges
2013-03-22
The adsorption behaviors of a neutral (caffeine) and a positively charged compound (nortriptylinium) are investigated on two RPLC/hybrid stationary phases, eluted with a low ionic strength buffer (phosphate buffer, W(S)pH 2.63, I=10mM). The first phase, bridge ethylene hybrid (BEH), is neutral at all pHs whereas the second, charged surface hybrid (CSH), contains a protonated ligand at W(W)pH <7. The band profiles of these two compounds eluted by mixture of acetonitrile and water were recorded under overloaded conditions. The adsorption isotherms of the neutral compound on both columns were well accounted for by a heterogeneous Linear-Langmuir (LL) model, which has an adsorption-desorption equilibrium constants about twice larger for caffeine on the CSH than on the BEH, due to charge-dipole interactions. In contrast, at low loadings (0.3 and 1.2μL, C=30g/L), the adsorption isotherm of the charged compound can be accounted for by a homogeneous electrostatically modified Langmuir (EML) or by a heterogeneous bi-EML implicit isotherms onto the CSH and BEH adsorbent, respectively. Electrostatic repulsions definitely account the lesser retention of the ionizable compound on CSH than on BEH. This is explained by the surface potential of CSH-C18 at 20mV and by the subsequent decrease of the equilibrium constant of weak adsorption sites (C18 environment) and removal of the strong adsorption sites (accessible silanols). At the highest sample loadings (5 and 20μL, C=30g/L), the EML and the bi-EML isotherms failed because some adsorbate-adsorbate interactions take place when bulk concentrations exceed 0.2g/L. The experimental data were then successively fitted to an empirical heterogeneous Langmuir-Moreau (LM) explicit isotherm. The best saturation capacities of the empirical heterogeneous LM isotherm is consistent with the manufacturer's estimate of the surface concentration of residual silanols onto the BEH- and CSH-C18 endcapped adsorbent (<0.1μmol/m(2)). Copyright © 2013 Elsevier B.V. All rights reserved.
Metal release profiles of orthodontic bands, brackets, and wires: an in vitro study.
Wendl, B; Wiltsche, H; Lankmayr, E; Winsauer, H; Walter, A; Muchitsch, A; Jakse, N; Wendl, M; Wendl, T
2017-11-01
The present study evaluated the temporal release of Co Cr, Mn, and Ni from the components of a typical orthodontic appliance during simulated orthodontic treatment. Several commercially available types of bands, brackets, and wires were exposed to an artificial saliva solution for at least 44 days and the metals released were quantified in regular intervals using inductively coupled plasma quadrupole mass spectrometry (ICP-MS, Elan DRC+, Perkin Elmer, USA). Corrosion products encountered on some products were investigated by a scanning electron microscope equipped with an energy dispersive X-ray microanalyzer (EDX). Bands released the largest quantities of Co, Cr, Mn, and Ni, followed by brackets and wires. Three different temporal metal release profiles were observed: (1) constant, though not necessarily linear release, (2) saturation (metal release stopped after a certain time), and (3) an intermediate release profile that showed signs of saturation without reaching saturation. These temporal metal liberation profiles were found to be strongly dependent on the individual test pieces. The corrosion products which developed on some of the bands after a 6-month immersion in artificial saliva and the different metal release profiles of the investigated bands were traced back to different attachments welded onto the bands. The use of constant release rates will clearly underestimate metal intake by the patient during the first couple of days and overestimate exposure during the remainder of the treatment which is usually several months long. While our data are consistent with heavy metal release by orthodontic materials at levels well below typical dietary intake, we nevertheless recommend the use of titanium brackets and replacement of the band with a tube in cases of severe Ni or Cr allergy.
NASA Astrophysics Data System (ADS)
Cui, Ning; Liang, Renrong; Wang, Jing; Xu, Jun
2012-06-01
Choosing novel materials and structures is important for enhancing the on-state current in tunnel field-effect transistors (TFETs). In this paper, we reveal that the on-state performance of TFETs is mainly determined by the energy band profile of the channel. According to this interpretation, we present a new concept of energy band profile modulation (BPM) achieved with gate structure engineering. It is believed that this approach can be used to suppress the ambipolar effect. Based on this method, a Si TFET device with a symmetrical tri-material-gate (TMG) structure is proposed. Two-dimensional numerical simulations demonstrated that the special band profile in this device can boost on-state performance, and it also suppresses the off-state current induced by the ambipolar effect. These unique advantages are maintained over a wide range of gate lengths and supply voltages. The BPM concept can serve as a guideline for improving the performance of nanoscale TFET devices.
Williams, Christopher; Jensen, Mike
2012-11-06
This data was collected by the NOAA 449-MHz and 2.8-GHz profilers in support of the Department of Energy (DOE) and NASA sponsored Mid-latitude Continental Convective Cloud Experiment (MC3E). The profiling radars were deployed in Northern Oklahoma at the DOE Atmospheric Radiation Mission (ARM) Southern Great Plans (SGP) Central Facility from 22 April through 6 June 2011. NOAA deployed three instruments: a Parsivel disdrometer, a 2.8-GHz profiler, and a 449-MHz profiler. The parasivel provided surface estimates of the raindrop size distribution and is the reference used to absolutely calibrate the 2.8 GHz profiler. The 2.8-GHz profiler provided unattenuated reflectivity profiles of the precipitation. The 449-MHz profiler provided estimates of the vertical air motion during precipitation from near the surface to just below the freezing level. By using the combination of 2.8-GHz and 449-MHz profiler observations, vertical profiles of raindrop size distributions can be retrieved. The profilers are often reference by their frequency band: the 2.8-GHz profiler operates in the S-band and the 449-MHz profiler operates in the UHF band. The raw observations are available as well as calibrated spectra and moments. This document describes how the instruments were deployed, how the data was collected, and the format of the archived data.
Williams, Christopher; Jensen, Mike
2012-11-06
This data was collected by the NOAA 449-MHz and 2.8-GHz profilers in support of the Department of Energy (DOE) and NASA sponsored Mid-latitude Continental Convective Cloud Experiment (MC3E). The profiling radars were deployed in Northern Oklahoma at the DOE Atmospheric Radiation Mission (ARM) Southern Great Plans (SGP) Central Facility from 22 April through 6 June 2011. NOAA deployed three instruments: a Parsivel disdrometer, a 2.8-GHz profiler, and a 449-MHz profiler. The parasivel provided surface estimates of the raindrop size distribution and is the reference used to absolutely calibrate the 2.8 GHz profiler. The 2.8-GHz profiler provided unattenuated reflectivity profiles of the precipitation. The 449-MHz profiler provided estimates of the vertical air motion during precipitation from near the surface to just below the freezing level. By using the combination of 2.8-GHz and 449-MHz profiler observations, vertical profiles of raindrop size distributions can be retrieved. The profilers are often reference by their frequency band: the 2.8-GHz profiler operates in the S-band and the 449-MHz profiler operates in the UHF band. The raw observations are available as well as calibrated spectra and moments. This document describes how the instruments were deployed, how the data was collected, and the format of the archived data.
Williams, Christopher; Jensen, Mike
2012-11-06
This data was collected by the NOAA 449-MHz and 2.8-GHz profilers in support of the Department of Energy (DOE) and NASA sponsored Mid-latitude Continental Convective Cloud Experiment (MC3E). The profiling radars were deployed in Northern Oklahoma at the DOE Atmospheric Radiation Mission (ARM) Southern Great Plans (SGP) Central Facility from 22 April through 6 June 2011. NOAA deployed three instruments: a Parsivel disdrometer, a 2.8-GHz profiler, and a 449-MHz profiler. The parasivel provided surface estimates of the raindrop size distribution and is the reference used to absolutely calibrate the 2.8 GHz profiler. The 2.8-GHz profiler provided unattenuated reflectivity profiles of the precipitation. The 449-MHz profiler provided estimates of the vertical air motion during precipitation from near the surface to just below the freezing level. By using the combination of 2.8-GHz and 449-MHz profiler observations, vertical profiles of raindrop size distributions can be retrieved. The profilers are often reference by their frequency band: the 2.8-GHz profiler operates in the S-band and the 449-MHz profiler operates in the UHF band. The raw observations are available as well as calibrated spectra and moments. This document describes how the instruments were deployed, how the data was collected, and the format of the archived data.
Thoß, M.; Luzynski, K.C.; Ante, M.; Miller, I.; Penn, D.J.
2016-01-01
House mice (Mus musculus) produce a variable number of major urinary proteins (MUPs), and studies suggest that each individual produces a unique MUP profile that provides a distinctive odor signature controlling individual and kin recognition. This ‘barcode hypothesis’ requires that MUP urinary profiles show high individual variability within populations and also high individual consistency over time, but tests of these assumptions are lacking. We analyzed urinary MUP profiles of 66 wild-caught house mice from eight populations using isoelectric focusing. We found that MUP profiles of wild male house mice are not individually unique, and though they were highly variable, closer inspection revealed that the variation strongly depended on MUP band type. The prominent (‘major) bands were surprisingly homogenous (and hence most MUPs are not polymorphic), but we also found inconspicuous (‘minor’) bands that were highly variable and therefore potential candidates for individual fingerprints. We also examined changes in urinary MUP profiles of 58 males over time (from 6 to 24 weeks of age), and found that individual MUP profiles and MUP concentration were surprisingly dynamic, and showed significant changes after puberty and during adulthood. Contrary to what we expected, however, the minor bands were the most variable over time, thus no good candidates for individual fingerprints. Although MUP profiles do not provide individual fingerprints, we found that MUP profiles were more similar among siblings than non-kin despite considerable fluctuation. Our findings show that MUP profiles are not highly stable over time, they do not show strong individual clustering, and thus challenge the barcode hypothesis. Within-individual dynamics of MUP profiles indicate a different function of MUPs in individual recognition than previously assumed and advocate an alternative hypothesis (‘dynamic changes’ hypothesis). PMID:26973837
Thoß, M; Luzynski, K C; Ante, M; Miller, I; Penn, D J
2015-06-30
House mice ( Mus musculus) produce a variable number of major urinary proteins (MUPs), and studies suggest that each individual produces a unique MUP profile that provides a distinctive odor signature controlling individual and kin recognition. This 'barcode hypothesis' requires that MUP urinary profiles show high individual variability within populations and also high individual consistency over time, but tests of these assumptions are lacking. We analyzed urinary MUP profiles of 66 wild-caught house mice from eight populations using isoelectric focusing. We found that MUP profiles of wild male house mice are not individually unique, and though they were highly variable, closer inspection revealed that the variation strongly depended on MUP band type. The prominent ('major) bands were surprisingly homogenous (and hence most MUPs are not polymorphic), but we also found inconspicuous ('minor') bands that were highly variable and therefore potential candidates for individual fingerprints. We also examined changes in urinary MUP profiles of 58 males over time (from 6 to 24 weeks of age), and found that individual MUP profiles and MUP concentration were surprisingly dynamic, and showed significant changes after puberty and during adulthood. Contrary to what we expected, however, the minor bands were the most variable over time, thus no good candidates for individual fingerprints. Although MUP profiles do not provide individual fingerprints, we found that MUP profiles were more similar among siblings than non-kin despite considerable fluctuation. Our findings show that MUP profiles are not highly stable over time, they do not show strong individual clustering, and thus challenge the barcode hypothesis. Within-individual dynamics of MUP profiles indicate a different function of MUPs in individual recognition than previously assumed and advocate an alternative hypothesis ('dynamic changes' hypothesis).
Cao, Xueli; Wang, Qiaoe; Li, Yan; Bai, Ge; Ren, Hong; Xu, Chunming; Ito, Yoichiro
2011-03-01
Counter-current chromatography (CCC) combined with pre-separation by ultrasonic solvent extraction was successively used for the separation of series bioactive compounds from the crude extract of Hypericum perforatum L. The petroleum ether extract was separated by the solvent system of n-heptane-methanol-acetonitrile (1.5:0.5:0.5, v/v) and n-heptane-methanol (1.5:1, v/v) in gradient elution, yielding a phloroglucinol compound, hyperforin with HPLC purity over 98%. The ethyl acetate extract was separated by using the solvent system composed of hexane-ethyl acetate-methanol-water (1:1:1:1 and 1:3:1:3, v/v) in gradient through both reverse phase and normal phase elution mode, yielding a naphthodianthrone compound, hypericin with HPLC purity about 95%. The n-butanol extract was separated with the solvent system composed of n-butanol-ethyl acetate-water (1:4:5 and 1.5:3.5:5, v/v) in elution and back-extrusion mode, yielding two of flavones, rutin and hyperoside, with HPLC purity over 95%. HPLC-MS, reference sample and UV spectrum were selectively used in separation to search for target compounds from HPLC-DAD profiles of different sub-extracts. The structures of isolated compounds were further identified by ESI-MS, ¹HNMR and ¹³CNMR. Copyright © 2011 Elsevier B.V. All rights reserved.
Center, S A; Thompson, M; Guida, L
1993-05-01
Concentrations of 3 alpha-hydroxylated bile acids were measured in serum and urine of clinically normal (healthy) cats (n = 6), cats with severe hepatic lipidosis (n = 9), and cats with complete bile duct occlusion (n = 4). Bile acid concentrations were measured by use of a gradient flow high-performance liquid chromatography procedure with an acetonitrile and ammonium phosphate mobile phase and an in-line postanalytic column containing 3 alpha-hydroxy-steroid dehydrogenase and a fluorescence detector. Specific identification of all bile acid peaks was not completed; unidentified moieties were represented in terms of their elution time (in minutes). Significant differences in serum and urine bile acid concentrations, quantitative and proportional, were determined among groups of cats. Cats with hepatic lipidosis and bile duct occlusion had significantly (P > or = 0.05) greater total serum and urine bile acids concentrations than did healthy cats. The proportion of hydrophobic bile acids in serum, those eluting at > or = 400 minutes, was 1.9% for healthy cats, 3.3% for cats with lipidosis, and 5.4% for bile duct-obstructed cats. Both groups of ill cats had a broader spectrum of unidentified late-eluting serum bile acids than did healthy cats; the largest spectrum developed in bile duct-occluded cats.(ABSTRACT TRUNCATED AT 250 WORDS)
Kisley, Lydia; Chen, Jixin; Mansur, Andrea P.; Dominguez-Medina, Sergio; Kulla, Eliona; Kang, Marci; Shuang, Bo; Kourentzi, Katerina; Poongavanam, Mohan-Vivekanandan; Dhamane, Sagar; Willson, Richard C.; Landes, Christy F.
2014-01-01
The retention and elution of proteins in ion-exchange chromatography is routinely controlled by adjusting the mobile phase salt concentration. It has repeatedly been observed, as judged from adsorption isotherms, that the apparent heterogeneity of adsorption is lower at more-eluting, higher ionic strength. Here, we present an investigation into the mechanism of this phenomenon using a single-molecule, super-resolution imaging technique called motion-blur Points Accumulation for Imaging in Nanoscale Topography (mbPAINT). We observed that the number of functional adsorption sites was smaller at high ionic strength and that these sites had reduced desorption kinetic heterogeneity, and thus narrower predicted elution profiles, for the anion-exchange adsorption of α-lactalbumin on an agarose-supported, clustered-charge ligand stationary phase. Explanations for the narrowing of the functional population such as inter-protein interactions and protein or support structural changes were investigated through kinetic analysis, circular dichroism spectroscopy, and microscopy of agarose microbeads, respectively. The results suggest the reduction of heterogeneity is due to both electrostatic screening between the protein and ligand and tuning the steric availability within the agarose support. Overall, we have shown that single molecule spectroscopy can aid in understanding the influence of ionic strength on the population of functional adsorbent sites participating in the ion-exchange chromatographic separation of proteins. PMID:24751557
Cao, Xueli; Wang, Qiaoe; Li, Yan; Bai, Ge; Ren, Hong; Ito, Yiochiro
2011-01-01
High-speed counter-current chromatography (HSCCC) combined with pre-separation by ultrasonic solvent extraction was successively used for the separation of series bioactive compounds from the crude extract of Hypericum perforatum L. The petroleum ether extract was separated by the solvent system of n-heptane-methanol-acetonitrile (1.5:0.5:0.5, v/v) and n-heptane-methanol (1.5:1, v/v) in gradient elution, yielding a phloroglucinol compound, hyperforin with HPLC purity over 98%. The ethyl acetate extract was separated by using the solvent system composed of hexane-ethyl acetate-methanol-water (1:1:1:1 and 1:3:1:3, v/v) in gradient through both reverse phase and normal phase elution mode, yielding a naphthodianthrone compound, hypericin with HPLC purity about 95%. The n-butanol extract was separated with the solvent system composed of n-butanol-ethyl acetate–water (1:4:5 and 1.5:3.5:5, v/v) in elution and back-extrusion mode, yielding two of flavones, rutin and hyperoside, with HPLC purity over 95%. HPLC-MS, reference sample and UV spectrum were selectively used in separation to search for target compounds from HPLC-DAD profiles of different sub-extracts. The structures of isolated compounds were further identified by ESI-MS, 1HNMR and 13CNMR. PMID:21306961
Infrared diffuse interstellar bands
NASA Astrophysics Data System (ADS)
Galazutdinov, G. A.; Lee, Jae-Joon; Han, Inwoo; Lee, Byeong-Cheol; Valyavin, G.; Krełowski, J.
2017-05-01
We present high-resolution (R ˜ 45 000) profiles of 14 diffuse interstellar bands in the ˜1.45 to ˜2.45 μm range based on spectra obtained with the Immersion Grating INfrared Spectrograph at the McDonald Observatory. The revised list of diffuse bands with accurately estimated rest wavelengths includes six new features. The diffuse band at 15 268.2 Å demonstrates a very symmetric profile shape and thus can serve as a reference for finding the 'interstellar correction' to the rest wavelength frame in the H range, which suffers from a lack of known atomic/molecular lines.
SDS-PAGE Electrophoretic Property of Human Chorionic Gonadotropin (hCG) and its β-subunit
2005-01-01
The microheterogeneity property of hCG with regards to its sialic acid contents resulted in variable mobility of the glycoprotein in SDS-PAGE. The intact hCG molecule is composed of two dissimilar subunits, namely α- and β-subunits. The identification of hCG bands in SDS-PAGE was accomplished by the immunoblotting experiment, whereby the antibody directed toward the specific region of β-subunit of hCG was used. The data shows that the different mobility of intact hCG was attributed to the different degree of desialylation of the glycoprotein. Nevertheless, unlike the intact hCG, the mobility of its β-subunit was not affected by its variety sialic acid content. This characteristic of β-hCG is beneficial when semi-quantification of total hCG is required. Quantification of hCG using the HPLC-reversed phase C18 analytical column is not possible as the glycoprotein was eluted in multiple fractions at different retention times. The identification of denatured hCG (HPLC eluted fractions) was carried out by immunoblotting experiment whilst immunoassay technique failed to detect its presence in any fraction. PMID:16094462
Ferritin (FER), isoferritins and aluminum
DOE Office of Scientific and Technical Information (OSTI.GOV)
Fleming, J.; Cho, S.W.; Clauberg, M.
FER from Alzheimer's brain contains more Al. One source of Al is beverages. Of the several common beverages analyzed, Pepsi, sold in bottles but not in cans, contained the highest conc. of Al (10..mu..M). Male albino rats were fed 10..mu..M Al in drinking water for one year. They were then sacrificed and their brain homogenates were analyzed for FER, Al and several enzymes. The results: compared to controls, the homogenates of the Al fed rats had 276.5% more Al bound to Fer (114.2 +/- 25.3 g atoms/mol) and 30% less hexokinase activity (150 units/mg protein). Acetyl choline esterase and alkalinemore » ribonuclease levels remained unchanged. Isoelectrofocusing (pH 4-6.5) of human-brain FER yielded at least five bands. None corresponded with those from human liver FER or horse spleen FER. Horse spleen FER was applied to DEAE sephadex and eluted by NaCl-batchwise gradient. Five distinct fractions were obtained. The most acidic eluted last. It contained least Fe, tended to precipitate on standing and required less Al or Be to ppt. Thus, isoferritins may differ in their metal binding capacity and perhaps in their related physiological functions.« less
Electronic properties of CdWO{sub 4}: Use of hybrid exchange and correlation functionals
DOE Office of Scientific and Technical Information (OSTI.GOV)
Meena, B. S., E-mail: bsmphysics@gmail.com; Mund, H. S.; Ahuja, B. L.
Energy bands, density of states (DOS), Mulliken population (MP) and electron momentum densities (EMDs) of CdWO{sub 4} are presented using hybrid exchange and correlation functionals namely B3LYP, B3PW and PBE0. To validate the present hybrid potentials, theoretical EMDs have been compared with the experimental Compton profile. It is found that LCAO-B3LYP based Compton profile gives a better agreement with experiment than other theoretical profiles. The energy bands and DOS show a wide band gap semiconducting nature of CdWO{sub 4}. The theoretical band gap obtained using B3LYP scheme reconciles well with the available experimental data. In addition, we have also presentedmore » the anisotropies in EMDs along [100], [110] and [001] directions and the bonding effects using the MP data.« less
Selection of an Aptamer Antidote to the Anticoagulant Drug Bivalirudin
Martin, Jennifer A.; Parekh, Parag; Kim, Youngmi; Morey, Timothy E.; Sefah, Kwame; Gravenstein, Nikolaus; Dennis, Donn M.; Tan, Weihong
2013-01-01
Adverse drug reactions, including severe patient bleeding, may occur following the administration of anticoagulant drugs. Bivalirudin is a synthetic anticoagulant drug sometimes employed as a substitute for heparin, a commonly used anticoagulant that can cause a condition called heparin-induced thrombocytopenia (HIT). Although bivalrudin has the advantage of not causing HIT, a major concern is lack of an antidote for this drug. In contrast, medical professionals can quickly reverse the effects of heparin using protamine. This report details the selection of an aptamer to bivalirudin that functions as an antidote in buffer. This was accomplished by immobilizing the drug on a monolithic column to partition binding sequences from nonbinding sequences using a low-pressure chromatography system and salt gradient elution. The elution profile of binding sequences was compared to that of a blank column (no drug), and fractions with a chromatographic difference were analyzed via real-time PCR (polymerase chain reaction) and used for further selection. Sequences were identified by 454 sequencing and demonstrated low micromolar dissociation constants through fluorescence anisotropy after only two rounds of selection. One aptamer, JPB5, displayed a dose-dependent reduction of the clotting time in buffer, with a 20 µM aptamer achieving a nearly complete antidote effect. This work is expected to result in a superior safety profile for bivalirudin, resulting in enhanced patient care. PMID:23483901
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bowen, W.D.; Kooper, G.
1986-01-01
Opiate receptors from whole rat brain (minus cerebellum) and cow striatum were labeled irreversibly using the intrinsic photolability of /sup 3/H-etorphine. After incubation with 2 nM /sup 3/H-etorphine and centrifugal washing, membranes were irradiated with light of 254 nm. Non-specific binding was determined by carrying out incubations in presence and absence of 10 microM levallorphan. Specific binding in photolabeled membranes was 75-80%, with a photo-incorporation yield of approximately 50%. Photolabeled membranes were extracted with CHAPS/Lubrol and unbound /sup 3/H-etorphine was removed by dialysis and passage over Sephadex G-25. Solubilized proteins were then subjected to chromatography on wheat germ agglutinin, andmore » retained proteins were eluted with N-acetyl D-glucosamine (NAG). Protein profiles from rat brain and cow striatum were identical, with 89% of the total protein flowing through unretained and 11% eluted by NAG. However, the profile of radioactivity was markedly different in the two species. With rat, the specific activity (cpm/A280) was the same for flow-through and NAG-eluate. With cow, the specific activity of the NAG-eluate was 17 times greater than the flow-through. These results indicate that cow striatum and rat whole brain contain populations of opiate receptors which are glycosylated differently.« less
Taibon, Judith; Sturm, Sonja; Seger, Christoph; Parth, Martin; Strasser, Hermann; Stuppner, Hermann
2014-11-01
A fast and selective ultrahigh-performance liquid chromatography diode array detector (UHPLC-DAD) method combined with an off-line solid phase extraction (SPE) protocol was established to monitor destruxins (dtxs), a secondary metabolite class of highly bioactive cyclic depsipeptides. Sample purification via SPE was tailored to remove both more polar and apolar matrix constituents by applying analyte class-selective washing and elution conditions. To separate and detect destruxin congeners an UHPLC-DAD system hyphenated to a quadrupole-time-of-flight (Q-TOF) hybrid mass spectrometer was utilized. Analyses were performed on a sub-2-μm-particle-size RP-18 column with an acidified (0.02% acetic acid) 12 min water/acetonitrile solvent gradient. In the dtx congener elution zone 22 chromatographic peaks were separated. Four of these were identified by comparison with reference materials as dtx A, dtx B, dtx E, and dtx E-diol; 16 were tentatively assigned as known or novel dtx congeners by the analysis of high resolution UHPLC-DAD-QTOF-MS/MS data recorded in the positive electrospray ionization (ESI) mode. The applicability of the UHPLC-DAD assay to investigate biological materials in a qualitative and quantitative manner was proven by the application of the platform to monitor the dtx production profile of three Metarhizium brunneum strain fungal culture broths.
Lemaire, Julien; Blanc, Claire-Line; Lutin, Florence; Théoleyre, Marc-André; Stambouli, Moncef; Pareau, Dominique
2016-08-05
Bio-based organic acids are promising renewable carbon sources for the chemical industry. However energy-consuming purification processes are used, like distillation or crystallization, to reach high purities required in some applications. That is why preparative chromatography was studied as an alternative separation technique. In a previous work dealing with the purification of lactic, succinic and citric acids, the Langmuir model was insufficient to explain the elution profiles obtained with a strong anionic resin. Consequently the Langmuir model was coupled with a usual ion-exchange model to take into account the retention of their conjugate bases (<2%), which are commonly neglected at low pH (<1.5). Elution simulations with both uptake mechanisms fitted very well with experimental pulse tests. Only two parameters were optimized (equilibrium constant of acid uptake and ion-exchange selectivity coefficient of conjugate base) and their value were coherent with experimental and resin suppliers' data. These results confirmed that the singular tailing and apparent delay observed with succinic and citric acids can be explained by the high affinity of succinate and citrate for resin cationic sites. The model was implemented in a preparative chromatography simulation program in order to optimize operating parameters of our pilot-scale ISMB unit (Improved Simulated Moving Bed). The comparison with experimental ISMB profiles was conclusive. Copyright © 2016 Elsevier B.V. All rights reserved.
Study of the isotopic features of Swan bands in comets
NASA Technical Reports Server (NTRS)
Krishna Swamy, K. S.
1987-01-01
It is shown from a detailed statistical equilibrium calculation of the (C-12)(C-13) molecule that the interpretation of the observed intensities of Swan bands of the normal and the isotopic molecule of C2 in terms of the abundance ratio of C-12 and C-13 is a reasonable one. The synthetic profile of some isotopic features in the (0.0) Swan band is compared with the observed profiles for comet West.
Endovascular Gene Delivery from a Stent Platform: Gene- Eluting Stents
Fishbein, Ilia; Chorny, Michael; Adamo, Richard F; Forbes, Scott P; Corrales, Ricardo A; Alferiev, Ivan S; Levy, Robert J
2015-01-01
A synergistic impact of research in the fields of post-angioplasty restenosis, drug-eluting stents and vascular gene therapy over the past 15 years has shaped the concept of gene-eluting stents. Gene-eluting stents hold promise of overcoming some biological and technical problems inherent to drug-eluting stent technology. As the field of gene-eluting stents matures it becomes evident that all three main design modules of a gene-eluting stent: a therapeutic transgene, a vector and a delivery system are equally important for accomplishing sustained inhibition of neointimal formation in arteries treated with gene delivery stents. This review summarizes prior work on stent-based gene delivery and discusses the main optimization strategies required to move the field of gene-eluting stents to clinical translation. PMID:26225356
A simple method of obtaining concentration depth-profiles from X-ray diffraction
NASA Technical Reports Server (NTRS)
Wiedemann, K. E.; Unnam, J.
1984-01-01
The construction of composition profiles from X-ray intensity bands was investigated. The intensity band-to-composition profile transformation utilizes a solution which can be easily evaluated. The technique can be applied to thin films and thick speciments for which the variation of lattice parameters, linear absorption coefficient, and reflectivity with composition are known. A deconvolution scheme with corrections for the instrumental broadening and ak-alfadoublet is discussed.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Kao, Kuo-Hsing; Meyer, Kristin De; Department of Electrical Engineering, KU Leuven, Leuven
Band-to-band tunneling parameters of strained indirect bandgap materials are not well-known, hampering the reliability of performance predictions of tunneling devices based on these materials. The nonlocal band-to-band tunneling model for compressively strained SiGe is calibrated based on a comparison of strained SiGe p-i-n tunneling diode measurements and doping-profile-based diode simulations. Dopant and Ge profiles of the diodes are determined by secondary ion mass spectrometry and capacitance-voltage measurements. Theoretical parameters of the band-to-band tunneling model are calculated based on strain-dependent properties such as bandgap, phonon energy, deformation-potential-based electron-phonon coupling, and hole effective masses of strained SiGe. The latter is determined withmore » a 6-band k·p model. The calibration indicates an underestimation of the theoretical electron-phonon coupling with nearly an order of magnitude. Prospects of compressively strained SiGe tunneling transistors are made by simulations with the calibrated model.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Victoria, E.J.; Pierce, S.W.; Branks, M.J.
1990-01-01
Red blood cell (RBC) autoantibodies from patients with IgG warm-type autoimmune hemolytic anemia were labeled with iodine 125 and their RBC binding behavior characterized. Epitope-bearing RBC membrane polypeptides were identified after autoantibody immunoprecipitation of labeled membranes and immunoblotting. Immunoaffinity isolation of labeled membrane proteins with 12 different IgG hemolytic autoantibodies with protein A-agarose revealed a major polypeptide at Mr 95 to 110 kd, which coelectrophoresed on sodium dodecylsulfate-polyacrylamide gel electrophoresis with a membrane component isolated with sheep IgG anti-band 3. Immunoprecipitation studies with chymotrypsinized RBCs resulted in the recovery of two labeled membrane polypeptides with molecular weights characteristically resulting frommore » the chymotryptic fragmentation of band 3. Immunoblotting with sheep IgG anti-band 3 of the immunoprecipitated polypeptides confirmed that hemolytic autoantibody binding led to recovery of band 3 or its fragments. Two 125I-labeled IgG hemolytic autoantibodies showed binding behavior consistent with epitope localization on band 3. The labeled RBC autoantibodies bound immunospecifically to all types of human RBC tested, including those of rare Rh type (Rh-null, D--) at a site density of approximately 10(6) per RBC. The 125I-IgG in two labeled autoantibodies was 84% and 92% adsorbable by human and higher nonhuman primate RBCs. Antigen-negative animal RBC bound less than 10%, consistent with immunospecific RBC binding. IgG-1 was the major subclass in five autoantibodies tested; one of six fixed complement; and autoantibody IgG appeared polyclonal by isoelectric focusing. We conclude that IgG eluted from RBCs of patients with autoimmune hemolytic anemia consists predominantly of a single totally RBC-adsorbable antibody population that binds to antigenic determinants on band 3.« less
Quantitative operando visualization of the energy band depth profile in solar cells.
Chen, Qi; Mao, Lin; Li, Yaowen; Kong, Tao; Wu, Na; Ma, Changqi; Bai, Sai; Jin, Yizheng; Wu, Dan; Lu, Wei; Wang, Bing; Chen, Liwei
2015-07-13
The energy band alignment in solar cell devices is critically important because it largely governs elementary photovoltaic processes, such as the generation, separation, transport, recombination and collection of charge carriers. Despite the expenditure of considerable effort, the measurement of energy band depth profiles across multiple layers has been extremely challenging, especially for operando devices. Here we present direct visualization of the surface potential depth profile over the cross-sections of operando organic photovoltaic devices using scanning Kelvin probe microscopy. The convolution effect due to finite tip size and cantilever beam crosstalk has previously prohibited quantitative interpretation of scanning Kelvin probe microscopy-measured surface potential depth profiles. We develop a bias voltage-compensation method to address this critical problem and obtain quantitatively accurate measurements of the open-circuit voltage, built-in potential and electrode potential difference.
Quantitative operando visualization of the energy band depth profile in solar cells
Chen, Qi; Mao, Lin; Li, Yaowen; Kong, Tao; Wu, Na; Ma, Changqi; Bai, Sai; Jin, Yizheng; Wu, Dan; Lu, Wei; Wang, Bing; Chen, Liwei
2015-01-01
The energy band alignment in solar cell devices is critically important because it largely governs elementary photovoltaic processes, such as the generation, separation, transport, recombination and collection of charge carriers. Despite the expenditure of considerable effort, the measurement of energy band depth profiles across multiple layers has been extremely challenging, especially for operando devices. Here we present direct visualization of the surface potential depth profile over the cross-sections of operando organic photovoltaic devices using scanning Kelvin probe microscopy. The convolution effect due to finite tip size and cantilever beam crosstalk has previously prohibited quantitative interpretation of scanning Kelvin probe microscopy-measured surface potential depth profiles. We develop a bias voltage-compensation method to address this critical problem and obtain quantitatively accurate measurements of the open-circuit voltage, built-in potential and electrode potential difference. PMID:26166580
Chen, Zhiqiang; Huang, Chao; Chennamsetty, Naresh; Xu, Xuankuo; Li, Zheng Jian
2016-08-19
Cation-exchange chromatography (CEX) of a structurally unstable Fc-fusion protein exhibited multi-peak elution profile upon a salt-step elution due to protein aggregation during intra-column buffer transition where low pH and high salt coexisted. The protein exhibited a single-peak elution behavior during a pH-step elution; nevertheless, the levels of soluble aggregates (i.e. high molecular weight species, HMW) in the CEX eluate were still found up to 12-fold higher than that for the load material. The amount of the aggregates formed upon the pH-step elution was dependent on column loading with maximum HMW achieved at intermediate loading levels, supporting the hypothesis that the aggregation was the result of both the conformational changes of the bound protein and the solution concentration of the aggregation-susceptible proteins during elution. Factors such as high load pH, short protein/resin contact time, hydrophilic resin surface, and weak ionizable ligand were effective, to some extent, to reduce aggregate formation by improving the structural integrity of the bound protein. An orthogonal technique, differential scanning fluorimetry (DSF) using Sypro Orange dye confirmed that the bound protein exposed more hydrophobic area than the native molecule in free solution, especially in the pH 4-5 range. The Sypro Orange dye study of resin surface property also demonstrated that the poly[styrene-divinylbenzene]-based Poros XS with polyhydroxyl surface coating is more hydrophobic compared to the agarose-based CM Sepharose FF and SP Sepharose FF. The hydrophobic property of Poros XS contributed to stronger interactions with the partially unfolded bound protein and consequently to the higher aggregate levels seen in Poros XS eluate. This work also investigates the aggregation reversibility in CEX eluate where up to 66% of the aggregates were observed to dissociate into native monomers over a period of 120h, and links the aggregate stability to such conditions as resin surface properties and charged ligand type. Experimental data was correlated semi-quantitatively with theoretical protein charge and hydrophobicity calculations using homology modeling within the BIOVIA Discovery Studio software. Finally, an arginine-sulphopropyl (Arg-SP) agarose resin immobilized with multi-functional ligands was prepared to verify the proposed hypothesis and to eliminate the aggregate formation. The findings of this work provide general insights in understanding aggregate formation and dissociation for structurally unstable proteins in the CEX step. Copyright © 2016 Elsevier B.V. All rights reserved.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Schmidt, Derek William; Cardenas, Tana; Doss, Forrest W.
In this paper, the High Energy Density Physics program at Los Alamos National Laboratory (LANL) has had a multiyear campaign to verify the predictive capability of the interface evolution of shock propagation through different profiles machined into the face of a plastic package with an iodine-doped plastic center region. These experiments varied the machined surface from a simple sine wave to a double sine wave and finally to a multitude of different profiles with power spectrum ranges and shapes to verify LANL’s simulation capability. The MultiMode-A profiles had a band-pass flat region of the power spectrum, while the MultiMode-B profilemore » had two band-pass flat regions. Another profile of interest was the 1-Peak profile, a band-pass concept with a spike to one side of the power spectrum. All these profiles were machined in flat and tilted orientations of 30 and 60 deg. Tailor-made machining profiles, supplied by experimental physicists, were compared to actual machined surfaces, and Fourier power spectra were compared to see the reproducibility of the machining process over the frequency ranges that physicists require.« less
Schmidt, Derek William; Cardenas, Tana; Doss, Forrest W.; ...
2018-01-15
In this paper, the High Energy Density Physics program at Los Alamos National Laboratory (LANL) has had a multiyear campaign to verify the predictive capability of the interface evolution of shock propagation through different profiles machined into the face of a plastic package with an iodine-doped plastic center region. These experiments varied the machined surface from a simple sine wave to a double sine wave and finally to a multitude of different profiles with power spectrum ranges and shapes to verify LANL’s simulation capability. The MultiMode-A profiles had a band-pass flat region of the power spectrum, while the MultiMode-B profilemore » had two band-pass flat regions. Another profile of interest was the 1-Peak profile, a band-pass concept with a spike to one side of the power spectrum. All these profiles were machined in flat and tilted orientations of 30 and 60 deg. Tailor-made machining profiles, supplied by experimental physicists, were compared to actual machined surfaces, and Fourier power spectra were compared to see the reproducibility of the machining process over the frequency ranges that physicists require.« less
Characterizing bars in low surface brightness disc galaxies
NASA Astrophysics Data System (ADS)
Peters, Wesley; Kuzio de Naray, Rachel
2018-05-01
In this paper, we use B-band, I-band, and 3.6 μm azimuthal light profiles of four low surface brightness galaxies (LSBs; UGC 628, F568-1, F568-3, F563-V2) to characterize three bar parameters: length, strength, and corotation radius. We employ three techniques to measure the radius of the bars, including a new method using the azimuthal light profiles. We find comparable bar radii between the I-band and 3.6 μm for all four galaxies when using our azimuthal light profile method, and that our bar lengths are comparable to those in high surface brightness galaxies (HSBs). In addition, we find the bar strengths for our galaxies to be smaller than those for HSBs. Finally, we use Fourier transforms of the B-band, I-band, and 3.6 μm images to characterize the bars as either `fast' or `slow' by measuring the corotation radius via phase profiles. When using the B- and I-band phase crossings, we find three of our galaxies have faster than expected relative bar pattern speeds for galaxies expected to be embedded in centrally dense cold dark matter haloes. When using the B-band and 3.6 μm phase crossings, we find more ambiguous results, although the relative bar pattern speeds are still faster than expected. Since we find a very slow bar in F563-V2, we are confident that we are able to differentiate between fast and slow bars. Finally, we find no relation between bar strength and relative bar pattern speed when comparing our LSBs to HSBs.
POST-OUTBURST RADIO OBSERVATIONS OF THE HIGH MAGNETIC FIELD PULSAR PSR J1119-6127
DOE Office of Scientific and Technical Information (OSTI.GOV)
Majid, Walid A.; Pearlman, Aaron B.; Dobreva, Tatyana
We have carried out high-frequency radio observations of the high magnetic field pulsar PSR J1119-6127 following its recent X-ray outburst. While initial observations showed no evidence of significant radio emission, subsequent observations detected pulsed emission across a large frequency band. In this Letter, we report on the initial disappearance of the pulsed emission and its prompt reactivation and dramatic evolution over several months of observation. The periodic pulse profile at S -band (2.3 GHz) after reactivation exhibits a multi-component emission structure, while the simultaneous X -band (8.4 GHz) profile shows a single emission peak. Single pulses were also detected atmore » S -band near the main emission peaks. We present measurements of the spectral index across a wide frequency bandwidth, which captures the underlying changes in the radio emission profile of the neutron star. The high-frequency radio detection, unusual emission profile, and observed variability suggest similarities with magnetars, which may independently link the high-energy outbursts to magnetar-like behavior.« less
NASA Astrophysics Data System (ADS)
Ishikawa, Haruki; Nakano, Takumi; Takashima, Tsukiko; Yabuguchi, Hiroki; Fuke, Kiyokazu
2013-06-01
In order to investigate the deuteration effect on the vibrational dynamics of the NH and/or ND stretch excited levels of the 7-azaindole (7-AI) normal dimer and its tautomeric dimer, we have carried out infrared spectroscopy of three isotopic species for each dimers; undeuterated one (NH-NH) and one or two hydrogen atom(s) of the NH groups is deuterated ones (NH-ND and ND-ND, respectively). It is found that the ND stretch band profiles of the NH-ND and ND-ND tautomeric dimers are very similar with each other. This result is very distinct from the result of the comparison of the NH stretch band profiles of the NH-NH and NH-ND dimers in our previous study. For a further discussion, we have examined the deuteration effect in the case of the 7-AI normal dimer. It is found that the NH stretch band profiles of the NH-NH and the NH-ND dimers and also the ND stretch band profiles of the NH-ND and the ND-ND dimers exhibit similar patterns, respectively. These facts indicates that the vibrational relaxation from the NH/ND stretch level of the normal dimer basically proceed within a monomer unit. The large deuteration effect of the NH stretch band profile observed previously is found to be characteristic of the tautomeric dimer. This behavior is related to a large anharmonicity of the potential energy surface originating from an existence of the double-proton transfer reaction barrier. H. Ishikawa, H. Yabuguchi, Y. Yamada, A. Fujihara, K. Fuke, J. Phys. Chem. A 114, 3199 (2010).
NASA Astrophysics Data System (ADS)
Yokoyama, S.; Shimomura, T.; Hisyamudin, M. N. N.; Takahashi, T.; Izaki, M.
2012-03-01
Fundamental study was carried out for provision for acidification of soil due to acid rain. The influence of weight of the additive slag on elution behavior of the slag into water was studied in this study. Elution experiment was carried out on a basis of JIS K 0058-1. Generally, the pH in the aqueous solution increased with an increase in weight of the additive slag. The pH converged to approximately eight. Calcium, magnesium and manganese, which were essential elements for plants, were eluted from the slag irrespective to elution condition. The eluted concentrations of Ca and Mg increased with an increase in weight of the additive slag. Silicon and zinc were also eluted depending on the conditions. Aluminum that was harmful for plants was not eluted from the used slag.
Manganese toxicity to chlorophyll synthesis in tobacco callus. [Nicotiana tabacum
DOE Office of Scientific and Technical Information (OSTI.GOV)
Clairmont, K.B.; Hagar, W.G.; Davis, E.A.
1986-01-01
Tobacco (Nicotiana tabacum) pith explants were grown on manganese containing medium. At moderate concentration (10 millimolar), manganese selectivity inhibited chlorophyll synthesis, resulting initially in growth of white callus. Several weeks later the white callus turned brown due to the accumulation of a pigment identified as protoporphyrin IX by its elution profile using high performance liquid chromatography, by its absorption spectrum, and by its fluorescence properties. At a concentration of 100 millimolar manganese the pigment accumulated without growth of the explant.
Multicomponent Calibration and Quantitation Methods.
1984-11-01
liquid chromatographic peaks (45). Applying rank annihilation to LC /UV data requires that the elution profiles of each individual component in the...measurements, e.g. LC /UV, CC/MS, or GC/FTIR analyses. The response of a single component can be described as M = a x y’ (45) 0 where M contains the...in the second dimension. For example, a GC/MS peak consisting - 3 of 50 mass spectra each composed of 20 distinct m/e ratios would result in a matrix
The profile of the bending mode band in solid CO2
NASA Astrophysics Data System (ADS)
Baratta, G. A.; Palumbo, M. E.
2017-12-01
Context. Solid carbon dioxide (CO2) is one of the most abundant species detected in icy grain mantles in dense molecular clouds. Its identification is based on the comparison between astronomical and laboratory spectra. In the past 30 yr the profile of solid CO2 infrared absorption bands has been extensively studied experimentally, however, the debate on the structure (amorphous versus crystalline) of CO2 samples obtained in laboratory by the thin-film technique is still open. Aims: The aim of this work is to investigate if the presence of the double peak feature in the profile of the CO2 bending mode band is related to the crystalline or amorphous structure of the sample. Methods: We performed new laboratory experiments depositing CO2 under ultra high vacuum (UHV) conditions at 17 K. We investigated, using infrared transmission spectroscopy, the influence of various experimental parameters on the profile of the CO2 bands, namely deposition rate, sample thickness, annealing, and presence of H2O, CH3OH or CO co-deposited with CO2. Results: We found that, within experimental uncertainties, under UHV conditions the profile of the CO2 bands in pure solid samples does not depend on the deposition rate or the sample thickness in the ranges investigated. In all cases the bending mode band profile shows a double peak (at 660 and 655 cm-1). The spectra also show the Fermi resonance features that cannot be active in crystalline samples. On the other hand, when a small fraction of H2O or CH3OH is co-deposited with CO2 the double peak is not observed while it is observed when a CO2:CO mixture is considered. Furthermore, we measured the density of solid CO2 and the refractive index (at 543.5 nm) at 17 K and at 70 K: ρ(17 K)= 1.17 g cm-3, ρ(70K)= 1.49 g cm-3, n(17K)= 1.285, and n(70K)= 1.372. Conclusions: Our experimental results indicate that the presence of the double peak in the profile of the bending mode band is not an indication of a crystalline structure of the sample and they do not exclude the presence of amorphous solid CO2 in space.
Shear-banding and superdiffusivity in entangled polymer solutions
NASA Astrophysics Data System (ADS)
Shin, Seunghwan; Dorfman, Kevin D.; Cheng, Xiang
2017-12-01
Using high-resolution confocal rheometry, we study the shear profiles of well-entangled DNA solutions under large-amplitude oscillatory shear in a rectilinear planar shear cell. With increasing Weissenberg number (Wi), we observe successive transitions from normal Newtonian linear shear profiles to wall-slip dominant shear profiles and, finally, to shear-banding profiles at high Wi. To investigate the microscopic origin of the observed shear banding, we study the dynamics of micron-sized tracers embedded in DNA solutions. Surprisingly, tracer particles in the shear frame exhibit transient superdiffusivity and strong dynamic heterogeneity. The probability distribution functions of particle displacements follow a power-law scaling at large displacements, indicating a Lévy-walk-type motion, reminiscent of tracer dynamics in entangled wormlike micelle solutions and sheared colloidal glasses. We further characterize the length and time scales associated with the abnormal dynamics of tracer particles. We hypothesize that the unusual particle dynamics arise from localized shear-induced chain disentanglement.
Profiling Polyphenols in Five Brassica species Microgreens by UHPLC-PDA-ESI/HRMSn
Sun, Jianghao; Xiao, Zhenlei; Lin, Long-ze; Lester, Gene E.; Wang, Qin; Harnly, James M.; Chen, Pei
2014-01-01
Brassica vegetables are known to contain relatively high concentrations of bioactive compounds associated with human health. A comprehensive profiling of polyphenols from five Brassica species microgreens was conducted using ultra high-performance liquid chromatography photo diode array high-resolution multi-stage mass spectrometry (UHPLC-PDA-ESI/HRMSn). A total of 164 polyphenols including 30 anthocyanins, 105 flavonol glycosides, and 29 hydroxycinnamic acid and hydroxybenzoic acid derivatives were putatively identified.The putative identifications were based on UHPLC-HRMSn analysis using retention times, elution orders, UV/Vis spectra and high resolution mass spectra, in-house polyphenol database, and as well as literature comparisons. This study showed that these five Brassica species microgreens could be considered as good sources of food polyphenols. PMID:24144328
Kandzari, David E; Mauri, Laura; Koolen, Jacques J; Massaro, Joseph M; Doros, Gheorghe; Garcia-Garcia, Hector M; Bennett, Johan; Roguin, Ariel; Gharib, Elie G; Cutlip, Donald E; Waksman, Ron
2017-10-21
The development of coronary drug-eluting stents has included use of new metal alloys, changes in stent architecture, and use of bioresorbable polymers. Whether these advancements improve clinical safety and efficacy has not been shown in previous randomised trials. We aimed to examine the clinical outcomes of a bioresorbable polymer sirolimus-eluting stent compared with a durable polymer everolimus-eluting stent in a broad patient population undergoing percutaneous coronary intervention. BIOFLOW V was an international, randomised trial done in patients undergoing elective and urgent percutaneous coronary intervention in 90 hospitals in 13 countries (Australia, Belgium, Canada, Denmark, Germany, Hungary, Israel, the Netherlands, New Zealand, South Korea, Spain, Switzerland, and the USA). Eligible patients were those aged 18 years or older with ischaemic heart disease undergoing planned stent implantation in de-novo, native coronary lesions. Patients were randomly assigned (2:1) to either an ultrathin strut (60 μm) bioresorbable polymer sirolimus-eluting stent or to a durable polymer everolimus-eluting stent. Randomisation was via a central web-based data capture system (mixed blocks of 3 and 6), and stratified by study site. The primary endpoint was 12-month target lesion failure. The primary non-inferiority comparison combined these data from two additional randomised trials of bioresorbable polymer sirolimus-eluting stent and durable polymer everolimus-eluting stent with Bayesian methods. Analysis was by intention to treat. The trial is registered with ClinicalTrials.gov, number NCT02389946. Between May 8, 2015, and March 31, 2016, 4772 patients were recruited into the study. 1334 patients met inclusion criteria and were randomly assigned to treatment with bioresorbable polymer sirolimus-eluting stents (n=884) or durable polymer everolimus-eluting stents (n=450). 52 (6%) of 883 patients in the bioresorbable polymer sirolimus-eluting stent group and 41 (10%) of 427 patients in the durable polymer everolimus-eluting stent group met the 12-month primary endpoint of target lesion failure (95% CI -6·84 to -0·29, p=0·0399), with differences in target vessel myocardial infarction (39 [5%] of 831 patients vs 35 [8%] of 424 patients, p=0·0155). The posterior probability that the bioresorbable polymer sirolimus-eluting stent is non-inferior to the durable polymer everolimus-eluting stent was 100% (Bayesian analysis, difference in target lesion failure frequency -2·6% [95% credible interval -5·5 to 0·1], non-inferiority margin 3·85%, n=2208). The outperformance of the ultrathin, bioresorbable polymer sirolimus-eluting stent over the durable polymer everolimus-eluting stent in a complex patient population undergoing percutaneous coronary intervention suggests a new direction in improving next generation drug-eluting stent technology. BIOTRONIK. Copyright © 2017 Elsevier Ltd. All rights reserved.
NASA Technical Reports Server (NTRS)
Varanasi, P.; Cess, R. D.; Bangaru, B. R. P.
1974-01-01
Measurements of the absolute intensity and integrated band absorption have been performed for the nu sub 9 fundamental band of ethane. The intensity is found to be about 34 per sq cm per atm at STP, and this is significantly higher than previous estimates. It is shown that a Gaussian profile provides an empirical representation of the apparent spectral absorption coefficient. Employing this empirical profile, a simple expression is derived for the integrated band absorption, which is in excellent agreement with experimental values. The band model is then employed to investigate the possible role of ethane as a source of thermal infrared opacity within the atmospheres of Jupiter and Saturn, and to interpret qualitatively observed brightness temperatures for Saturn.
Legutko, Jacek; Zasada, Wojciech; Kałuża, Grzegorz L.; Heba, Grzegorz; Rzeszutko, Lukasz; Jakala, Jacek; Dragan, Jacek; Klecha, Artur; Giszterowicz, Dawid; Dobrowolski, Wojciech; Partyka, Łukasz; Jayaraman, Swaminathan; Dudek, Dariusz
2013-01-01
Aims Evaluation of safety and efficacy of ProNOVA XR, a new generation of polymer-free sirolimus eluting stents (SES), utilizing a pharmaceutical excipient for timed release of sirolimus from the XR platform. Methods and results Safety and efficacy of ProNOVA XR coronary stent system was examined in EURONOVA prospective, single arm, multi-center registry of 50 patients with de novo native coronary lesions up to 28 mm in length in arteries between 2.25 and 4 mm. At 6-month, in-stent late lumen loss by QCA was 0.45 ± 0.41 mm and in-stent neointimal volume obstruction in the IVUS sub-study was 14 ± 11%. One-year clinical follow-up revealed a favorable safety profile, with 2% of in-hospital MACE and 6.4% of MACE from hospital discharge up to 12 months (including 1 cardiac death >30 days after stent implantation and 2 TLRs). According to the ARC definition, there was no definite or probable stent thrombosis and 1 possible stent thrombosis (2%) up to 12 months of clinical follow-up. Conclusions In this preliminary evaluation, ProNOVA XR polymer-free sirolimus eluting stent system appeared safe with an early promise of adequate effectiveness in the treatment of de novo coronary lesions in up to 12 months of clinical, angiographic and IVUS follow-up. PMID:23992999
Amor-Coarasa, Alejandro; Kelly, James M; Gruca, Monika; Nikolopoulou, Anastasia; Vallabhajosula, Shankar; Babich, John W
2017-10-01
Performance of a second itG 68 Ge/ 68 Ga generator system and production of 68 Ga-DOTATOC and 68 Ga-PSMA-HBED-CC were tested over one year as an accompaniment to a previously published study (J Nucl Med. 2016;57:1402-1405). Performance of a 1951MBq 68 Ge/ 68 Ga generator was characterized and the eluate used for preparation of 68 Ga-DOTATOC and 68 Ga-PSMA-HBED-CC. Weekly elution profiles of 68 Ga elution yield and 68 Ge breakthrough were determined. 68 Ga elution yields averaged 82% (61.8-98.4%) and 68 Ge breakthrough averaged 0.002% (0.0007% to 0.004%). The radiochemical purities of 68 Ga-DOTATOC and 68 Ga-PSMA-HBED-CC were determined by HPLC analysis to be >98% and specific activity was 12.6 and 42GBq/μmol, respectively. 68 Ge contamination in the product was under the detection limit (0.00001%). Final sterile, pyrogen-free formulation of 68 Ga-DOTATOC and 68 Ga-PSMA-HBED-CC in physiologic saline with 5%-7% ethanol was achieved. Performance of a 68 Ge/ 68 Ga generator was studied over one year with satisfactory results. The generator eluate was used to synthesize 68 Ga-DOTATOC and 68 Ga-PSMA-HBED-CC on a routine basis in high purity. Copyright © 2017. Published by Elsevier Inc.
Holzmann, Johann; Fuchs, Johannes; Pichler, Peter; Peters, Jan-Michael; Mechtler, Karl
2011-02-04
Affinity purification of proteins using antibodies coupled to beads and subsequent mass spectrometric analysis has become a standard technique for the identification of protein complexes. With the recent transfer of the isotope dilution mass spectrometry principle (IDMS) to the field of proteomics, quantitative analyses-such as the stoichiometry determination of protein complexes-have become achievable. Traditionally proteins were eluted from antibody-conjugated beads using glycine at low pH or using diluted acids such as HCl, TFA, or FA, but elution was often found to be incomplete. Using the cohesin complex and the anaphase promoting complex/cyclosome (APC/C) as examples, we show that a short 15-60 min predigestion with a protease such as LysC (modified on-bead digest termed protease elution) increases the elution efficiency 2- to 3-fold compared to standard acid elution protocols. While longer incubation periods-as performed in standard on-bead digestion-led to partial proteolysis of the cross-linked antibodies, no or only insignificant cleavage was observed after 15-60 min protease mediated elution. Using the protease elution method, we successfully determined the stoichiometry of the cohesin complex by absolute quantification of the four core subunits using LC-SRM analysis and 19 reference peptides generated with the EtEP strategy. Protease elution was 3-fold more efficient compared to HCl elution, but measurements using both elution techniques are in agreement with a 1:1:1:1 stoichiometry. Furthermore, using isoform specific reference peptides, we determined the exact STAG1:STAG2 stoichiometry within the population of cohesin complexes. In summary, we show that the protease elution protocol increases the recovery from affinity beads and is compatible with quantitative measurements such as the stoichiometry determination of protein complexes.
NASA Astrophysics Data System (ADS)
Rambe, A. H.; Abdillah, K.
2018-02-01
This paper discussed a low profile rectangular patch microstrip antenna design working on dual-band 1.8 GHz and 2.4 GHz. Dual-band characteristic is achieved by using inset-feed point and slot size adjustment. The designed antenna was printed on a FR4 substrate with relative permittivity of 4.4 and a thickness of 1.6 mm with patch size 40 x 29 mm. The measurement results show that the realized antenna successfully working on dual-band, achieving bandwidth of 45 MHz and 95 MHz, gain of 4.08 dBi and 5.79 dBi for 1.8 GHz and 2.4 GHz subsequently.
Simulation of amide I' band profiles of trans polyproline based on an excitonic coupling model
NASA Astrophysics Data System (ADS)
Measey, Thomas; Schweitzer-Stenner, Reinhard
2005-06-01
We measured the amide I' band profile of the IR, isotropic Raman, anisotropic Raman, and Vibrational Circular Dichroism spectrum of poly- L-proline in D 2O. The band shapes were modeled by using an algorithm that exploits the delocalized character of the excited vibrational states [R. Schweitzer-Stenner, J. Phys. Chem. B. 108 (2004) 16965]. The band shapes could be quantitatively reproduced by invoking the polyproline II or 3 1-helix conformation for all peptide residues. This corroborates the notion that the combined use of the above spectroscopies is an ideal tool to discriminate different conformations associated with the so-called random coil state of peptides.
Drug-eluting versus bare-metal coronary stents: where are we now?
Amoroso, Nicholas S; Bangalore, Sripal
2012-11-01
Drug-eluting stents have dramatically reduced the risk of restenosis, but concerns of an increased risk of stent thrombosis have provided uncertainty about their use. Recent studies have continued to show improved procedural and clinical outcomes with drug-eluting stents both in the setting of acute coronary syndromes and stable coronary artery disease. Newer generation drug-eluting stents (especially everolimus-eluting stents) have been shown to be not only efficacious but also safe with reduced risk of stent thrombosis when compared with bare-metal stents, potentially changing the benchmark for stent safety from bare-metal stents to everolimus-eluting stents. While much progress is being made in the development of bioabsorbable polymer stents, nonpolymer stents and bioabsorbable stent technology, it remains to be seen whether these stents will have superior safety and efficacy outcomes compared with the already much improved rates of revascularization and stent thrombosis seen with newer generation stents (everolimus-eluting stents and resolute zotarolimus-eluting stents).
NASA Astrophysics Data System (ADS)
Lauer, Tobias; Frechen, Manfred; Vlaminck, Stefan; Kehl, Martin; Sharifi, Jafar; Rolf, Christian; Khormali, Farhad
2016-04-01
The northern Iranian loess profiles host important information on quaternary climate and palaeoenvironmental changes in the region. Furthermore, they build an important link to correlate European and Central Asian archives. Due to a significant climatic gradient with decreasing precipitation from the west to the east and from the south to the north, loess-palaeosol sequences which were formed synchronously under different climatic conditions can be studied. The Agh Band profile is located in the so called Iranian "Loess Plateau", a semi-arid region with about 300 mm annual precipitation. The loess deposits reach a thickness of > 60 meters and are subdivided by several weak soil horizons in the more upper part and by a pedo-complex of 3 Bw(y) horizons in the lower part of the loess. The Agh Band profile was sampled in 2 cm intervals for multi-proxy analyses (e.g. magnetic susceptibility and grain size measurements). Furthermore, samples for palaeomangentic studies and luminescence dating were collected and a pIRIR290 approach was applied to fine-grain polyminerals. The results show that the Agh Band profile yields a climate archive reaching from MIS 7 to MIS 2. Several chronological hiatuses of some 10 ka show that periods of intense loess accumulation were interrupted by phases of only minor loess sedimentation and/or erosion. The Agh Band profile hosts an extraordinary good temporal resolution for MIS 4 and MIS 5. The pedocomplex at the bottom part of the profile indicates a period of increased humidity and landscape stability during late MIS 7 and MIS 6 following the luminescence ages. The loess-profile is also subdivided by several shifts in grain-size distribution. The coarsening- and fining up trends correlate with increasing and decreasing wind- velocity, respectively.
Ranjard, Lionel; Brothier, Elisabeth; Nazaret, Sylvie
2000-01-01
Two major emerging bands (a 350-bp band and a 650-bp band) within the RISA (ribosomal intergenic spacer analysis) profile of a soil bacterial community spiked with Hg(II) were selected for further identification of the populations involved in the response of the community to the added metal. The bands were cut out from polyacrylamide gels, cloned, characterized by restriction analysis, and sequenced for phylogenetic affiliation of dominant clones. The sequences were the intergenic spacer between the rrs and rrl genes and the first 130 nucleotides of the rrl gene. Comparison of sequences derived from the 350-bp band to The GenBank database permitted us to identify the bacteria as being mostly close relatives to low G+C firmicutes (Clostridium-like genera), while the 650-bp band permitted us to identify the bacteria as being mostly close relatives to β-proteobacteria (Ralstonia-like genera). Oligonucleotide probes specific for the identified dominant bacteria were designed and hybridized with the RISA profiles derived from the control and spiked communities. These studies confirmed the contribution of these populations to the community response to the metal. Hybridization of the RISA profiles from subcommunities (bacterial pools associated with different soil microenvironments) also permitted to characterize the distribution and the dynamics of these populations at a microscale level following mercury spiking. PMID:11097911
Kang, Si-Hyuck; Park, Kyung Woo; Kang, Do-Yoon; Lim, Woo-Hyun; Park, Kyung Taek; Han, Jung-Kyu; Kang, Hyun-Jae; Koo, Bon-Kwon; Oh, Byung-Hee; Park, Young-Bae; Kandzari, David E; Cohen, David J; Hwang, Seung-Sik; Kim, Hyo-Soo
2014-05-01
The aim of this study was to compare the safety and efficacy of biodegradable-polymer (BP) drug-eluting stents (DES), bare metal stents (BMS), and durable-polymer DES in patients undergoing coronary revascularization, we performed a systematic review and network meta-analysis using a Bayesian framework. Study stents included BMS, paclitaxel-eluting (PES), sirolimus-eluting (SES), endeavor zotarolimus-eluting (ZES-E), cobalt-chromium everolimus-eluting (CoCr-EES), platinium-chromium everolimus-eluting (PtCr-EES), resolute zotarolimus-eluting (ZES-R), and BP biolimus-eluting stents (BP-BES). After a systematic electronic search, 113 trials with 90 584 patients were selected. The principal endpoint was definite or probable stent thrombosis (ST) defined according to the Academic Research Consortium within 1 year. Biodegradable polymer-biolimus-eluting stents [OR, 0.56; 95% credible interval (CrI), 0.33-0.90], SES (OR, 0.53; 95% CrI, 0.38-0.73), CoCr-EES (OR, 0.34; 95% CrI, 0.23-0.52), and PtCr-EES (OR, 0.31; 95% CrI, 0.10-0.90) were all superior to BMS in terms of definite or probable ST within 1 year. Cobalt-chromium everolimus-eluting stents demonstrated the lowest risk of ST of all stents at all times after stent implantation. Biodegradable polymer-biolimus-eluting stents was associated with a higher risk of definite or probable ST than CoCr-EES (OR, 1.72; 95% CrI, 1.04-2.98). All DES reduced the need for repeat revascularization, and all but PES reduced the risk of myocardial infarction compared with BMS. All DESs but PES and ZES-E were superior to BMS in terms of ST within 1 year. Cobalt-chromium everolimus-eluting stents was safer than any DES even including BP-BES. Our results suggest that not only the biodegradability of polymer, but the optimal combination of stent alloy, design, strut thickness, polymer, and drug all combined determine the safety of DES.
Kong, Weiping; Huang, Wenjiang; Casa, Raffaele; Zhou, Xianfeng; Ye, Huichun; Dong, Yingying
2017-11-23
Monitoring the vertical profile of leaf chlorophyll (Chl) content within winter wheat canopies is of significant importance for revealing the real nutritional status of the crop. Information on the vertical profile of Chl content is not accessible to nadir-viewing remote or proximal sensing. Off-nadir or multi-angle sensing would provide effective means to detect leaf Chl content in different vertical layers. However, adequate information on the selection of sensitive spectral bands and spectral index formulas for vertical leaf Chl content estimation is not yet available. In this study, all possible two-band and three-band combinations over spectral bands in normalized difference vegetation index (NDVI)-, simple ratio (SR)- and chlorophyll index (CI)-like types of indices at different viewing angles were calculated and assessed for their capability of estimating leaf Chl for three vertical layers of wheat canopies. The vertical profiles of Chl showed top-down declining trends and the patterns of band combinations sensitive to leaf Chl content varied among different vertical layers. Results indicated that the combinations of green band (520 nm) with NIR bands were efficient in estimating upper leaf Chl content, whereas the red edge (695 nm) paired with NIR bands were dominant in quantifying leaf Chl in the lower layers. Correlations between published spectral indices and all NDVI-, SR- and CI-like types of indices and vertical distribution of Chl content showed that reflectance measured from 50°, 30° and 20° backscattering viewing angles were the most promising to obtain information on leaf Chl in the upper-, middle-, and bottom-layer, respectively. Three types of optimized spectral indices improved the accuracy for vertical leaf Chl content estimation. The optimized three-band CI-like index performed the best in the estimation of vertical distribution of leaf Chl content, with R² of 0.84-0.69, and RMSE of 5.37-5.56 µg/cm² from the top to the bottom layers, while the optimized SR-like index was recommended for the bottom Chl estimation due to its simple and universal form. We suggest that it is necessary to take into account the penetration characteristic of the light inside the canopy for different Chl absorption regions of the spectrum and the formula used to derive spectral index when estimating the vertical profile of leaf Chl content using off-nadir hyperspectral data.
A Small Fullerene (C{sub 24}) may be the Carrier of the 11.2 μ m Unidentified Infrared Band
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bernstein, L. S.; Shroll, R. M.; Lynch, D. K.
2017-02-20
We analyze the spectrum of the 11.2 μ m unidentified infrared band (UIR) from NGC 7027 and identify a small fullerene (C{sub 24}) as a plausible carrier. The blurring effects of lifetime and vibrational anharmonicity broadening obscure the narrower, intrinsic spectral profiles of the UIR band carriers. We use a spectral deconvolution algorithm to remove the blurring, in order to retrieve the intrinsic profile of the UIR band. The shape of the intrinsic profile—a sharp blue peak and an extended red tail—suggests that the UIR band originates from a molecular vibration–rotation band with a blue band head. The fractional areamore » of the band-head feature indicates a spheroidal molecule, implying a nonpolar molecule and precluding rotational emission. Its rotational temperature should be well approximated by that measured for nonpolar molecular hydrogen, ∼825 K for NGC 7027. Using this temperature, and the inferred spherical symmetry, we perform a spectral fit to the intrinsic profile, which results in a rotational constant implying C{sub 24} as the carrier. We show that the spectroscopic parameters derived for NGC 7027 are consistent with the 11.2 μ m UIR bands observed for other objects. We present density functional theory (DFT) calculations for the frequencies and infrared intensities of C{sub 24}. The DFT results are used to predict a spectral energy distribution (SED) originating from absorption of a 5 eV photon, and characterized by an effective vibrational temperature of 930 K. The C{sub 24} SED is consistent with the entire UIR spectrum and is the dominant contributor to the 11.2 and 12.7 μ m bands.« less
Metal elution from Ni- and Fe-based alloy reactors under hydrothermal conditions.
Faisal, Muhammad; Quitain, Armando T; Urano, Shin-Ya; Daimon, Hiroyuki; Fujie, Koichi
2004-05-20
Elution of metals from Ni- and Fe-based alloy (i.e. Inconel 625 and SUS 316) under hydrothermal conditions was investigated. Results showed that metals could be eluted even in a short contact time. At subcritical conditions, a significant amount of Cr was extracted from SUS 316, while only traces of Ni, Fe, Mo, and Mn were eluted. In contrast, Ni was removed in significant amounts compared to Cr when Inconel 625 was tested. Several factors including temperature and contact time were found to affect elution behavior. The presence of air in the fluid even promoted elution under subcritical conditions.
Nakagawa, Mizuki; Sugawara, Kotomi; Goto, Tatsufumi; Wakui, Hideki; Nunomura, Wataru
2016-05-13
Hydroxychloroquine (HCQ) is a widely used drug in the treatment of autoimmune diseases, such as arthritis and systemic lupus erythematosus. It has also been prescribed for the treatment of malaria owing to its lower toxicity compared to its closely related compound chloroquine (CQ). However, the mechanisms of action of HCQ in erythrocytes (which bind preferentially this drug) have not been documented and the reasons underlying the lower side effects of HCQ compared to CQ remain unclear. Here we show that, although the activity of erythrocyte lactate dehydrogenase (LDH), but not GAPDH, was inhibited by both HCQ and CQ in vitro, LDH activity in erythrocytes incubated with 20 mM HCQ was not significantly reduced within 5 h in contrast to CQ did. Using HCQ coupled Sepharose chromatography (HCQ-Sepharose), we identified Band 3, spectrin, ankyrin, protein 4.1R and protein 4.2 as HCQ binding proteins in human erythrocyte plasma membrane. Recombinant cytoplasmic N-terminal 43 kDa domain of Band 3 bound to HCQ-Sepharose and was eluted with 40 mM (but not 20 mM) HCQ. Band 3 transport activity was reduced by only 23% in the presence of 20 mM HCQ. Taken together, these data demonstrate that HCQ binds to the cytoplasmic N-terminal domain of Band 3 in human erythrocytes but does not inhibit dramatically its transport activity. We hypothesize that the trapping of HCQ on Band 3 contributes to the lower side effects of the drug on energy production in erythrocytes. Copyright © 2016 Elsevier Inc. All rights reserved.
Concentration of perrhenate and pertechnetate solutions
Knapp, F.F.; Beets, A.L.; Mirzadeh, S.; Guhlke, S.
1998-03-17
A method is described for preparing a concentrated solution of a carrier-free radioisotope which includes the steps of: (a) providing a generator column loaded with a composition containing a parent radioisotope; (b) eluting the generator column with an eluent solution which includes a salt of a weak acid to elute a target daughter radioisotope from the generator column in a first eluate; (c) eluting a cation-exchange column with the first eluate to exchange cations of the salt for hydrogen ions and to elute the target daughter radioisotope and a weak acid in a second eluate; (d) eluting an anion-exchange column with the second eluate to trap and concentrate the target daughter radioisotope and to elute the weak acid solution therefrom; and (e) eluting the concentrated target daughter radioisotope from the anion-exchange column with a saline solution. 1 fig.
Concentration of perrhenate and pertechnetate solutions
Knapp, Furn F.; Beets, Arnold L.; Mirzadeh, Saed; Guhlke, Stefan
1998-01-01
A method of preparing a concentrated solution of a carrier-free radioisotope which includes the steps of: a. providing a generator column loaded with a composition containing a parent radioisotope; b. eluting the generator column with an eluent solution which includes a salt of a weak acid to elute a target daughter radioisotope from the generator column in a first eluate. c. eluting a cation-exchange column with the first eluate to exchange cations of the salt for hydrogen ions and to elute the target daughter radioisotope and a weak acid in a second eluate; d. eluting an anion-exchange column with the second eluate to trap and concentrate the target daughter radioisotope and to elute the weak acid solution therefrom; and e. eluting the concentrated target daughter radioisotope from the anion-exchange column with a saline solution.
NASA Astrophysics Data System (ADS)
Ma, J.; Zhang, Z.; Wei, G.; Zhang, L.
2017-12-01
A method including a novel column Rb separation procedure and high-precision Rb isotope measurement in geological materials by using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) in standard-sample-bracketing (SSB) mode has been developed. Sr-Spec resin was employed, in which the distribution coefficients for Rb, K, Ba and Sr are different in nitric acid, to sequentially separate them from the matrix. The dissolved samples were loaded on the column in 3 M HNO3, the main matrix such as Al, Ca, Fe, Mg, Mn and Na were removed by rinsing with 4.5 mL HNO3, Rb and K were then sequentially eluted by 3 M HNO3 in different volumes. After that, Ba was eluted by 8 M HNO3, and Sr was finally eluted by Milli-Q water. This enable us to collect the pure Rb, K, Ba and Sr one by one with recovery close to 100% for their isotopic compositions measurement on MC-ICP-MS. We here focus on Rb isotope measurement. The measurement using MC-ICP-MS yielded an internal precision for δ87Rb of < ± 0.03‰ (2SE), and the external precision was generally better than ± 0.06‰ (2SD) based on the long-term results of the Rb standard solutions NIST SRM 984. A series of geological rock standards, were analyzed using this method, and the results indicate significant Rb isotope differences in different geologic materials. This will provide a powerful tool to investigate Rb isotope fractionation during geological processes.Based on this method, Rb isotope compositions from a basaltic weathering profile were carried out. The data show the lighter Rb (85Rb) isotope is preferentially leached from the weathering profile and remains heavy Rb isotope (87Rb) in the weathered residues during the incipient weathering stage. From the moderate to advanced weathering stage, the significant variations of Rb isotope were observed and multiple factors, such as leaching, adsorption, desorption, and precipitation, should play important role in fractionating Rb isotope.
Otte, T; Pasch, H; Macko, T; Brüll, R; Stadler, F J; Kaschta, J; Becker, F; Buback, M
2011-07-08
The molar mass distribution (MMD) of synthetic polymers is frequently analyzed by size exclusion chromatography (SEC) coupled to multi angle light scattering (MALS) detection. For ultrahigh molar mass (UHM) or branched polymers this method is not sufficient, because shear degradation and abnormal elution effects falsify the calculated molar mass distribution and information on branching. High temperatures above 130 °C have to be applied for dissolution and separation of semi-crystalline materials like polyolefins which requires special hardware setups. Asymmetrical flow field-flow fractionation (AF4) offers the possibility to overcome some of the main problems of SEC due to the absence of an obstructing porous stationary phase. The SEC-separation mainly depends on the pore size distribution of the used column set. The analyte molecules can enter the pores of the stationary phase in dependence on their hydrodynamic volume. The archived separation is a result of the retention time of the analyte species inside SEC-column which depends on the accessibility of the pores, the residence time inside the pores and the diffusion ability of the analyte molecules. The elution order in SEC is typically from low to high hydrodynamic volume. On the contrary AF4 separates according to the diffusion coefficient of the analyte molecules as long as the chosen conditions support the normal FFF-separation mechanism. The separation takes place in an empty channel and is caused by a cross-flow field perpendicular to the solvent flow. The analyte molecules will arrange in different channel heights depending on the diffusion coefficients. The parabolic-shaped flow profile inside the channel leads to different elution velocities. The species with low hydrodynamic volume will elute first while the species with high hydrodynamic volume elute later. The AF4 can be performed at ambient or high temperature (AT-/HT-AF4). We have analyzed one low molar mass polyethylene sample and a number of narrow distributed polystyrene standards as reference materials with known structure by AT/HT-SEC and AT/HT-AF4. Low density polyethylenes as well as polypropylene and polybutadiene, containing high degrees of branching and high molar masses, have been analyzed with both methods. As in SEC the relationship between the radius of gyration (R(g)) or the molar mass and the elution volume is curved up towards high elution volumes, a correct calculation of the MMD and the molar mass average or branching ratio is not possible using the data from the SEC measurements. In contrast to SEC, AF4 allows the precise determination of the MMD, the molar mass averages as well as the degree of branching because the molar mass vs. elution volume curve and the conformation plot is not falsified in this technique. In addition, higher molar masses can be detected using HT-AF4 due to the absence of significant shear degradation in the channel. As a result the average molar masses obtained from AF4 are higher compared to SEC. The analysis time in AF4 is comparable to that of SEC but the adjustable cross-flow program allows the user to influence the separation efficiency which is not possible in SEC without a costly change of the whole column combination. Copyright © 2011 Elsevier B.V. All rights reserved.
EVALUATION OF FACTORS IN THE ELUTION OF HYDROCORTISONE FROM PAPER CHROMATOGRAMS
DOE Office of Scientific and Technical Information (OSTI.GOV)
Ganis, F.M.; Hendrickson, M.W.; Giunta, P.D.
An assessment was made of a number of variable factors which affect the recovery of hydrocortisone from eluted filter paper chromatographic fractions. Factors tested included time of elution, sample concentration, rinsing of eluting fractions and pre-washing of the filter paper. It was noted that a 50 mu g sample could be quantitatively recovered after a 15-minute elution time from a pre-washed filter paper fraction. The results were subjected to a statistical analysis and were found to be highly significant. (auth)
Everolimus-eluting stents in interventional cardiology
Townsend, Jacob C; Rideout, Phillip; Steinberg, Daniel H
2012-01-01
Bare metal stents have a proven safety record, but limited long-term efficacy due to in-stent restenosis. First-generation drug-eluting stents successfully countered the restenosis rate, but were hampered by concerns about their long-term safety. Second generation drug-eluting stents have combined the low restenosis rate of the first generation with improved long-term safety. We review the evolution of drug-eluting stents with a focus on the safety, efficacy, and unique characteristics of everolimus-eluting stents. PMID:22910420
Xiao, Yuewu; Stone, Thomas; Moya, Wilson; Killian, Paul; Herget, Thomas
2014-01-21
Confocal Raman spectroscopy is a nondestructive analytical technique that combines the chemical information from vibrational spectroscopy with the spatial resolution of confocal microscopy. It was applied, for the first time, to measure protein desorption from chromatographic particles. Monoclonal antibody was loaded onto the Fractogel EMD SO3 (M) cation exchanger at either pH 5 or pH 4. Confocal Raman measurement suggests that only the protein loaded at pH 5 is able to release from chromatographic particles in the elution buffer. Detailed comparison of high-quality spectra indicates that, while proteins loaded at both pH values showed a predominant β-sheet conformation, protein loaded at pH 4 has a broader amide I band with more intensity in the >1680 cm(-1) region. This small but clear and reproducible amide I bandwidth increase is not observed for protein in the solution state at pH 4. No definitive assignment of the increased Raman intensity in the >1680 cm(-1) region could be made, but it might be related to structural changes involved in the association of protein molecules in the adsorbed state, which helps to explain the nearly 100% retention under elution conditions of the monoclonal antibody adsorbed at pH 4 in chromatographic particles.
Heparin-binding growth factor isolated from human prostatic extracts.
Mydlo, J H; Bulbul, M A; Richon, V M; Heston, W D; Fair, W R
1988-01-01
Prostatic tissue extracts from patients with benign prostatic hyperplasia (BPH) and prostatic carcinoma were fractionated using heparin-Sepharose chromatography. The mitogenic activity of eluted fractions on quiescent subconfluent Swiss Albino 3T3 fibroblasts was tested employing a tritiated-thymidine-incorporation assay. Two peaks of activity were consistently noted--one in the void volume and a second fraction which eluted with 1.3-1.6 M NaCl and contained the majority of the mitogenic activity. Both non-heparin- and heparin-binding fractions increased tritiated incorporation into a mouse osteoblast cell line (MC3T3), while only the heparin-binding fractions stimulated a human umbilical vein endothelial cell line (HUV). No increased uptake of thymidine was seen using a human prostatic carcinoma cell line (PC-3). Sodium dodecyl sulfate/polyacrylamide gel electrophoresis (SDS/PAGE) of lyophilized active fractions showed a persistent band at 17,500 daltons. The purified protein demonstrated angiogenic properties using the chick embryo chorioallantoic membrane (CAM) assay. Western blot analysis using antibodies specific to basic fibroblast growth factor (bFGF) or acidic FGF (aFGF) demonstrated that the former, but not the latter, bound to prostatic growth factor (PrGF), and inhibited its mitogenic activity as well. It appears that PrGF shares homology with basic fibroblast growth factors.
CN-GELFrEE - Clear Native Gel-eluted Liquid Fraction Entrapment Electrophoresis
Skinner, Owen S.; Do Vale, Luis H. F.; Catherman, Adam D.; Havugimana, Pierre C.; Valle de Sousa, Marcelo; Domont, Gilberto B.; Kelleher, Neil L.; Compton, Philip D.
2016-01-01
Protein complexes perform an array of crucial cellular functions. Elucidating their non-covalent interactions and dynamics is paramount for understanding the role of complexes in biological systems. While the direct characterization of biomolecular assemblies has become increasingly important in recent years, native fractionation techniques that are compatible with downstream analysis techniques, including mass spectrometry, are necessary to further expand these studies. Nevertheless, the field lacks a high-throughput, wide-range, high-recovery separation method for native protein assemblies. Here, we present clear native gel-eluted liquid fraction entrapment electrophoresis (CN-GELFrEE), which is a novel separation modality for non-covalent protein assemblies. CN-GELFrEE separation performance was demonstrated by fractionating complexes extracted from mouse heart. Fractions were collected over 2 hr and displayed discrete bands ranging from ~30 to 500 kDa. A consistent pattern of increasing molecular weight bandwidths was observed, each ranging ~100 kDa. Further, subsequent reanalysis of native fractions via SDS-PAGE showed molecular-weight shifts consistent with the denaturation of protein complexes. Therefore, CN-GELFrEE was proved to offer the ability to perform high-resolution and high-recovery native separations on protein complexes from a large molecular weight range, providing fractions that are compatible with downstream protein analyses. PMID:26967310
Klein, R; Adler, A; Beanlands, R S; deKemp, R A
2004-01-01
A rubidium-82 (/sup 82/Rb) elution system is described for use with clinical positron emission tomography. The system is self-calibrating with 1.4% repeatability, independent of generator activity and elution flow rate. Saline flow is switched between a /sup 82/Sr//sup 82/Rb generator and a bypass line to achieve a constant activity elution of /sup 82/Rb. In the present study, pulse width modulation (PWM) of a solenoid valve is compared to simple threshold control as a means to simulate a proportional valve. A predictive-corrective control algorithm is developed which produces a constant activity elution within the constraints of long feedback delay and short elution time. Accurate constant-activity elutions of 10-70% of the total generator activity were demonstrated using the threshold comparison control. The adaptive-corrective control of the PWM valve provided a substantial improvement in precision of the steady-state output.
Method for enhanced accuracy in predicting peptides using liquid separations or chromatography
Kangas, Lars J.; Auberry, Kenneth J.; Anderson, Gordon A.; Smith, Richard D.
2006-11-14
A method for predicting the elution time of a peptide in chromatographic and electrophoretic separations by first providing a data set of known elution times of known peptides, then creating a plurality of vectors, each vector having a plurality of dimensions, and each dimension representing the elution time of amino acids present in each of these known peptides from the data set. The elution time of any protein is then be predicted by first creating a vector by assigning dimensional values for the elution time of amino acids of at least one hypothetical peptide and then calculating a predicted elution time for the vector by performing a multivariate regression of the dimensional values of the hypothetical peptide using the dimensional values of the known peptides. Preferably, the multivariate regression is accomplished by the use of an artificial neural network and the elution times are first normalized using a transfer function.
Chai, Tingting; Yang, Wenwen; Qiu, Jing; Hou, Shicong
2015-01-01
The enantiomeric separation of eight pesticides including bitertanol (), diclobutrazol (), fenbuconazole (), triticonazole (), imazalil (), triapenthenol (), ancymidol (), and carfentrazone-ethyl () was achieved, using normal-phase high-performance liquid chromatography on two cellulosed-based chiral columns. The effects of isopropanol composition from 2% to 30% in the mobile phase and column temperature from 5 to 40 °C were investigated. Satisfactory resolutions were obtained for bitertanol (), triticonazole (), imazalil () with the (+)-enantiomer eluted first and fenbuconazole () with the (-)-enantiomer eluted first on Lux Cellulose-2 and Lux Cellulose-3. (+)-Enantiomers of diclobutrazol () and triapenthenol () were first eluted on Lux Cellulose-2. (-)-Carfentrazone-ethyl () were eluted first on Lux Cellulose-2 and Lux Cellulose-3 with incomplete separation. Reversed elution orders were obtained for ancymidol (7). (+)-Ancymidol was first eluted on Lux Cellulose-2 while on Lux Cellulose-3 (-)-ancymidol was first eluted. The results of the elution order at different column temperatures suggested that column temperature did not affect the optical signals of the enantiomers. These results will be helpful to prepare and analyze individual enantiomers of chiral pesticides. © 2014 Wiley Periodicals, Inc.
Balss, K M; Llanos, G; Papandreou, G; Maryanoff, C A
2008-04-01
Raman spectroscopy was used to differentiate each component found in the CYPHER Sirolimus-eluting Coronary Stent. The unique spectral features identified for each component were then used to develop three separate calibration curves to describe the solid phase distribution found on drug-polymer coated stents. The calibration curves were obtained by analyzing confocal Raman spectral depth profiles from a set of 16 unique formulations of drug-polymer coatings sprayed onto stents and planar substrates. The sirolimus model was linear from 0 to 100 wt % of drug. The individual polymer calibration curves for poly(ethylene-co-vinyl acetate) [PEVA] and poly(n-butyl methacrylate) [PBMA] were also linear from 0 to 100 wt %. The calibration curves were tested on three independent drug-polymer coated stents. The sirolimus calibration predicted the drug content within 1 wt % of the laboratory assay value. The polymer calibrations predicted the content within 7 wt % of the formulation solution content. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectra from five formulations confirmed a linear response to changes in sirolimus and polymer content. Copyright 2007 Wiley Periodicals, Inc.
Characterization of a heparin-binding growth factor from adenocarcinoma of the kidney.
Mydlo, J H; Heston, W D; Fair, W R
1988-12-01
A polypeptide isolated from tissue extracts of renal adenocarcinoma was mitogenic for BALB/c 3T3 cells and human umbilical vein (HUV) cells in culture. It also demonstrated angiogenic ability using the chorioallantoic membrane bioassay. Using heparin-sepharose affinity chromatography the purified protein eluted with a NaCl concentration between 1.4 and 1.8 M and demonstrated a molecular weight of approximately 17,000 daltons based on SDS polyacrylamide gel electrophoresis. Half maximal stimulation of tritiated thymidine incorporation into BALB/c 3T3 cells was achieved by 1.6 ng./ml. of the heparin binding material. Western blot analysis using antibodies specific to basic fibroblast growth factor (bFGF) only or acidic FGF (aFGF) only demonstrated that the purified protein binds to the former and not the latter. The characteristics of this material, in effect the elution profile off heparin-Sepharose, the molecular weight, angiogenic activity and the results of western blot analysis, suggest that this growth factor is similar to the family of basic fibroblast growth factors.
Bai, Yingchen; Wu, Fengchang; Xing, Baoshan; Meng, Wei; Shi, Guolan; Ma, Yan; Giesy, John P
2015-03-04
XAD-8 adsorption technique coupled with stepwise elution using pyrophosphate buffers with initial pH values of 3, 5, 7, 9, and 13 was developed to isolate Chinese standard fulvic acid (FA) and then separated the FA into five sub-fractions: FApH3, FApH5, FApH7, FApH9 and FApH13, respectively. Mass percentages of FApH3-FApH13 decreased from 42% to 2.5%, and the recovery ratios ranged from 99.0% to 99.5%. Earlier eluting sub-fractions contained greater proportions of carboxylic groups with greater polarity and molecular mass, and later eluting sub-fractions had greater phenolic and aliphatic content. Protein-like components, as well as amorphous and crystalline poly(methylene)-containing components were enriched using neutral and basic buffers. Three main mechanisms likely affect stepwise elution of humic components from XAD-8 resin with pyrophosphate buffers including: 1) the carboxylic-rich sub-fractions are deprotonated at lower pH values and eluted earlier, while phenolic-rich sub-fractions are deprotonated at greater pH values and eluted later. 2) protein or protein-like components can be desorbed and eluted by use of stepwise elution as progressively greater pH values exceed their isoelectric points. 3) size exclusion affects elution of FA sub-fractions. Successful isolation of FA sub-fractions will benefit exploration of the origin, structure, evolution and the investigation of interactions with environmental contaminants.
Bai, Yingchen; Wu, Fengchang; Xing, Baoshan; Meng, Wei; Shi, Guolan; Ma, Yan; Giesy, John P.
2015-01-01
XAD-8 adsorption technique coupled with stepwise elution using pyrophosphate buffers with initial pH values of 3, 5, 7, 9, and 13 was developed to isolate Chinese standard fulvic acid (FA) and then separated the FA into five sub-fractions: FApH3, FApH5, FApH7, FApH9 and FApH13, respectively. Mass percentages of FApH3-FApH13 decreased from 42% to 2.5%, and the recovery ratios ranged from 99.0% to 99.5%. Earlier eluting sub-fractions contained greater proportions of carboxylic groups with greater polarity and molecular mass, and later eluting sub-fractions had greater phenolic and aliphatic content. Protein-like components, as well as amorphous and crystalline poly(methylene)-containing components were enriched using neutral and basic buffers. Three main mechanisms likely affect stepwise elution of humic components from XAD-8 resin with pyrophosphate buffers including: 1) the carboxylic-rich sub-fractions are deprotonated at lower pH values and eluted earlier, while phenolic-rich sub-fractions are deprotonated at greater pH values and eluted later. 2) protein or protein-like components can be desorbed and eluted by use of stepwise elution as progressively greater pH values exceed their isoelectric points. 3) size exclusion affects elution of FA sub-fractions. Successful isolation of FA sub-fractions will benefit exploration of the origin, structure, evolution and the investigation of interactions with environmental contaminants. PMID:25735451
Optically-initiated silicon carbide high voltage switch with contoured-profile electrode interfaces
DOE Office of Scientific and Technical Information (OSTI.GOV)
Sullivan, James S.; Hawkins, Steven A.
An improved photoconductive switch having a SiC or other wide band gap substrate material with opposing contoured profile cavities which have a contoured profile selected from one of Rogowski, Bruce, Chang, Harrison, and Ernst profiles, and two electrodes with matching contoured-profile convex interface surfaces.
Luedemann, Alexander; Strassburg, Katrin; Erban, Alexander; Kopka, Joachim
2008-03-01
Typical GC-MS-based metabolite profiling experiments may comprise hundreds of chromatogram files, which each contain up to 1000 mass spectral tags (MSTs). MSTs are the characteristic patterns of approximately 25-250 fragment ions and respective isotopomers, which are generated after gas chromatography (GC) by electron impact ionization (EI) of the separated chemical molecules. These fragment ions are subsequently detected by time-of-flight (TOF) mass spectrometry (MS). MSTs of profiling experiments are typically reported as a list of ions, which are characterized by mass, chromatographic retention index (RI) or retention time (RT), and arbitrary abundance. The first two parameters allow the identification, the later the quantification of the represented chemical compounds. Many software tools have been reported for the pre-processing, the so-called curve resolution and deconvolution, of GC-(EI-TOF)-MS files. Pre-processing tools generate numerical data matrices, which contain all aligned MSTs and samples of an experiment. This process, however, is error prone mainly due to (i) the imprecise RI or RT alignment of MSTs and (ii) the high complexity of biological samples. This complexity causes co-elution of compounds and as a consequence non-selective, in other words impure MSTs. The selection and validation of optimal fragment ions for the specific and selective quantification of simultaneously eluting compounds is, therefore, mandatory. Currently validation is performed in most laboratories under human supervision. So far no software tool supports the non-targeted and user-independent quality assessment of the data matrices prior to statistical analysis. TagFinder may fill this gap. TagFinder facilitates the analysis of all fragment ions, which are observed in GC-(EI-TOF)-MS profiling experiments. The non-targeted approach allows the discovery of novel and unexpected compounds. In addition, mass isotopomer resolution is maintained by TagFinder processing. This feature is essential for metabolic flux analyses and highly useful, but not required for metabolite profiling. Whenever possible, TagFinder gives precedence to chemical means of standardization, for example, the use of internal reference compounds for retention time calibration or quantitative standardization. In addition, external standardization is supported for both compound identification and calibration. The workflow of TagFinder comprises, (i) the import of fragment ion data, namely mass, time and arbitrary abundance (intensity), from a chromatography file interchange format or from peak lists provided by other chromatogram pre-processing software, (ii) the annotation of sample information and grouping of samples into classes, (iii) the RI calculation, (iv) the binning of observed fragment ions of equal mass from different chromatograms into RI windows, (v) the combination of these bins, so-called mass tags, into time groups of co-eluting fragment ions, (vi) the test of time groups for intensity correlated mass tags, (vii) the data matrix generation and (viii) the extraction of selective mass tags supported by compound identification. Thus, TagFinder supports both non-targeted fingerprinting analyses and metabolite targeted profiling. Exemplary TagFinder workspaces and test data sets are made available upon request to the contact authors. TagFinder is made freely available for academic use from http://www-en.mpimp-golm.mpg.de/03-research/researchGroups/01-dept1/Root_Metabolism/smp/TagFinder/index.html.
ELUTION OF URANIUM VALUES FROM ION EXCHANGE RESINS
Kennedy, R.H.
1959-11-24
A process is described for eluting complex uranium ions absorbed on ion exchange resins. The resin is subjected to the action of an aqueous eluting solution contuining sulfuric acid and an alkali metal, ammonium, or magnesium chloride or nitrate, the elution being carried out until the desired amount of the uranium is removed from the resin.
NASA Technical Reports Server (NTRS)
King, Michael D.; Menzel, W. Paul; Kaufman, Yoram J.; Tanre, Didier; Gao, Bo-Cai; Platnick, Steven; Ackerman, Steven A.; Remer, Lorraine A.; Pincus, Robert; Hubanks, Paul A.
2003-01-01
The Moderate Resolution Imaging Spectroradiometer (MODIS) is an earth-viewing sensor that flies on the Earth Observing System (EOS) Terra and Aqua satellites, launched in 1999 and 2002, respectively. MODIS scans a swath width of 2330 km that is sufficiently wide to provide nearly complete global coverage every two days from a polar-orbiting, sun-synchronous, platform at an altitude of 705 km. MODIS provides images in 36 spectral bands between 0.415 and 14.235 pm with spatial resolutions of 250 m (2 bands), 500 m (5 bands) and 1000 m (29 bands). These bands have been carefully selected to en- able advanced studies of land, ocean, and atmospheric properties. Twenty-six bands are used to derive atmospheric properties such as cloud mask, atmospheric profiles, aerosol properties, total precipitable water, and cloud properties. In this paper we describe each of these atmospheric data products, including characteristics of each of these products such as file size, spatial resolution used in producing the product, and data availability.
Covalently Linked Tandem Lesions in DNA
Patrzyc, Helen B.; Dawidzik, Jean B.; Budzinski, Edwin E.; Freund, Harold G.; Wilton, John H.; Box, Harold C.
2013-01-01
Reactive oxygen species (ROS) generate a type of DNA damage called tandem lesions, two adjacent nucleotides both modified. A subcategory of tandem lesions consists of adjacent nucleotides linked by a covalent bond. Covalently linked tandem lesions generate highly characteristic liquid chromotography-tandem mass spectrometry (LC-MS/MS) elution profiles. We have used this property to comprehensively survey X-irradiated DNA for covalently linked tandem lesions. A total of 15 tandem lesions were detected in DNA irradiated in deoxygenated aqueous solution, five tandem lesions were detected in DNA that was irradiated in oxygenated solution. PMID:23106212
The 11.2 μm emission of PAHs in astrophysical objects
NASA Astrophysics Data System (ADS)
Candian, A.; Sarre, P. J.
2015-04-01
The 11.2-μm emission band belongs to the family of the `unidentified' infrared emission bands seen in many astronomical environments. In this work, we present a theoretical interpretation of the band characteristics and profile variation for a number of astrophysical sources in which the carriers are subject to a range of physical conditions. The results of Density Functional Theory calculations for the solo out-of-plane vibrational bending modes of large polycyclic aromatic hydrocarbon (PAH) molecules are used as input for a detailed emission model which includes the temperature and mass dependence of PAH band wavelength, and a PAH mass distribution that varies with object. Comparison of the model with astronomical spectra indicates that the 11.2-μm band asymmetry and profile variation can be explained principally in terms of the mass distribution of neutral PAHs with a small contribution from anharmonic effects.
Measurement of temperature profiles in flames by emission-absorption spectroscopy
NASA Technical Reports Server (NTRS)
Simmons, F. S.; Arnold, C. B.; Lindquist, G. H.
1972-01-01
An investigation was conducted to explore the use of infrared and ultraviolet emission-absorption spectroscopy for determination of temperature profiles in flames. Spectral radiances and absorptances were measured in the 2.7-micron H2O band and the 3064-A OH band in H2/O2 flames for several temperature profiles which were directly measured by a sodium line-reversal technique. The temperature profiles, determined by inversion of the infrared and ultraviolet spectra, showed an average disagreement with line-reversal measurements of 50 K for the infrared and 200 K for the ultraviolet at a temperature of 2600 K. The reasons for these discrepancies are discussed in some detail.
ON PREDICTING INFRAGRAVITY ENERGY IN THE SURF ZONE.
Sallenger,, Asbury H.; Holman, Robert A.; Edge, Billy L.
1985-01-01
Flow data were obtained in the surf zone across a barred profile during a storm. RMS cross-shore velocities due to waves in the intragravity band (wave periods greater than 20 s) had maxima in excess of 0. 5 m/s over the bar crest. For comparison to measured spectra, synthetic spectra of cross-shore flow were computed using measured nearshore profiles. The structure, in the infragravity band, of these synthetic spectra corresponded reasonably well with the structure of the measured spectra. Total variances of measured cross-shore flow within the infragravity band were nondimensionalized by dividing by total infragravity variances of synthetic spectra. These nondimensional variances were independent of distance offshore and increased with the square of the breaker height. Thus, cross-shore flow due to infragravity waves can be estimated with knowledge of the nearshore profile and incident wave conditions. Refs.
Lemos, Pedro A; Abizaid, Alexandre A C; Meireles, George C; Sarmento-Leite, Rogério; Prudente, Mauricio; Cantarelli, Marcelo; Dourado, Adriano D; Mariani, Jose; Perin, Marco A; Costantini, Costantino; Costa, Ricardo A; Costa, José Ribamar; Chamie, Daniel; Campos, Carlos A; Ribeiro, Expedito
2015-12-01
To evaluate the outcomes of patients treated with a new drug-eluting stent formulation with low doses of sirolimus, built in an ultra-thin-strut platform coated with biodegradable abluminal coating. This study is a randomized trial that tested the main hypothesis that the angiographic late lumen loss of the novel sirolimus-eluting stent is noninferior compared with commercially available biolimus-eluting stent. A final study population comprising 170 patients with one or two de novo lesions was randomized in the ratio 2:1 for sirolimus-eluting stent or biolimus-eluting stent, respectively. The primary endpoint was 9-month angiographic in-stent late lumen loss. Adverse clinical events were prospectively collected for 1 year. After 9 months, the novel sirolimus-eluting stent was shown noninferior compared with the biolimus stent for the primary endpoint (angiographic in-stent late lumen loss: 0.20 ± 0.29 mm vs. 0.15 ± 0.20 mm, respectively; P value for noninferiority <0.001). The 1-year incidence of death, myocardial infarction, repeat revascularization, and stent thrombosis remained low and not significantly different between the groups. The present randomized trial demonstrates that the tested novel sirolimus-eluting stent was angiographically noninferior in comparison with a last-generation biolimus-eluting stent. © 2015 John Wiley & Sons Ltd.
Jakobsen, Simon S; Christensen, Jan H; Verdier, Sylvain; Mallet, Claude R; Nielsen, Nikoline J
2017-09-05
This work demonstrates the development of an online two-dimensional liquid chromatography (2D-LC) method where the first dimension column is eluted by a sequence of pulses of increasing eluotropic strength generated by the LC pumps (pulsed-elution 2D-LC). Between the pulses, the first dimension is kept in a no-elution state using low eluent strength. The eluate from the first dimension is actively modulated using trap columns and subsequently analyzed in the second dimension. We demonstrate that by tuning the length and eluotropic strength of the pulses, peaks with retention factors in water, k w , above 150 can be manipulated to elute in 3-4 pulses. The no-elution state can be kept for 1-10 min with only minor changes as to which and how many pulses the peaks elute in. Pulsed-elution 2D-LC combined with active modulation tackles three of the main challenges encountered in 2D-LC and specifically online comprehensive 2D-LC: undersampling, difficulties in refocusing, and lack of flexibility in the selection of column dimensions and flow rates because the two dimensions constrain each other. The pulsed-elution 2D-LC was applied for the analysis of a basic fraction of vacuum gas oil. Peak capacity was 4018 for a 540 min analysis and 4610 for a 1040 min analysis.
An optimized method for elution of enteroviral RNA from a cellulose-based substrate.
Li, Yan; Yoshida, Hiromu; Wang, Lu; Tao, Zexin; Wang, Haiyan; Lin, Xiaojuan; Xu, Aiqiang
2012-12-01
The Flinders Technology Australia (FTA) Elute Card is a commercial product that facilitates the collection, transport, archiving and processing of nucleic acids from a wide variety of biological samples at room temperature. While the cards have been designed so that sterile/deionized water can elute DNA easily, they are not suitable for some less stable RNAs. This study was undertaken to determine the optimal conditions such as the buffer type, buffer pH and incubation temperature for the elution of enteroviral RNA from FTA Elute Cards prior to quantitative analysis using real-time PCR (qPCR) or consensus degenerate hybrid oligonucleotide primer VP1 RT-semi nested PCR (CODEHOP VP1 RT-snPCR). TE-1 (pH 8.0), rather than sterile water, was the best buffer for high efficiency elution of enteroviral RNA at 95°C. However, as the estimated recovery rate of viral RNA eluted from the cards averaged to be only 6.1%, enterovirus assays using FTA elution should be considered qualitative, especially at low virus titers, and therefore the results of the assay should be interpreted carefully. Copyright © 2012 Elsevier B.V. All rights reserved.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Lencioni, Riccardo, E-mail: riccardo.lencioni@med.unipi.it; Baere, Thierry de; Burrel, Marta
2012-10-15
Tranarterial chemoembolization (TACE) has been established by a meta-analysis of randomized controlled trials as the standard of care for nonsurgical patients with large or multinodular noninvasive hepatocellular carcinoma (HCC) isolated to the liver and with preserved liver function. Although conventional TACE with administration of an anticancer-in-oil emulsion followed by embolic agents has been the most popular technique, the introduction of embolic drug-eluting beads has provided an alternative to lipiodol-based regimens. Experimental studies have shown that TACE with drug-eluting beads has a safe pharmacokinetic profile and results in effective tumor killing in animal models. Early clinical experiences have confirmed that drug-elutingmore » beads provide a combined ischemic and cytotoxic effect locally with low systemic toxic exposure. Recently, the clinical value of a TACE protocol performed by using the embolic microsphere DC Bead loaded with doxorubicin (DEBDOX; drug-eluting bead doxorubicin) has been shown by randomized controlled trials. An important limitation of conventional TACE has been the inconsistency in the technique and the treatment schedules. This limitation has hampered the acceptance of TACE as a standard oncology treatment. Doxorubicin-loaded DC Bead provides levels of consistency and repeatability not available with conventional TACE and offers the opportunity to implement a standardized approach to HCC treatment. With this in mind, a panel of physicians took part in a consensus meeting held during the European Conference on Interventional Oncology in Florence, Italy, to develop a set of technical recommendations for the use of DEBDOX in HCC treatment. The conclusions of the expert panel are summarized.« less
Hehn, Mathias; Wagner, Thomas; Hiller, Wolf
2014-01-07
Online LCCC-NMR and SEC-NMR are compared regarding the determination of molar masses of block copolymers. Two different direct referencing methods are particularly demonstrated in LCCC-NMR for a detailed characterization of diblock copolymers and their co-monomers. First, an intramolecular reference group was used for the direct determination of block lengths and molar masses. For the first time, it was shown that LCCC-NMR can be used for an accurate determination of Mw and Mn of copolymers. These data were in perfect agreement with SEC-NMR measurements using the same intramolecular referencing method. In contrast, the determination of molar masses with common relative methods based on calibrations with homopolymers delivered inaccurate results for all investigated diblock copolymers due to different hydrodynamic volumes of the diblock copolymer compared to their homopolymers. The intramolecular referencing method provided detailed insights in the co-monomer behavior during the chromatographic separation of LCCC. Especially, accurate chain lengths and chemical compositions of the "invisible" and "visible" blocks were quantified during the elution under critical conditions and provided new aspects to the concept of critical conditions. Second, an external reference NMR signal was used to directly determine concentrations and molar masses of the block copolymers from the chromatographic elution profile. Consequently, the intensity axes of the resulting chromatograms were converted to molar amounts and masses, allowing for determination of the amount of polymer chains with respect to elution volume, the evaluation of the limiting magnitude of concentration for LCCC-NMR, and determination of the molar masses of copolymers.
Verheye, Stefan; Khattab, Ahmed A; Carrie, Didier; Stella, Pieter; Slagboom, Ton; Bartunek, Jozef; Onuma, Yoshinobu; Serruys, Patrick W
2016-08-05
Our aim was to demonstrate the safety and efficacy of the Svelte sirolimus-eluting coronary stent-on-a-wire Integrated Delivery System (IDS) with bioresorbable drug coating compared to the Resolute Integrity zotarolimus-eluting stent with durable polymer in patients with de novo coronary artery lesions. Direct stenting, particularly in conjunction with transradial intervention (TRI), has been associated with reduced bleeding complications, procedure time, radiation exposure and contrast administration compared to conventional stenting with wiring and predilatation. The low-profile Svelte IDS is designed to facilitate TRI and direct stenting, reducing the number of procedural steps, time and cost associated with coronary stenting. DIRECT II was a prospective, multicentre trial which enrolled 159 patients to establish non-inferiority of the Svelte IDS versus Resolute Integrity using a 2:1 randomisation. The primary endpoint was angiographic in-stent late lumen loss (LLL) at six months. Target vessel failure (TVF), as well as secondary clinical endpoints, will be assessed annually up to five years. At six months, in-stent LLL was 0.09±0.31 mm in the Svelte IDS group compared to 0.13±0.27 mm in the Resolute Integrity group (p<0.001 for non-inferiority). TVF at one year was similar across the Svelte IDS and Resolute Integrity groups (6.5% vs. 9.8%, respectively). DIRECT II demonstrated the non-inferiority of the Svelte IDS to Resolute Integrity with respect to in-stent LLL at six months. Clinical outcomes at one year were comparable between the two groups.
Geometric flow control of shear bands by suppression of viscous sliding
Viswanathan, Koushik; Mahato, Anirban; Sundaram, Narayan K.; M'Saoubi, Rachid; Trumble, Kevin P.; Chandrasekar, Srinivasan
2016-01-01
Shear banding is a plastic flow instability with highly undesirable consequences for metals processing. While band characteristics have been well studied, general methods to control shear bands are presently lacking. Here, we use high-speed imaging and micro-marker analysis of flow in cutting to reveal the common fundamental mechanism underlying shear banding in metals. The flow unfolds in two distinct phases: an initiation phase followed by a viscous sliding phase in which most of the straining occurs. We show that the second sliding phase is well described by a simple model of two identical fluids being sheared across their interface. The equivalent shear band viscosity computed by fitting the model to experimental displacement profiles is very close in value to typical liquid metal viscosities. The observation of similar displacement profiles across different metals shows that specific microstructure details do not affect the second phase. This also suggests that the principal role of the initiation phase is to generate a weak interface that is susceptible to localized deformation. Importantly, by constraining the sliding phase, we demonstrate a material-agnostic method—passive geometric flow control—that effects complete band suppression in systems which otherwise fail via shear banding. PMID:27616920
Geometric flow control of shear bands by suppression of viscous sliding
NASA Astrophysics Data System (ADS)
Sagapuram, Dinakar; Viswanathan, Koushik; Mahato, Anirban; Sundaram, Narayan K.; M'Saoubi, Rachid; Trumble, Kevin P.; Chandrasekar, Srinivasan
2016-08-01
Shear banding is a plastic flow instability with highly undesirable consequences for metals processing. While band characteristics have been well studied, general methods to control shear bands are presently lacking. Here, we use high-speed imaging and micro-marker analysis of flow in cutting to reveal the common fundamental mechanism underlying shear banding in metals. The flow unfolds in two distinct phases: an initiation phase followed by a viscous sliding phase in which most of the straining occurs. We show that the second sliding phase is well described by a simple model of two identical fluids being sheared across their interface. The equivalent shear band viscosity computed by fitting the model to experimental displacement profiles is very close in value to typical liquid metal viscosities. The observation of similar displacement profiles across different metals shows that specific microstructure details do not affect the second phase. This also suggests that the principal role of the initiation phase is to generate a weak interface that is susceptible to localized deformation. Importantly, by constraining the sliding phase, we demonstrate a material-agnostic method-passive geometric flow control-that effects complete band suppression in systems which otherwise fail via shear banding.
Quintana, José Benito; Miró, Manuel; Estela, José Manuel; Cerdà, Víctor
2006-04-15
In this paper, the third generation of flow injection analysis, also named the lab-on-valve (LOV) approach, is proposed for the first time as a front end to high-performance liquid chromatography (HPLC) for on-line solid-phase extraction (SPE) sample processing by exploiting the bead injection (BI) concept. The proposed microanalytical system based on discontinuous programmable flow features automated packing (and withdrawal after single use) of a small amount of sorbent (<5 mg) into the microconduits of the flow network and quantitative elution of sorbed species into a narrow band (150 microL of 95% MeOH). The hyphenation of multisyringe flow injection analysis (MSFIA) with BI-LOV prior to HPLC analysis is utilized for on-line postextraction treatment to ensure chemical compatibility between the eluate medium and the initial HPLC gradient conditions. This circumvents the band-broadening effect commonly observed in conventional on-line SPE-based sample processors due to the low eluting strength of the mobile phase. The potential of the novel MSFI-BI-LOV hyphenation for on-line handling of complex environmental and biological samples prior to reversed-phase chromatographic separations was assessed for the expeditious determination of five acidic pharmaceutical residues (viz., ketoprofen, naproxen, bezafibrate, diclofenac, and ibuprofen) and one metabolite (viz., salicylic acid) in surface water, urban wastewater, and urine. To this end, the copolymeric divinylbenzene-co-n-vinylpyrrolidone beads (Oasis HLB) were utilized as renewable sorptive entities in the micromachined unit. The automated analytical method features relative recovery percentages of >88%, limits of detection within the range 0.02-0.67 ng mL(-1), and coefficients of variation <11% for the column renewable mode and gives rise to a drastic reduction in operation costs ( approximately 25-fold) as compared to on-line column switching systems.
Huang, Wenjiang; Zhou, Xianfeng; Ye, Huichun; Dong, Yingying
2017-01-01
Monitoring the vertical profile of leaf chlorophyll (Chl) content within winter wheat canopies is of significant importance for revealing the real nutritional status of the crop. Information on the vertical profile of Chl content is not accessible to nadir-viewing remote or proximal sensing. Off-nadir or multi-angle sensing would provide effective means to detect leaf Chl content in different vertical layers. However, adequate information on the selection of sensitive spectral bands and spectral index formulas for vertical leaf Chl content estimation is not yet available. In this study, all possible two-band and three-band combinations over spectral bands in normalized difference vegetation index (NDVI)-, simple ratio (SR)- and chlorophyll index (CI)-like types of indices at different viewing angles were calculated and assessed for their capability of estimating leaf Chl for three vertical layers of wheat canopies. The vertical profiles of Chl showed top-down declining trends and the patterns of band combinations sensitive to leaf Chl content varied among different vertical layers. Results indicated that the combinations of green band (520 nm) with NIR bands were efficient in estimating upper leaf Chl content, whereas the red edge (695 nm) paired with NIR bands were dominant in quantifying leaf Chl in the lower layers. Correlations between published spectral indices and all NDVI-, SR- and CI-like types of indices and vertical distribution of Chl content showed that reflectance measured from 50°, 30° and 20° backscattering viewing angles were the most promising to obtain information on leaf Chl in the upper-, middle-, and bottom-layer, respectively. Three types of optimized spectral indices improved the accuracy for vertical leaf Chl content estimation. The optimized three-band CI-like index performed the best in the estimation of vertical distribution of leaf Chl content, with R2 of 0.84–0.69, and RMSE of 5.37–5.56 µg/cm2 from the top to the bottom layers, while the optimized SR-like index was recommended for the bottom Chl estimation due to its simple and universal form. We suggest that it is necessary to take into account the penetration characteristic of the light inside the canopy for different Chl absorption regions of the spectrum and the formula used to derive spectral index when estimating the vertical profile of leaf Chl content using off-nadir hyperspectral data. PMID:29168757
Variability in Comet P/Swift-Tuttle
NASA Technical Reports Server (NTRS)
Schulz, Rita; Mcfadden, Lucy A.; Chamberlin, Alan B.; A'Hearn, Michael F.; Schleicher, David G.
1994-01-01
Spatial profiles of the coma of Comet P/Swift-Tuttle perpendicular to the projected Sun-comet line were obtained for the emission bands of CN, C2, and C3 as well as for two continuum bands from spectrophotometric observations taken from Oct. 5 to 8, 1992. The intensities were converted into emissivities per sq km in the cases of the continua and into column densities for the emission band profiles. Spatial and temporal variabilities have been found in all five investigated components, which are consistent with the rotational period of the nucleus determined from the observations of the comet during its last perihelion passage in 1862. The emission band profiles were fitted with the vectorial model and the production rates of CN, C2, and C3 were determined. One half of the profiles was fitted adequately under steady state conditions for the production rate in a first approximation, whereas the other half showed prominent bumps, which could only be explained by introducing a time-dependent production rate. Further investigations showed evidence for the presence of gaseous as well as dust jets in the coma, which indicated the presence of at least two active areas on the surface of the nucleus. The projected radial expansion velocities of two different features were determined to be (430 +/- 100) and (460 +/- 100) m/sec, respectively.
Park, Yongwoo; Malacarne, Antonio; Azaña, José
2011-02-28
A simple, highly accurate measurement technique for real-time monitoring of the group delay (GD) profiles of photonic dispersive devices over ultra-broad spectral bandwidths (e.g. an entire communication wavelength band) is demonstrated. The technique is based on time-domain self-interference of an incoherent light pulse after linear propagation through the device under test, providing a measurement wavelength range as wide as the source spectral bandwidth. Significant enhancement in the signal-to-noise ratio of the self-interference signal has been observed by use of a relatively low-noise incoherent light source as compared with the theoretical estimate for a white-noise light source. This fact combined with the use of balanced photo-detection has allowed us to significantly reduce the number of profiles that need to be averaged to reach a targeted GD measurement accuracy, thus achieving reconstruction of the device GD profile in real time. We report highly-accurate monitoring of (i) the group-delay ripple (GDR) profile of a 10-m long chirped fiber Bragg grating over the full C band (~42 nm), and (ii) the group velocity dispersion (GVD) and dispersion slope (DS) profiles of a ~2-km long dispersion compensating fiber module over an ~72-nm wavelength range, both captured at a 15 frames/s video rate update, with demonstrated standard deviations in the captured GD profiles as low as ~1.6 ps.
Lin, Bin; Braster, Martin; van Breukelen, Boris M.; van Verseveld, Henk W.; Westerhoff, Hans V.; Röling, Wilfred F. M.
2005-01-01
Relationships between community composition of the iron-reducing Geobacteraceae, pollution levels, and the occurrence of biodegradation were established for an iron-reducing aquifer polluted with landfill leachate by using cultivation-independent Geobacteraceae 16S rRNA gene-targeting techniques. Numerical analysis of denaturing gradient gel electrophoresis (DGGE) profiles and sequencing revealed a high Geobacteraceae diversity and showed that community composition within the leachate plume differed considerably from that of the unpolluted aquifer. This suggests that pollution has selected for specific species out of a large pool of Geobacteraceae. DGGE profiles of polluted groundwater taken near the landfill (6- to 39-m distance) clustered together. DGGE profiles from less-polluted groundwater taken further downstream did not fall in the same cluster. Several individual DGGE bands were indicative of either the redox process or the level of pollution. This included a pollution-indicative band that dominated the DGGE profiles from groundwater samples taken close to the landfill (6 to 39 m distance). The clustering of these profiles and the dominance by a single DGGE band corresponded to the part of the aquifer where organic micropollutants and reactive dissolved organic matter were attenuated at relatively high rates. PMID:16204512
Kang, Si-Hyuck; Chae, In-Ho; Park, Jin-Joo; Lee, Hak Seung; Kang, Do-Yoon; Hwang, Seung-Sik; Youn, Tae-Jin; Kim, Hyo-Soo
2016-06-27
This study sought to perform a systematic review and network meta-analysis to compare the relative safety and efficacy of contemporary DES and BVS. To improve outcomes of patients undergoing percutaneous coronary revascularization, there have been advances in the design of drug-eluting stents (DES), including the development of drug-eluting bioresorbable vascular scaffolds (BVS). Prospective, randomized, controlled trials comparing bare-metal stents (BMS), paclitaxel-eluting stents (PES), sirolimus-eluting stents (SES), Endeavor zotarolimus-eluting stents (E-ZES), cobalt-chromium (CoCr) everolimus-eluting stents (EES), platinum-chromium (PtCr)-EES, biodegradable polymer (BP)-EES, Resolute zotarolimus-eluting stents (R-ZES), BP biolimus-eluting stents (BP-BES), hybrid sirolimus-eluting stents (H [Orsiro]-SES), polymer-free sirolimus- and probucol-eluting stents, or BVS were searched in online databases. The primary endpoint was definite or probable stent thrombosis at 1 year. A total of 147 trials including 126,526 patients were analyzed in this study. All contemporary DES were superior to BMS and PES in terms of definite or probable stent thrombosis at 1 year. CoCr-EES, PtCr-EES, and H-SES were associated with significantly lower risk than BVS. CoCr-EES and H-SES were superior to SES and BP-BES. The risk of myocardial infarction was significantly lower with H-SES than with BVS. There were no significant differences regarding all-cause or cardiac mortality. Contemporary devices including BVS showed comparably low risks of repeat revascularization. Contemporary DES, including biocompatible DP-DES, BP-DES, and polymer-free DES, showed a low risk of definite or probable stent thrombosis at 1 year. BVS had an increased risk of device thrombosis compared with CoCr-EES, PtCr-EES, and H-SES. Data from extended follow-up are warranted to confirm the long-term safety of contemporary coronary devices. Copyright © 2016 American College of Cardiology Foundation. Published by Elsevier Inc. All rights reserved.
Lee, Yi Feng; Jöhnck, Matthias; Frech, Christian
2018-02-21
The efficiencies of mono gradient elution and dual salt-pH gradient elution for separation of six mAb charge and size variants on a preparative-scale ion exchange chromatographic resin are compared in this study. Results showed that opposite dual salt-pH gradient elution with increasing pH gradient and simultaneously decreasing salt gradient is best suited for the separation of these mAb charge and size variants on Eshmuno ® CPX. Besides giving high binding capacity, this type of opposite dual salt-pH gradient also provides better resolved mAb variant peaks and lower conductivity in the elution pools compared to single pH or salt gradients. To have a mechanistic understanding of the differences in mAb variants retention behaviors of mono pH gradient, parallel dual salt-pH gradient, and opposite dual salt-pH gradient, a linear gradient elution model was used. After determining the model parameters using the linear gradient elution model, 2D plots were used to show the pH and salt dependencies of the reciprocals of distribution coefficient, equilibrium constant, and effective ionic capacity of the mAb variants in these gradient elution systems. Comparison of the 2D plots indicated that the advantage of opposite dual salt-pH gradient system with increasing pH gradient and simultaneously decreasing salt gradient is the noncontinuous increased acceleration of protein migration. Furthermore, the fitted model parameters can be used for the prediction and optimization of mAb variants separation in dual salt-pH gradient and step elution. © 2018 American Institute of Chemical Engineers Biotechnol. Prog., 2018. © 2018 American Institute of Chemical Engineers.
Fujiwara, Keigo; Cabanos, Cerrone; Toyota, Kenji; Kobayashi, Yasunori; Maruyama, Nobuyuki
2014-06-01
Basic 7S globulin (Bg7S), which accumulates in mature soybean (Glycine max) seeds, is an extracellular matrix protein. A large amount of Bg7S is synthesized de novo and is eluted from soybean seeds when immersed in 50-60°C water (hot water treatment, HWT). However, the Bg7S elution mechanism remains unclear. Under HWT, the seeds probably undergo heat stress and flooding stress. To obtain fundamental knowledge related to how Bg7S is eluted from hot-water-treated seeds, this study compared Bg7S elution among soybean cultivars having different flooding tolerance during pre-germination. The amounts of Bg7S eluted from seeds varied significantly among cultivars. Elution was suppressed by seed coats regarded as preventing the leakage of seed contents by rapid water imbibition. Furthermore, Bg7S expression levels differed among cultivars, although the difference did not result from any variation in Bg7S promoter sequences. However, the expression levels of Bg7S under HWT were not associated with the flooding tolerance level. Immunoelectron microscopy revealed that the Bg7S accumulated in the intercellular space of hot-water-treated seeds. Plasma membrane shrinkage was observed. The main proteins eluted from seeds under HWT were located in the extracellular space. This study clarified the mechanism of Bg7S elution from seeds under HWT. Copyright © 2013 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Guiochon, Georges
The goal of our research was a fundamental investigation of methods available for the coupling of two separate chromatographic separations that would considerably enhance the individual separation power of each of these two separations. This gain arises from the combination of two independent retention mechanisms, one of them separating the components that coelute on the other column, making possible the separation of many more compounds in a given time. The two separation mechanisms used must be very different. This is possible because many retention mechanisms are available, using different kinds of molecular interactions, hydrophobic or hydrophilic interactions, polar interactions, hydrogenmore » bonding, complex formation, ionic interactions, steric exclusion. Two methods can be used, allowing separations to be performed in space (spreading the bands of sample components on a plate covered with stationary phase layer) or in time (eluting the sample components through a column and detecting the bands leaving the column). Both offer a wide variety of possible combinations and were studied.« less
Characterization of two N-acetyl muramoylhydrolases of Streptococcus faecium ATCC 9790
DOE Office of Scientific and Technical Information (OSTI.GOV)
Dolinger, D.L.
Purified muramidase-1 of S. faecium has been shown to contain a covalently attached nucleotide. The nucleotide was isolated and identified as 5-mercaptouridine monophosphate, and to occur as multiple monomeric substitutions on the polypeptide chain, via a phosphodiester bond. Exhaustive proteolytic hydrolysis of purified muramidase-1 yielded a peptide fragment consisting of 5-mercaptouridine, tyrosine, alanine, glycine, and leucine. A second peptidoglycan hydrolase (muramidase-2) has been purified to apparent homogeneity. The enzymatic activity has been shown to be consistent with that of a 3-1,4-N-acetylmuramoylhydrolase and differs in substrate specificity and possibility mechanism of hydrolysis from muramidase-1. Purified enzyme appears as two protein stainingmore » bands of molecular masses 125 and 75 kDa after sodium dodecylsulfate polyacrylamide gel ectrophoresis. Elution and renaturation of the protein bands showed that both proteins contain muramidase-2 activity. In addition both proteins have also been shown to specifically bind ({sup 14}C)penicillin G and been tentatively identified as penicillin binding proteins 1 and 5, respectively.« less
Using spin-label W-band EPR to study membrane fluidity profiles in samples of small volume
NASA Astrophysics Data System (ADS)
Mainali, Laxman; Hyde, James S.; Subczynski, Witold K.
2013-01-01
Conventional and saturation-recovery (SR) EPR at W-band (94 GHz) using phosphatidylcholine spin labels (labeled at the alkyl chain [n-PC] and headgroup [T-PC]) to obtain profiles of membrane fluidity has been demonstrated. Dimyristoylphosphatidylcholine (DMPC) membranes with and without 50 mol% cholesterol have been studied, and the results have been compared with similar studies at X-band (9.4 GHz) (L. Mainali, J.B. Feix, J.S. Hyde, W.K. Subczynski, J. Magn. Reson. 212 (2011) 418-425). Profiles of the spin-lattice relaxation rate (T1-1) obtained from SR EPR measurements for n-PCs and T-PC were used as a convenient quantitative measure of membrane fluidity. Additionally, spectral analysis using Freed's MOMD (microscopic-order macroscopic-disorder) model (E. Meirovitch, J.H. Freed J. Phys. Chem. 88 (1984) 4995-5004) provided rotational diffusion coefficients (R⊥ and R||) and order parameters (S0). Spectral analysis at X-band provided one rotational diffusion coefficient, R⊥. T1-1, R⊥, and R|| profiles reflect local membrane dynamics of the lipid alkyl chain, while the order parameter shows only the amplitude of the wobbling motion of the lipid alkyl chain. Using these dynamic parameters, namely T1-1, R⊥, and R||, one can discriminate the different effects of cholesterol at different depths, showing that cholesterol has a rigidifying effect on alkyl chains to the depth occupied by the rigid steroid ring structure and a fluidizing effect at deeper locations. The nondynamic parameter, S0, shows that cholesterol has an ordering effect on alkyl chains at all depths. Conventional and SR EPR measurements with T-PC indicate that cholesterol has a fluidizing effect on phospholipid headgroups. EPR at W-band provides more detailed information about the depth-dependent dynamic organization of the membrane compared with information obtained at X-band. EPR at W-band has the potential to be a powerful tool for studying membrane fluidity in samples of small volume, ˜30 nL, compared with a representative sample volume of ˜3 μL at X-band.
Costa, Fernanda das Neves; Jerz, Gerold; Figueiredo, Fabiana de Souza; Winterhalter, Peter; Leitão, Gilda Guimarães
2015-03-13
For the development of an efficient two-stage isolation process for high-speed countercurrent chromatography (HSCCC) with focus on principal metabolites from the ethyl acetate extract of the halophyte plant Salicornia gaudichaudiana, separation selectivities of two different biphasic solvent systems with similar polarities were evaluated using the elution and extrusion approach. Efficiency in isolation of target compounds is determined by the solvent system selectivity and their chronological use in multiple separation steps. The system n-hexane-ethyl acetate-methanol-water (0.5:6:0.5:6, v/v/v/v) resulted in a comprehensive separation of polyphenolic glycosides. The system n-hexane-n-butanol-water (1:1:2, v/v/v) was less universal but was highly efficient in the fractionation of positional isomers such as di-substituted cinnamic acid quinic acid derivatives. Multiple metabolite detection performed on recovered HSCCC tube fractions was done with rapid mass-spectrometry profiling by sequential off-line injections to electrospray mass-spectrometry (ESI-MS/MS). Selective ion traces of metabolites delivered reconstituted preparative HSCCC runs. Molecular weight distribution of target compounds in single HSCCC tube fractions and MS/MS fragment data were available. Chromatographic areas with strong co-elution effects and fractions of pure recoverable compounds were visualized. In total 11 metabolites have been identified and monitored. Result of this approach was a fast isolation protocol for S. gaudichaudiana metabolites using two solvent systems in a strategic sequence. The process could easily be scaled-up to larger lab-scale or industrial recovery. Copyright © 2015 Elsevier B.V. All rights reserved.
Peak distortion effects in analytical ion chromatography.
Wahab, M Farooq; Anderson, Jordan K; Abdelrady, Mohamed; Lucy, Charles A
2014-01-07
The elution profile of chromatographic peaks provides fundamental understanding of the processes that occur in the mobile phase and the stationary phase. Major advances have been made in the column chemistry and suppressor technology in ion chromatography (IC) to handle a variety of sample matrices and ions. However, if the samples contain high concentrations of matrix ions, the overloaded peak elution profile is distorted. Consequently, the trace peaks shift their positions in the chromatogram in a manner that depends on the peak shape of the overloading analyte. In this work, the peak shapes in IC are examined from a fundamental perspective. Three commercial IC columns AS16, AS18, and AS23 were studied with borate, hydroxide and carbonate as suppressible eluents. Monovalent ions (chloride, bromide, and nitrate) are used as model analytes under analytical (0.1 mM) to overload conditions (10-500 mM). Both peak fronting and tailing are observed. On the basis of competitive Langmuir isotherms, if the eluent anion is more strongly retained than the analyte ion on an ion exchanger, the analyte peak is fronting. If the eluent is more weakly retained on the stationary phase, the analyte peak always tails under overload conditions regardless of the stationary phase capacity. If the charge of the analyte and eluent anions are different (e.g., Br(-) vs CO3(2-)), the analyte peak shapes depend on the eluent concentration in a more complex pattern. It was shown that there are interesting similarities with peak distortions due to strongly retained mobile phase components in other modes of liquid chromatography.
Cheng, Yanping; Gasior, Pawel; Xia, Jing-Gang; Ramzipoor, Kamal; Lee, Chang; Estrada, Edward A; Dokko, Daniell; McGregor, Jenn C; Conditt, Gerard B; McAndrew, Thomas; Kaluza, Greg L; Granada, Juan F
2017-07-01
Mechanical strength of bioresorbable scaffolds (BRS) is highly dependent on strut dimensions and polymer features. To date, the successful development of thin-walled BRS has been challenging. We compared the biomechanical behavior and vascular healing profile of a novel thin-walled (115 µm) sirolimus-eluting ultrahigh molecular weight amorphous poly-l-lactic acid-based BRS (APTITUDE, Amaranth Medical [AMA]) to Absorb (bioresorbable vascular scaffold [BVS]) using different experimental models. In vitro biomechanical testing showed no fractures in the AMA-BRS when overexpanded 1.3 mm above nominal dilatation values (≈48%) and lower number of fractures on accelerated cycle testing over time (at 21 K cycles=20.0 [19.5-20.5] in BVS versus 4.0 [3.0-4.3] in AMA-BRS). In the healing response study, 35 AMA-BRS and 23 BVS were implanted in 58 coronary arteries of 23 swine and followed-up to 180 days. Scaffold strut healing was evaluated in vivo using weekly optical coherence tomography analysis. At 14 days, the AMA-BRS demonstrated a higher percentage of embedded struts (71.0% [47.6, 89.1] compared with BVS 40.3% [20.5, 63.2]; P =0.01). At 21 days, uncovered struts were still present in the BVS group (3.8% [2.1, 10.2]). Histopathology revealed lower area stenosis (AMA-BRS, 21.0±6.1% versus BVS 31.0±4.5%; P =0.002) in the AMA-BRS at 28 days. Neointimal thickness and inflammatory scores were comparable between both devices at 180 days. A new generation thinned wall BRS displayed a more favorable biomechanical behavior and strut healing profile compared with BVS in normal porcine coronary arteries. This novel BRS concept has the potential to improve the clinical outcomes of current generation BRS. © 2017 American Heart Association, Inc.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Boateng, F; Ngwa, W; Harvard Medical School, Boston, MA
Purpose: Brachytherapy application with in situ dose-painting using gold nanoparticles (GNP) released from GNP-loaded brachytherapy spacers has been proposed as an innovative approach to increase therapeutic efficacy during brachytherapy. This work investigates the dosimetric impact of slow versus burst release of GNP from next generation biodegradable spacers. Methods: Mathematical models were developed based on experimental data to study the release of GNP from a spacer designed with FDA approved poly(lactic-co-glycolic acid) (PLGA) polymer. The diffusion controlled released process and PLGA polymer degradation kinetics was incorporated in the calculations for the first time. An in vivo determined diffusion coefficient was usedmore » for determining the concentration profiles and corresponding dose enhancement based on initial GNP-loading concentrations of 7 mg/g. Results: The results showed that there is significant delay before the concentration profile of GNP diffusion in the tumor is similar to that when burst release is assumed as in previous studies. For example, in the case of burst release after spacer administration, it took up to 25 days for all the GNP to be released from the spacer using diffusion controlled release process only. However, it took up to 45 days when a combined model for both diffusion and polymer degradation processes was used. Based on the tumor concentration profiles, a significant dose enhancement factor (DEF >20%), could be attained at a tumor distances of 5 mm from a spacer loaded with 10 nm GNP sizes. Conclusion: The results highlight the need to take the slow release of GNP from spacers and factors such as biodegradation of polymers into account in research development of GNP-eluting spacers for brachytherapy applications with in-situ dose-painting using gold nanoparticles. The findings suggest that I-125 may be the more appropriate for such applications given the relatively longer half-live compared to other radioisotopes like Pd-103 and Cs-131.« less
Schmidt, Wolfram; Lanzer, Peter; Behrens, Peter; Brandt-Wunderlich, Christoph; Öner, Alper; Ince, Hüseyin; Schmitz, Klaus-Peter; Grabow, Niels
2018-01-08
Drug-eluting stents (DES) compared to bare metal stents (BMS) have shown superior clinical performance, but are considered less suitable in complex cases. Most studies do not distinguish between DES and BMS with respect to their mechanical performance. The objective was to obtain mechanical parameters for direct comparison of BMS and DES. In vitro bench tests evaluated crimped stent profiles, crossability in stenosis models, elastic recoil, bending stiffness (crimped and expanded), and scaffolding properties. The study included five pairs of BMS and DES each with the same stent platforms (all n = 5; PRO-Kinetic Energy, Orsiro: BIOTRONIK AG, Bülach, Switzerland; MULTI-LINK 8, XIENCE Xpedition: Abbott Vascular, Temecula, CA; REBEL Monorail, Promus PREMIER, Boston Scientific, Marlborough, MA; Integrity, Resolute Integrity, Medtronic, Minneapolis, MN; Kaname, Ultimaster: Terumo Corporation, Tokyo, Japan). Statistical analysis used pooled variance t tests for pairwise comparison of BMS with DES. Crimped profiles in BMS groups ranged from 0.97 ± 0.01 mm (PRO-Kinetic Energy) to 1.13 ± 0.01 mm (Kaname) and in DES groups from 1.02 ± 0.01 mm (Orsiro) to 1.13 ± 0.01 mm (Ultimaster). Crossability was best for low profile stent systems. Elastic recoil ranged from 4.07 ± 0.22% (Orsiro) to 5.87 ± 0.54% (REBEL Monorail) including both BMS and DES. The bending stiffness of crimped and expanded stents showed no systematic differences between BMS and DES neither did the scaffolding. Based on in vitro measurements BMS appear superior to DES in some aspects of mechanical performance, yet the differences are small and not class uniform. The data provide assistance in selecting the optimal system for treatment and assessment of new generations of bioresorbable scaffolds. not applicable.
Wide-band profile domain pulsar timing analysis
NASA Astrophysics Data System (ADS)
Lentati, L.; Kerr, M.; Dai, S.; Hobson, M. P.; Shannon, R. M.; Hobbs, G.; Bailes, M.; Bhat, N. D. Ramesh; Burke-Spolaor, S.; Coles, W.; Dempsey, J.; Lasky, P. D.; Levin, Y.; Manchester, R. N.; Osłowski, S.; Ravi, V.; Reardon, D. J.; Rosado, P. A.; Spiewak, R.; van Straten, W.; Toomey, L.; Wang, J.; Wen, L.; You, X.; Zhu, X.
2017-04-01
We extend profile domain pulsar timing to incorporate wide-band effects such as frequency-dependent profile evolution and broad-band shape variation in the pulse profile. We also incorporate models for temporal variations in both pulse width and in the separation in phase of the main pulse and interpulse. We perform the analysis with both nested sampling and Hamiltonian Monte Carlo methods. In the latter case, we introduce a new parametrization of the posterior that is extremely efficient in the low signal-to-noise regime and can be readily applied to a wide range of scientific problems. We apply this methodology to a series of simulations, and to between seven and nine years of observations for PSRs J1713+0747, J1744-1134 and J1909-3744 with frequency coverage that spans 700-3600 Mhz. We use a smooth model for profile evolution across the full frequency range, and compare smooth and piecewise models for the temporal variations in dispersion measure (DM). We find that the profile domain framework consistently results in improved timing precision compared to the standard analysis paradigm by as much as 40 per cent for timing parameters. Incorporating smoothness in the DM variations into the model further improves timing precision by as much as 30 per cent. For PSR J1713+0747, we also detect pulse shape variation uncorrelated between epochs, which we attribute to variation intrinsic to the pulsar at a level consistent with previously published analyses. Not accounting for this shape variation biases the measured arrival times at the level of ˜30 ns, the same order of magnitude as the expected shift due to gravitational waves in the pulsar timing band.
Kirchner, R Michael; Abbott, J Dawn
2009-01-01
Drug-eluting stents (DES) have had a major impact in interventional cardiology. Compared to bare metal stents, they significantly reduce restenosis and the need for target vessel revascularization. Four DES are available in the US, the first-generation sirolimus-eluting (Cypher®) and paclitaxel-eluting (Taxus®) stents and later approved second-generation everolimus-eluting (Xience V®) and zotarolimus-eluting (Endeavor®) stents. The Xience V stent was approved on the basis of clinical efficacy and safety data from 3 studies in the SPIRIT clinical trial program. Within this trial series, the Xience V was superior to its bare metal stent counterpart, the Vision® stent, and noninferior to the paclitaxel-eluting stent for target vessel failure at 9 months. This review provides a comprehensive assessment of the data derived from both the pre- and post-approval randomized controlled trials and registry studies of Xience V that comprise the SPIRIT clinical trial program including recently published mid-term outcomes. The implications of the results in terms of interventional practice will be discussed. PMID:20057901
Ishihara, Takashi; Kadoya, Toshihiko; Endo, Naomi; Yamamoto, Shuichi
2006-05-05
Our simple method for optimization of the elution salt concentration in stepwise elution was applied to the actual protein separation system, which involves several difficulties such as detection of the target. As a model separation system, reducing residual protein A by cation-exchange chromatography in human monoclonal antibody (hMab) purification was chosen. We carried out linear gradient elution experiments and obtained the data for the peak salt concentration of hMab and residual protein A, respectively. An enzyme-linked immunosorbent assay was applied to the measurement of the residual protein A. From these data, we calculated the distribution coefficient of the hMab and the residual protein A as a function of salt concentration. The optimal salt concentration of stepwise elution to reduce the residual protein A from the hMab was determined based on the relationship between the distribution coefficient and the salt concentration. Using the optimized condition, we successfully performed the separation, resulting in high recovery of hMab and the elimination of residual protein A.
Gu, Dongyu; Lazo-Portugal, Rodrigo; Fang, Chen; Wang, Zhantong; Ma, Ying; Knight, Martha; Ito, Yoichiro
2018-06-15
Centrifugal precipitation chromatography (CpC) is a powerful chromatographic technique invented in the year 2000 but so far very little applied. The method combines dialysis, counter-current and salting out processes. The separation rotor consists of two identical spiral channels separated by a dialysis membrane (6-8 K MW cut-off) in which the upper channel is eluted with an ammonium sulfate gradient and the lower channel with water, and the mixtures are separated according to their solubility in ammonium sulfate as a chromatographic technique. In the present study, the method was successfully applied for separation and purification of R-phycoerythrin (R-PE), a protein widely used as a fluorescent probe, from the red alga Gracilaria lemaneiformis. The separation was performed with the elution of ammonium sulfate from 50% to 0% in 21.5 h at a flow rate of 0.5 ml/min, while the lower channel was eluted with water at a flow rate of 0.05 ml/min after sample charge, and the column was rotated at 200 rpm. After a single run, the absorbance ratio A 565 /A 280 (a criterion for the purity of R-PE) was increased from 0.5 of the crude to 6.5. The purified R-PE exhibited a typical "three peaks" spectrum with absorbance maximum at 497, 538 and 565 nm. The Native-PAGE showed one single protein band and 20 kDa (subunits α and β) and 30 kDa (subunit γ) can be observed in SDS-PAGE analysis which were consistent with the (αβ) 6 γ subunit composition of R-PE. The results indicated that CpC is an efficient method to obtain protein with the high purity from a complex source. Copyright © 2018 Elsevier B.V. All rights reserved.
Data descriptions are provided at the following urls:GADEP Continuous PM2.5 mass concentration data - https://aqs.epa.gov/aqsweb/documents/data_mart_welcome.htmlhttps://www3.epa.gov/ttn/amtic/files/ambient/pm25/qa/QA-Handbook-Vol-II.pdfVIIRS Day Night Band SDR (SVDNB) http://www.class.ngdc.noaa.gov/saa/products/search?datatype_family=VIIRS_SDRMODIS Terra Level 2 water vapor profiles (infrared algorithm for atmospheric profiles for both day and night -MOD0&_L2; http://modis-atmos.gsfc.nasa.gov/MOD07_L2/index.html NWS surface meteorological data - https://www.ncdc.noaa.gov/isdThis dataset is associated with the following publication:Wang, J., C. Aegerter, and J. Szykman. Potential Application of VIIRS Day/Night Band for Monitoring Nighttime Surface PM2.5 Air Quality From Space. ATMOSPHERIC ENVIRONMENT. Elsevier Science Ltd, New York, NY, USA, 124(0): 55-63, (2016).
Biggs, Kevin B; Balss, Karin M; Maryanoff, Cynthia A
2012-05-29
Drug release from and coating morphology on a CYPHER sirolimus-eluting coronary stent (SES) during in vitro elution were studied by correlated confocal Raman and atomic force microscopy (CRM and AFM, respectively). Chemical surface and subsurface maps of the SES were generated in the same region of interest by CRM and were correlated with surface topography measured by AFM at different elution times. For the first time, a direct correlation between drug-rich regions and the coating morphology was made on a drug-eluting medical device, linking drug release with pore formation, pore throats, and pore networks. Drug release was studied on a drug-eluting stent (DES) system with a multicomponent carrier matrix (poly(n-butyl methacrylate) [PBMA] and poly(ethylene-co-vinyl acetate) [PEVA]). The polymer was found to rearrange postelution because confluence of the carrier polymer matrix reconstituted the voids created by drug release.
Development of an elution device for ViroCap virus filters.
Fagnant, Christine Susan; Toles, Matthew; Zhou, Nicolette Angela; Powell, Jacob; Adolphsen, John; Guan, Yifei; Ockerman, Byron; Shirai, Jeffry Hiroshi; Boyle, David S; Novosselov, Igor; Meschke, John Scott
2017-10-19
Environmental surveillance of waterborne pathogens is vital for monitoring the spread of diseases, and electropositive filters are frequently used for sampling wastewater and wastewater-impacted surface water. Viruses adsorbed to electropositive filters require elution prior to detection or quantification. Elution is typically facilitated by a peristaltic pump, although this requires a significant startup cost and does not include biosafety or cross-contamination considerations. These factors may pose a barrier for low-resource laboratories that aim to conduct environmental surveillance of viruses. The objective of this study was to develop a biologically enclosed, manually powered, low-cost device for effectively eluting from electropositive ViroCap™ virus filters. The elution device described here utilizes a non-electric bilge pump, instead of an electric peristaltic pump or a positive pressure vessel. The elution device also fully encloses liquids and aerosols that could contain biological organisms, thereby increasing biosafety. Moreover, all elution device components that are used in the biosafety cabinet are autoclavable, reducing cross-contamination potential. This device reduces costs of materials while maintaining convenience in terms of size and weight. With this new device, there is little sample volume loss due to device inefficiency, similar virus yields were demonstrated during seeded studies with poliovirus type 1, and the time to elute filters is similar to that required with the peristaltic pump. The efforts described here resulted in a novel, low-cost, manually powered elution device that can facilitate environmental surveillance of pathogens through effective virus recovery from ViroCap filters while maintaining the potential for adaptability to other cartridge filters.
Alfonso, Fernando; Pérez-Vizcayno, María José; Cuesta, Javier; García Del Blanco, Bruno; García-Touchard, Arturo; López-Mínguez, José Ramón; Masotti, Mónica; Zueco, Javier; Cequier, Angel; Velázquez, Maite; Moreno, Raúl; Mainar, Vicente; Domínguez, Antonio; Moris, Cesar; Molina, Eduardo; Rivero, Fernando; Jiménez-Quevedo, Pilar; Gonzalo, Nieves; Fernández-Pérez, Cristina
2018-05-28
This study sought to compare the long-term safety and efficacy of drug-eluting balloons (DEB) and everolimus-eluting stents (EES) in patients with in-stent restenosis (ISR) of drug-eluting stents (DES). Treatment of patients with DES-ISR remains a challenge. The RIBS IV (Restenosis Intra-Stent of Drug-Eluting Stents: Drug-Eluting Balloons vs Everolimus-Eluting Stents) trial is a prospective multicenter randomized clinical trial comparing DEB and EES in patients with DES-ISR. The pre-specified comparison of the 3-year clinical outcomes obtained with these interventions is the main objective of the present study. A total of 309 patients with DES-ISR were randomized to DEB (n = 154) or EES (n = 155). At angiographic follow-up, the in-segment minimal lumen diameter was larger in the EES arm (2.03 ± 0.7 mm vs. 1.80 ± 0.6 mm; p < 0.01). Three-year clinical follow-up was obtained in all enrolled patients (100%). The combined clinical outcome measure of cardiac death, myocardial infarction and target lesion revascularization was significantly reduced in the EES arm (19 [12.3%] vs. 31 [20.1%]; p = 0.04; hazard ratio: 0.57 [95% confidence interval: 0.34 to 0.96]), driven by a lower need for target lesion revascularization (11 [7.1%] vs. 24 [15.6%]; p = 0.015; hazard ratio: 0.43 [95% confidence interval: 0.21 to 0.87]). The need for "late" (>1 year) target lesion revascularization (2.6% vs. 4%) and target vessel revascularization (4% vs. 6.6%) was similar in the 2 arms. Rates of cardiac death (3.9% vs. 3.2%), myocardial infarction (2.6% vs. 4.5%), and stent thrombosis (1.3% vs. 2.6%) at 3 years were also similar in both arms. The 3-year clinical follow-up of this randomized clinical trial demonstrates that in patients with DES-ISR, EES reduce the need for repeat interventions compared with DEB. (Restenosis Intra-Stent of Drug-Eluting Stents: Drug-Eluting Balloons vs Everolimus-Eluting Stents [RIBS IV]; NCT01239940). Published by Elsevier Inc.
Vidal, Rocío B Pellegrino; Ibañez, Gabriela A; Escandar, Graciela M
2016-10-01
The aim of this study was to develop a novel analytical method for the determination of bisphenol A, nonylphenol, octylphenol, diethyl phthalate, dibutyl phthalate and diethylhexyl phthalate, compounds known for their endocrine-disruptor properties, based on liquid chromatography with simultaneous diode array and fluorescent detection. Following the principles of green analytical chemistry, solvent consumption and chromatographic run time were minimized. To deal with the resulting incomplete resolution in the chromatograms, a second-order calibration was proposed. Second-order data (elution time-absorbance wavelength and elution time-fluorescence emission wavelength matrices) were obtained and processed by multivariate curve resolution-alternating least-squares (MCR-ALS). Applying MCR-ALS allowed quantification of the analytes even in the presence of partially overlapped chromatographic and spectral bands among these compounds and the potential interferents. The obtained results from the analysis of beer, wine, soda, juice, water and distilled beverage samples were compared with gas chromatography-mass spectrometry (GC-MS). Limits of detection (LODs) in the range 0.04-0.38ngmL(-1) were estimated in real samples after a very simple solid-phase extraction. All the samples were found to contain at least three EDs, in concentrations as high as 334ngmL(-1). Copyright © 2016 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Wandekoken, Flávia G.; Duyck, Christiane B.; Fonseca, Teresa C. O.; Saint'Pierre, Tatiana D.
2016-05-01
High performance liquid chromatography hyphenated by flow injection to inductively coupled plasma mass spectrometry (HPLC-FI-ICP-MS) was used to investigate V linked to porphyrins present in fractions of crude oil. First, the crude oil sample was submitted to fractionation by preparative liquid chromatography with UV detection, at the porphyrin Soret band wavelength (400 nm). The obtained porphyrin fractions were then separated in a 250 mm single column, in the HPLC, and eluted with different mobile phases (methanol or methanol:toluene (80:20; v:v)). The quantification of V-porphyrins in the fractions eluted from HPLC was carried out by online measuring the 51V isotope in the ICP-MS, against vanadyl octaethylporphine standard solutions (VO-OEP), prepared in the same solvent as the mobile phase, and injected post-column directly into the plasma. A 20 μg L- 1 Ge in methanol was used as internal standard for minimizing non-spectral interference, such as short-term variations due to injection. The mathematical treatment of the signal based on Fast Fourier Transform smoothing algorithm was employed to improve the precision. The concentrations of V as V-porphyrins were between 2.7 and 11 mg kg- 1 in the fractions, which were close to the total concentration of V in the porphyrin fractions of the studied crude oil.
Post-elution concentration of (188)Re by an electrochemical method.
Chakravarty, Rubel; Dash, Ashutosh; Pillai, M R A; Venkatesh, Meera
2010-12-01
High specific activity (188)Re required for nuclear medicine is mostly obtained from (188)W/(188)Re generators. As the parent radionuclide (188)W is of low specific activity (<185 GBq/g), a relatively large volume of 0.9% saline is required for the elution of (188)Re. Post-elution concentration is needed in order to increase the radioactive concentration of the eluted (188)Re. An electrochemical procedure to concentrate (188)Re suitable for the preparation of radiopharmaceuticals is developed. (188)Re eluted from an alumina generator could be concentrated approximately 100 fold, and it could be used to label DMSA and HEDP with >98% yield. Copyright 2010 Elsevier Ltd. All rights reserved.
Econazole-releasing porous space maintainers for fungal periprosthetic joint infection.
Tatara, Alexander M; Rozich, Allison J; Kontoyiannis, Panayiotis D; Watson, Emma; Albert, Nathaniel D; Bennett, George N; Mikos, Antonios G
2018-05-11
While antibiotic-eluting polymethylmethacrylate space maintainers have shown efficacy in the treatment of bacterial periprosthetic joint infection and osteomyelitis, antifungal-eluting space maintainers are associated with greater limitations for treatment of fungal musculoskeletal infections including limited elution concentration and duration. In this study, we have designed a porous econazole-eluting space maintainer capable of greater inhibition of fungal growth than traditional solid space maintainers. The eluted econazole demonstrated bioactivity in a concentration-dependent manner against the most common species responsible for fungal periprosthetic joint infection as well as staphylococci. Lastly, these porous space maintainers retain compressive mechanical properties appropriate to maintain space before definitive repair of the joint or bony defect.
Riddell, Nicole; Mullin, Lauren Gayle; van Bavel, Bert; Ericson Jogsten, Ingrid; McAlees, Alan; Brazeau, Allison; Synnott, Scott; Lough, Alan; McCrindle, Robert; Chittim, Brock
2016-11-10
Hexabromocyclododecane (HBCDD) is an additive brominated flame retardant which has been listed in Annex A of the Stockholm Convention for elimination of production and use. It has been reported to persist in the environment and has the potential for enantiomer-specific degradation, accumulation, or both, making enantioselective analyses increasingly important. The six main stereoisomers of technical HBCDD (i.e., the (+) and (-) enantiomers of α-, β-, and γ-HBCDD) were separated and isolated for the first time using enantioselective packed column supercritical fluid chromatography (pSFC) separation methods on a preparative scale. Characterization was completed using published chiral liquid chromatography (LC) methods and elution profiles, as well as X-ray crystallography, and the isolated fractions were definitively identified. Additionally, the resolution of the enantiomers, along with two minor components of the technical product (δ- and ε-HBCDD), was investigated on an analytical scale using both LC and pSFC separation techniques, and changes in elution order were highlighted. Baseline separation of all HBCDD enantiomers was achieved by pSFC on an analytical scale using a cellulose-based column. The described method emphasizes the potential associated with pSFC as a green method of isolating and analyzing environmental contaminants of concern.
Fan, Wenzhe; Zhang, Yu; Carr, Peter W; Rutan, Sarah C; Dumarey, Melanie; Schellinger, Adam P; Pritts, Wayne
2009-09-18
Fourteen judiciously selected reversed phase columns were tested with 18 cationic drug solutes under the isocratic elution conditions advised in the Snyder-Dolan (S-D) hydrophobic subtraction method of column classification. The standard errors (S.E.) of the least squares regressions of logk' vs. logk'(REF) were obtained for a given column against a reference column and used to compare and classify columns based on their selectivity. The results are consistent with those obtained with a study of the 16 test solutes recommended by Snyder and Dolan. To the extent these drugs are representative, these results show that the S-D classification scheme is also generally applicable to pharmaceuticals under isocratic conditions. That is, those columns judged to be similar based on the 16 S-D solutes were similar based on the 18 drugs; furthermore those columns judged to have significantly different selectivities based on the 16 S-D probes appeared to be quite different for the drugs as well. Given that the S-D method has been used to classify more than 400 different types of reversed phases the extension to cationic drugs is a significant finding.
Functional Nanoarchitectures For Enhanced Drug Eluting Stents
NASA Astrophysics Data System (ADS)
Saleh, Yomna E.; Gepreel, Mohamed A.; Allam, Nageh K.
2017-01-01
Different strategies have been investigated to allow for optimum duration and conditions for endothelium healing through the enhancement of coronary stents. In this study, a nanoarchitectured system is proposed as a surface modification for drug eluting stents. Highly oriented nanotubes were vertically grown on the surface of a new Ni-free biocompatible Ti-based alloy, as a potential material for self-expandable stents. The fabricated nanotubes were self-grown from the potential stent substrate, which are also proposed to enhance endothelial proliferation while acting as drug reservoir to hinder Vascular Smooth Muscle Cells (VSMC) proliferation. Two morphologies were synthesized to investigate the effect of structure homogeneity on the intended application. The material was characterized by field-emission scanning electron microscope (FESEM), X-ray diffraction (XRD), Raman spectroscopy, energy dispersive X-ray spectroscopy (EDX), and X-ray photoelectron spectroscopy (XPS). Nanoindentation technique was used to study the mechanical properties of the fabricated material. Cytotoxicity and proliferation studies were performed and compared for the two fabricated nanoarchitectures, versus smooth untextured samples, using in-vitro cultured endothelial cells. Finally, the drug loading capacity was experimentally studied and further supported by computational modeling of the release profile.
Alcaráz, Mirta R; Bortolato, Santiago A; Goicoechea, Héctor C; Olivieri, Alejandro C
2015-03-01
Matrix augmentation is regularly employed in extended multivariate curve resolution-alternating least-squares (MCR-ALS), as applied to analytical calibration based on second- and third-order data. However, this highly useful concept has almost no correspondence in parallel factor analysis (PARAFAC) of third-order data. In the present work, we propose a strategy to process third-order chromatographic data with matrix fluorescence detection, based on an Augmented PARAFAC model. The latter involves decomposition of a three-way data array augmented along the elution time mode with data for the calibration samples and for each of the test samples. A set of excitation-emission fluorescence matrices, measured at different chromatographic elution times for drinking water samples, containing three fluoroquinolones and uncalibrated interferences, were evaluated using this approach. Augmented PARAFAC exploits the second-order advantage, even in the presence of significant changes in chromatographic profiles from run to run. The obtained relative errors of prediction were ca. 10 % for ofloxacin, ciprofloxacin, and danofloxacin, with a significant enhancement in analytical figures of merit in comparison with previous reports. The results are compared with those furnished by MCR-ALS.
Harris, Michael A; Beenken, Karen E; Smeltzer, Mark S; Haggard, Warren O; Jennings, J Amber
2017-07-01
Phosphatidylcholine coatings have been shown to elute antibiotics for several days. A recently developed biofilm inhibitor, cis-2-decenoic acid (C2DA), has been shown to exhibit synergistic activity with several common antibiotics. This study aims to evaluate the effectiveness of C2DA and amikacin dual drug delivery from a phosphatidylcholine coating. (1) What are the in vitro elution profiles of amikacin and C2DA from phosphatidylcholine-coated coupons in incubated phosphate-buffered saline? (2) Does the presence of C2DA in eluate samples lower the amount of amikacin needed for bacterial inhibition in overnight bacterial turbidity assays? (3) Does addition of amikacin and C2DA result in decreased colony-forming units (CFUs) on wire implants and bone when compared with phosphatidylcholine coatings alone in a mouse model of periprosthetic joint infection? Effects of loading concentrations were assessed during 7-day in vitro elution studies for coatings containing all mixtures of 0%, 5%, 15%, and 25% wt of amikacin and C2DA (n = 4) through quantitative high-performance liquid chromatography concentration determination and plotting concentration eluted over time. Antimicrobial activity was assessed by overnight turbidity testing of elution study samples against Staphylococcus aureus or Pseudomonas aeruginosa. In vivo efficacy was assessed using phosphatidylcholine-coated wire implants in a murine (mouse) model of infection (n = 3). Wire implants were coated with phosphatidylcholine containing no antimicrobials, amikacin alone, C2DA alone, or amikacin and C2DA and then inserted into the intramedullary femur of each mouse and inoculated with S aureus. The number of viable bacterial colonies on the implant surface and in the surrounding bone was determined after 1 week with the goal of achieving complete bacterial clearance. Total viable CFU count and proportion of samples achieving complete clearance were compared between groups. Elution samples showed a burst response of amikacin and C2DA for 1 to 2 days with C2DA release continuing at low levels through Day 4. All tested eluate samples inhibited P aeruginosa. Samples from coatings containing 25% amikacin or 15% amikacin and any amount of C2DA were able to inhibit S aureus formation, but all coatings with 5% amikacin or 15% amikacin but no C2DA were not inhibitory. All in vivo treatment groups achieved complete bacterial clearance on the wire implant, and the C2DA alone and amikacin alone coatings cleared all CFUs in bone (pin: phosphatidylcholine only one of three; amikacin three of three, C2DA three of three, amikacin + C2DA three of three, p = 0.04 [Fisher's exact test]; bone: coating only: zero of three; amikacin: three of three; C2DA; three of three; C2DA + amikacin: one of three; p = 0.03 [Fisher's exact test]). Phosphatidylcholine coatings elute antimicrobials in vitro under infinite sink conditions for up to 4 days in phosphate-buffered saline and were able to reduce bacterial colonies in a preliminary in vivo model. Turbidity testing with eluate samples containing varying amounts of C2DA and amikacin agrees with previous studies showing synergy between them. Used as an adjunctive to systemic therapy, C2DA-loaded phosphatidylcholine coatings have potential value as a prophylactic infection prevention measure. Future studies may include different antibiotics, animal studies with larger sample sizes and more controls, and advanced coating delivery methods.
Likić, Vladimir A
2009-01-01
Gas chromatography-mass spectrometry (GC-MS) is a widely used analytical technique for the identification and quantification of trace chemicals in complex mixtures. When complex samples are analyzed by GC-MS it is common to observe co-elution of two or more components, resulting in an overlap of signal peaks observed in the total ion chromatogram. In such situations manual signal analysis is often the most reliable means for the extraction of pure component signals; however, a systematic manual analysis over a number of samples is both tedious and prone to error. In the past 30 years a number of computational approaches were proposed to assist in the process of the extraction of pure signals from co-eluting GC-MS components. This includes empirical methods, comparison with library spectra, eigenvalue analysis, regression and others. However, to date no approach has been recognized as best, nor accepted as standard. This situation hampers general GC-MS capabilities, and in particular has implications for the development of robust, high-throughput GC-MS analytical protocols required in metabolic profiling and biomarker discovery. Here we first discuss the nature of GC-MS data, and then review some of the approaches proposed for the extraction of pure signals from co-eluting components. We summarize and classify different approaches to this problem, and examine why so many approaches proposed in the past have failed to live up to their full promise. Finally, we give some thoughts on the future developments in this field, and suggest that the progress in general computing capabilities attained in the past two decades has opened new horizons for tackling this important problem. PMID:19818154
A simple method to separate red wine nonpolymeric and polymeric phenols by solid-phase extraction.
Pinelo, Manuel; Laurie, V Felipe; Waterhouse, Andrew L
2006-04-19
Simple polyphenols and tannins differ in the way that they contribute to the organoleptic profile of wine and their effects on human health. Very few straightforward techniques to separate red wine nonpolymeric phenols from the polymeric fraction are available in the literature. In general, they are complex, time-consuming, and generate large amounts of waste. In this procedure, the separation of these compounds was achieved using C18 cartridges, three solvents with different elution strengths, and pH adjustments of the experimental matrices. Two full factorial 2(3) experimental designs were performed to find the optimal critical variables and their values, allowing for the maximization of tannin recovery and separation efficiency (SE). Nonpolymeric phenols such as phenolic acids, monomers, and oligomers of flavonol and flavan-3-ols and anthocyanins were removed from the column by means of an aqueous solvent followed by ethyl acetate. The polymeric fraction was then eluted with a combination of methanol/acetone/water. The best results were attained with 1 mL of wine sample, a 10% methanol/water solution (first eluant), ethyl acetate (second eluant), and 66% acetone/water as the polymeric phenols-eluting solution (third eluant), obtaining a SE of ca. 90%. Trials with this method on fruit juices also showed high separation efficiency. Hence, this solid-phase extraction method has been shown to be a simple and efficient alternative for the separation of nonpolymeric phenolic fractions and the polymeric ones, and this method could have important applications to sample purification prior to biological testing due to the nonspecific binding of polymeric phenolics to nearly all enzymes and receptor sites.
All in the Family: Award-Winning New York Band Director Builds a Nurturing Classroom
ERIC Educational Resources Information Center
Olson, Catherine Applefeld
2008-01-01
This article profiles Evonne Michel, a band director at Heim Middle School in Williamsville, New York, who received a Music Education Excellence award from the Buffalo Philharmonic Orchestra and the Erie County Music Educators Association. Evonne Michel was so passionate about her experience in middle school band that she decided, while still in…
Jackson, George W; Willson, Richard
2005-11-01
A "column-format" preparative electrophoresis device which obviates the need for gel extraction or secondary electro-elution steps is described. Separated biomolecules are continuously detected and eluted directly into a minimal volume of free solution for subsequent use. An optical fiber allows the species of interest to be detected just prior to elution from the gel column, and a small collection volume is created by addition of an ion-exchange membrane near the end of the column.
Recovery of monosaccharides from lignocellulosic hydrolysates by ion exclusion chromatography.
Lodi, Gabriele; Pellegrini, Laura Annamaria; Aliverti, Alessandro; Rivas Torres, Beatriz; Bernardi, Marco; Morbidelli, Massimo; Storti, Giuseppe
2017-05-05
The production of sugars from lignocellulosic biomass is the key to a sustainable, renewable chemical industry. Glucose, xylose and other monosaccharides can be easily produced by hydrolyzing cellulose and hemicellulose, the primary polysaccharides in biomass. However, the hydrolysis of biomass generates byproducts that, together with the mineral acid normally added in the hydrolysis step, have to be removed before the downstream conversion processes. In this work, the recovery of monosaccharides from lignocellulosic hydrolysates by means of Ion Exclusion Chromatography (IEC) has been studied. The analyzed process relies on new pretreatment and hydrolysis steps, involving the neutralization of the hydrolysate with sodium hydroxide. The adsorption behavior of the main components involved in the separation has been experimentally investigated. Pulse tests at the high loading encountered in preparative conditions have been performed for a selected group of model components found in the hydrolysates. For all the electrolytes, the retention volume fraction was always between the interparticle porosity and the total column porosity, confirming that ion exclusion was the dominant retention mechanism. On the other hand, sugars eluted before the total column porosity, indicating partial steric exclusion from the resin pores. This observation was then confirmed by size-exclusion experiments with polyethylene glycol standards, from which the distribution coefficient of the studied sugars has been determined. The comparison between the elution profiles of the same sugars in pure form and as a mixture present in the hydrolysate showed differences in both peak shape and retention times. Therefore, an investigation of the influence of the main electrolytes contained in the hydrolysates on sugars adsorption has been performed through the pulse on a plateau method. The electrolytes were found to enhance the sugars retention by promoting their adsorption onto the resin. However, this effect was not sufficient to explain the observed differences, which were effectively explained in terms of viscous fingering, due to the high viscosity differences between the eluent and the sample. A previously developed model for IEC has been updated to take into account all the observed phenomena and applied to simulate the experimental results. The proposed model was in good agreement with the batch-column elution profiles both for the pure components and for the actual hydrolysate, allowing a quantitative description of the separation. Copyright © 2017 Elsevier B.V. All rights reserved.
SOLAR MERIDIONAL FLOW IN THE SHALLOW INTERIOR DURING THE RISING PHASE OF CYCLE 24
DOE Office of Scientific and Technical Information (OSTI.GOV)
Zhao, Junwei; Bogart, R. S.; Kosovichev, A. G.
2014-07-01
Solar subsurface zonal- and meridional-flow profiles during the rising phase of solar cycle 24 are studied using the time-distance helioseismology technique. The faster zonal bands in the torsional-oscillation pattern show strong hemispheric asymmetries and temporal variations in both width and speed. The faster band in the northern hemisphere is located closer to the equator than the band in the southern hemisphere and migrates past the equator when the magnetic activity in the southern hemisphere is reaching maximum. The meridional-flow speed decreases substantially with the increase of magnetic activity, and the flow profile shows two zonal structures in each hemisphere. Themore » residual meridional flow, after subtracting a mean meridional-flow profile, converges toward the activity belts and shows faster and slower bands like the torsional-oscillation pattern. More interestingly, the meridional-flow speed above latitude 30° shows an anti-correlation with the poleward-transporting magnetic flux, slower when the following-polarity flux is transported and faster when the leading-polarity flux is transported. It is expected that this phenomenon slows the process of magnetic cancellation and polarity reversal in high-latitude areas.« less
NASA Astrophysics Data System (ADS)
Mohammed, P. N.; Steffes, P. G.; Kliore, A. J.; Anabtawi, A.; Asmar, S. W.; Barbinis, E.; Goltz, G.; Johnston, D.; Marouf, E. A.
2005-08-01
The results from the first Cassini Radio Science Subsystem(RSS) occultation, which occurred at the Rev 7 periapse, are being used to derive profiles of the atmospheric constituents encountered by the three frequency (S-, X-, and Ka-band) radio link. A computer model has been developed to simulate ray paths and the ray path parameters in the atmosphere of Saturn encountered during occultation (see Mohammed and Steffes, Bull. Amer. Astron. Soc., 36, no. 4, 1107, 2004). This forward model, which can be used on any oblate planet, will be used to determine the refractive defocusing and derive the profiles of phosphine and ammonia using data observed at Ka-band (32 GHz or 9.3 mm), X-band (8.4 GHz or 3.6 cm) and S-band (2.3 GHz or 13 cm). The results of laboratory measurements of the 9 mm opacity of phosphine and ammonia (Mohammed and Steffes, ICARUS 166, 425-435, 2003) and the centimeter wavelength opacity of these constituents measured under simulated conditions for Saturn (see, e.g., Hoffman et. al. ICARUS 152, 172-184, 2001) were incorporated into the forward radio occultation model used in these derivations.
Khattab, Ahmed A; Richardt, Gert; Verin, Vitali; Kelbaek, Henning; Macaya, Carlos; Berland, Jacques; Miquel-Hebert, Karine; Dorange, Cécile; Serruys, Patrick W
2008-03-01
Restenosis is higher among certain subpopulations when subjected to percutaneous coronary interventions even when using drug-eluting stents. The randomised SPIRIT II trial demonstrated the superiority of the XIENCE V Everolimus Eluting Coronary Stent System over the TAXUS Paclitaxel-Eluting Stent System in terms of in-stent late loss at six months among 300 patients treated for de novo native coronary artery lesions. In this post-hoc analysis of SPIRIT II we focused on six-month angiographic outcomes of diabetic patients (n=69), left anterior descending arteries (n=149), long lesions >20 mm (n=43), small vessels <3.0 mm (n=209) and type B2 and C lesions (n=233). In-stent late loss was consistently less among all subgroups when treated by everolimus-eluting stents compared to paclitaxel-eluting stents: diabetics 0.15+/-0.26 mm versus 0.39+/-0.34 mm, p=0.006; LAD 0.12+/-0.23 mm versus 0.44+/-0.37 mm, p<0.001; long lesions 0.13+/-0.26 mm versus 0.43+/-0.46 mm, p=0.070; small vessels 0.17+/-0.28 mm versus 0.37+/-0.39 mm, p<0.001; B2/C lesions 0.12+/-0.31 mm versus 0.36+/-0.36 mm, p<0.001. The everolimus-eluting stent remained superior in terms of in-stent late loss in a variety of higher risk populations for restenosis compared to the paclitaxel-eluting stent. These analyses were consistent with the in-stent late loss results of the overall SPIRIT II trial population.
Regeneration of pilot-scale ion exchange columns for hexavalent chromium removal.
Korak, Julie A; Huggins, Richard; Arias-Paic, Miguel
2017-07-01
Due to stricter regulations, some drinking water utilities must implement additional treatment processes to meet potable water standards for hexavalent chromium (Cr(VI)), such as the California limit of 10 μg/L. Strong base anion exchange is effective for Cr(VI) removal, but efficient resin regeneration and waste minimization are important for operational, economic and environmental considerations. This study compared multiple regeneration methods on pilot-scale columns on the basis of regeneration efficiency, waste production and salt usage. A conventional 1-Stage regeneration using 2 N sodium chloride (NaCl) was compared to 1) a 2-Stage process with 0.2 N NaCl followed by 2 N NaCl and 2) a mixed regenerant solution with 2 N NaCl and 0.2 N sodium bicarbonate. All methods eluted similar cumulative amounts of chromium with 2 N NaCl. The 2-Stage process eluted an additional 20-30% of chromium in the 0.2 N fraction, but total resin capacity is unaffected if this fraction is recycled to the ion exchange headworks. The 2-Stage approach selectively eluted bicarbonate and sulfate with 0.2 N NaCl before regeneration using 2 N NaCl. Regeneration approach impacted the elution efficiency of both uranium and vanadium. Regeneration without co-eluting sulfate and bicarbonate led to incomplete uranium elution and potential formation of insoluble uranium hydroxides that could lead to long-term resin fouling, decreased capacity and render the resin a low-level radioactive solid waste. Partial vanadium elution occurred during regeneration due to co-eluting sulfate suppressing vanadium release. Waste production and salt usage were comparable for the 1- and 2-Stage regeneration processes with similar operational setpoints with respect to chromium or nitrate elution. Published by Elsevier Ltd.
Nickel elution properties of contemporary interatrial shunt closure devices.
Verma, Divya Ratan; Khan, Muhammad F; Tandar, Anwar; Rajasekaran, Namakkal S; Neuharth, Renée; Patel, Amit N; Muhlestein, Joseph B; Badger, Rodney S
2015-02-01
We sought to compare nickel elution properties of contemporary interatrial shunt closure devices in vitro. There are two United States Food and Drug Administration (FDA)-approved devices for percutaneous closure of secundum atrial septal defect: the Amplatzer septal occluder (ASO; St Jude Medical Corporation) and Gore Helex septal occluder (HSO; W.L. Gore & Associates). The new Gore septal occluder (GSO) device is in clinical trials. These are also used off-label for patent foramen ovale closure in highly selected patients. These devices have high nickel content. Nickel allergy is the most common reason for surgical device explantation. Nickel elution properties of contemporary devices remain unknown. We compared nickel elution properties of 4 devices - ASO, GSO, HSO, and sternal wire (SW) - while Dulbecco's phosphate-buffered saline (DPBS) served as control. Three samples of each device were submerged in DPBS. Nickel content was measured at 14 intervals over 90 days. Nickel elution at 24 hours, compared to control (0.005 ± 0.0 mg/L), was significantly higher for ASO (2.98 ± 1.65 mg/L; P=.04) and SW (0.03 ± 0.014 mg/L; P=.03). Nickel levels at 90 days, compared to control (0.005 ± 0.0 mg/L) and adjusting for multiple comparisons, were significantly higher for ASO (19.80 ± 2.30 mg/L; P=.01) and similar for HSO (P=.34), GSO (P=.34), and SW (P=.34). ASO had significantly higher nickel elution compared to HSO, GSO, and SW (P=.01). There is substantial variability in nickel elution; devices with less exposed nickel (HSO and GSO) have minimal elution. The safety of low nickel elution devices in patients with nickel allergy needs to be evaluated in prospective trials.
Sumida, M; Ichimori, H; Johchi, S; Takaoka, A; Yuhki, T; Mori, H; Matsubara, F
1992-01-01
1. Antibacterial activity inducible in the haemolymph of the silkworm, Bombyx mori, by immunization, i.e. by injection of formalin-treated Escherichia coli (E. coli) K-12 during the fifth larval instar and pharate adult development that was reared aseptically on an artificial diet was determined by inhibition zone assay using the same bacterium as a test organism. 2. A peak of antibacterial activity was observed in each development stage; approximately 8 mm in diameter of a clear zone at days 3 or 4 in the fifth larval instar and approximately 5 mm at day 1 in the pharate adults. 3. Acid polyacrylamide gel electrophoresis of immunized haemolymph followed by overlay assay showed that an activity band was associated with two peptide bands that were similar to the cecropin-like peptides A and B that were reported in the silkworm (Morishima et al., 1988, Agri. Biol. Chem. 52, 929-934). Any other activity bands were not observed. No activity band was detectable from the haemolymph of non-immunized insects. 4. Fractionation of antibacterial peptides in immunized haemolymph on a CM-cellulose column resulted in separation of two groups of activity, both in the fifth instar larvae and in the pharate adults with a slight difference in elution conditions. 5. Duration of high antibacterial activity induced by a single immunization was approximately 12 hr in the fifth instar day 3 larvae and 48 hr in the day 2 pharate adults.
Lievens, Hans; Vernieuwe, Hilde; Álvarez-Mozos, Jesús; De Baets, Bernard; Verhoest, Niko E.C.
2009-01-01
In the past decades, many studies on soil moisture retrieval from SAR demonstrated a poor correlation between the top layer soil moisture content and observed backscatter coefficients, which mainly has been attributed to difficulties involved in the parameterization of surface roughness. The present paper describes a theoretical study, performed on synthetical surface profiles, which investigates how errors on roughness parameters are introduced by standard measurement techniques, and how they will propagate through the commonly used Integral Equation Model (IEM) into a corresponding soil moisture retrieval error for some of the currently most used SAR configurations. Key aspects influencing the error on the roughness parameterization and consequently on soil moisture retrieval are: the length of the surface profile, the number of profile measurements, the horizontal and vertical accuracy of profile measurements and the removal of trends along profiles. Moreover, it is found that soil moisture retrieval with C-band configuration generally is less sensitive to inaccuracies in roughness parameterization than retrieval with L-band configuration. PMID:22399956
An efficient routine for infrared radiative transfer in a cloudy atmosphere
NASA Technical Reports Server (NTRS)
Chou, M. D.; Kouvaris, L.
1981-01-01
A FORTRAN program that calculates the atmospheric cooling rate and infrared fluxes for partly cloudy atmospheres is documented. The IR fluxes in the water bands and the 9.6 and 15 micron bands are calculated at 15 levels ranging from 1.39 mb to the surface. The program is generalized to accept any arbitrary atmospheric temperature and humidity profiles and clouds as input and return the cooling rate and fluxes as output. Sample calculations for various atmospheric profiles and cloud situations are demonstrated.
Characterisation of the SOFC material, LaCrO 3, using vibrational spectroscopy
NASA Astrophysics Data System (ADS)
Tompsett, G. A.; Sammes, N. M.
LaCrO 3 is reported to undergo a low to high temperature (HT) phase transition from orthorhombic ( Pnma) to rhombohedral ( R-3 c), at ca. 255 °C. The phases involved in the low temperature phase transition of LaCrO 3 have been determined using Raman spectroscopy at temperatures from -196 to 300 °C. There are nine Raman bands observed from a total of 24 predicted modes, seven of which are assigned from comparison with the Raman profile and relative band positions observed and calculated for the isostructural compound, YMnO 3, as follows: 131(B 2g), 150(B 3g), 174(A g), 252(B 1g), 279(A g), 441(A g) and 590(A g) cm -1. A phase transformation was observed at ca. 260 °C from the change in the Raman profile. The high temperature rhombohedral phase of LaCrO 3 had four bands which are assigned as follows: 58(E g), 161(E g), 288(A 1g) and 434(E g, E g) cm -1, from comparison with the Raman profile and relative band positions observed for the isostructural compound, NdAlO 3. The Fourier transform infrared (FTIR) spectrum of LaCrO 3 showed a total of eight bands discernible at room temperature from 25 predicted modes for the orthorhombic structure. The mode assignments were determined by comparison with the Raman profile and relative band positions observed and calculated for the isostructural compound, SmAlO 3, as follows: 138(B 2u), 166(B 3u), 197(B 1u), 240(B 3u), 266(B 2u), 332(B 2u), 357(B 2u), 381(B 3u), 425(B 3u), 446(B 1u), 471(B 3u), 493(B 3u), 573(B 1u), 606(B 3u) and 670 (B 1u) cm -1.
Rocha, Ariane A; Pinto, Carlos J C; Samuels, Richard I; Alexandre, Daniel; Silva, Carlos P
2014-03-01
The leaffooted bug, Leptoglossus zonatus (Hemiptera: Coreidae) is an emerging pest of several crops around the World and up to now very little is known of its digestive system. In this article, glycoside hydrolase (carbohydrase) activities in the adult midgut cells and in the luminal contents of L. zonatus adult females were studied. The results showed the distribution of digestive carbohydrases in adults of this heteropteran species in the different intestinal compartments. Determination of the spatial distribution of α-glucosidase activity in L. zonatus midgut showed only one major molecular form, which was not equally distributed between soluble and membrane-bound isoforms, being more abundant as a membrane-bound enzyme. The majority of digestive carbohydrases were found in the soluble fractions. Activities against starch, maltose and the synthetic substrate NPαGlu were found to show the highest levels of activity, followed by enzymes active against galactosyl oligosaccharides. Based on ion-exchange chromatography elution profiles and banding patterns in mildly denaturing electrophoresis, both midgut α-amylases and α-galactosidases showed at least two isoforms. The data suggested that the majority of carbohydrases involved in initial digestion were present in the midgut lumen, whereas final digestion of starch and of galactosyl oligosaccharides takes place partially within the lumen and partially at the cell surface. The complex of carbohydrases here described was qualitatively appropriate for the digestion of free oligosaccharides and oligomaltodextrins released by α-amylases acting on maize seed starch granules. © 2014 Wiley Periodicals, Inc.
NASA Astrophysics Data System (ADS)
Sato, T.; Kasaba, Y.; Takahashi, Y.; Murata, I.; Uno, T.; Tokimasa, N.; Sakamoto, M.
2008-12-01
We conducted ground-based observation of Jupiter with the liquid crystal tunable filter (LCTF) and EM-CCD camera in two methane absorption bands (700-757nm, 872-950nm at 3 nm step: total of 47 wavelengths) to derive detailed Jupiter's vertical cloud structure. The 2-meter reflector telescope at Nishi-Harima astronomical observatory in Japan was used for our observation on 26-30 May, 2008. After a series of image processing (composition of high quality images in each wavelength and geometry calibration), we converted observed intensity to absolute reflectivity at each pixel using standard star. As a result, we acquired Jupiter's data cubes with high-spatial resolution (about 1") and narrow band imaging (typically 7nm) in each methane absorption band by superimposing 30 Jupiter's images obtained in short exposure time (50 ms per one image). These data sets enable us to probe different altitudes of Jupiter from 100 mbar down to 1bar level with higher vertical resolution than using convectional interference filters. To interpret observed center-limb profiles, we developed radiative transfer code based on layer adding doubling algorithm to treat multiple scattering of solar light theoretically and extracted information on aerosol altitudes and optical properties using two-cloud model. First, we fit 5 different profiles simultaneously in continuum data (745-757 nm) to retrieve information on optical thickness of haze and single scattering albedo of cloud. Second, we fit 15 different profiles around 727nm methane absorption band and 13 different profiles around 890 nm methane absorption band to retrieve information on the aerosol altitude location and optical thickness of cloud. In this presentation, we present the results of these modeling simulations and discuss the latitudinal variations of Jupiter's vertical cloud structure.
Towards enhanced automated elution systems for waterborne protozoa using megasonic energy.
Horton, B; Katzer, F; Desmulliez, M P Y; Bridle, H L
2018-02-01
Continuous and reliable monitoring of water sources for human consumption is imperative for public health. For protozoa, which cannot be multiplied efficiently in laboratory settings, concentration and recovery steps are key to a successful detection procedure. Recently, the use of megasonic energy was demonstrated to recover Cryptosporidium from commonly used water industry filtration procedures, forming thereby a basis for a simplified and cost effective method of elution of pathogens. In this article, we report the benefits of incorporating megasonic sonication into the current methodologies of Giardia duodenalis elution from an internationally approved filtration and elution system used within the water industry, the Filta-Max®. Megasonic energy assisted elution has many benefits over current methods since a smaller final volume of eluent allows removal of time-consuming centrifugation steps and reduces manual involvement resulting in a potentially more consistent and more cost-effective method. We also show that megasonic sonication of G. duodenalis cysts provides the option of a less damaging elution method compared to the standard Filta-Max® operation, although the elution from filter matrices is not currently fully optimised. A notable decrease in recovery of damaged cysts was observed in megasonic processed samples, potentially increasing the abilities of further genetic identification options upon isolation of the parasite from a filter sample. This work paves the way for the development of a fully automated and more cost-effective elution method of Giardia from water samples. Copyright © 2017 Elsevier B.V. All rights reserved.
Molecular instability induced by aluminum stress in Plantago species.
Correia, Sofia; Matos, Manuela; Ferreira, Vanessa; Martins, Neusa; Gonçalves, Sandra; Romano, Anabela; Pinto-Carnide, Olinda
2014-08-01
Aluminum (Al) is one of the most abundant metals on earth's crust and Al toxicity represents one of the major factors that limit plant growth and productivity in acid soils (with a pH≤5.0). In this study the mutagenic/genotoxic effects of Al were evaluated in roots and leaves of two Plantago, species, Plantago almogravensis and Plantago lagopus, using ISSRs markers. Both species were exposed to 400 μM Al during 7 and 21 days. Ten ISSR primers produced polymorphic bands. In P. almogravensis, a total of 257 and 258 bands in roots and 255 and 265 bands in leaves were produced in the presence and absence of Al, respectively. In P. lagopus were produced 279 and 278 a total bands in roots and 275 and 274 bands in leaves, under the same conditions. The changes in ISSR profiles after Al treatment were considered as gain and/or loss of bands compared with the controls. The results suggest that changes in genomic template stability (GTS) could be detected with ISSR profiles. This molecular marker proved to be a good tool to detect the effects of Al on DNA profiles. It seems that Al did not interfere significantly with DNA integrity in both species but generated less ISSR stability in P. almogravensis than in P. lagopus. The results confirm the tolerance of P. almogravensis and suggest the same behavior of P. lagopus. Although further studies are required for confirmation the Al tolerance behavior of P. lagopus, a potential application for phytoremediation can be also considered due its wide distribution. Copyright © 2014 Elsevier B.V. All rights reserved.
Diffuse interstellar bands in reflection nebulae
NASA Technical Reports Server (NTRS)
Fischer, O.; Henning, Thomas; Pfau, Werner; Stognienko, R.
1994-01-01
A Monte Carlo code for radiation transport calculations is used to compare the profiles of the lambda lambda 5780 and 6613 Angstrom diffuse interstellar bands in the transmitted and the reflected light of a star embedded within an optically thin dust cloud. In addition, the behavior of polarization across the bands were calculated. The wavelength dependent complex indices of refraction across the bands were derived from the embedded cavity model. In view of the existence of different families of diffuse interstellar bands the question of other parameters of influence is addressed in short.
Dual-Band Microstrip Antenna With Reactive Loading
NASA Technical Reports Server (NTRS)
Davidson, Shayla E.
1988-01-01
Effective but bulky coaxial stub replaced. Short-circuited microstrip transmission line serves as reactive loading element for microstrip antenna. Constructed integrally with stripline radiating element, shorted line preserves low microstrip profile and enables tuning of antenna for two-band operation.
Dual-Band Optical Bench for Terahertz Radiometer for Outer Planet Atmospheres (TROPA)
NASA Technical Reports Server (NTRS)
Schlecht, Erich; Jamnejad, Vahraz
2012-01-01
We have developed a wide-band dual frequency spectrometer for use in deep space planetary atmospheric spectroscopy. The instrument uses a dual-band architecture, both to be able to observe spectral lines from a wide range of atmospheric species, and to allow a higher precision retrieval of temperature/pressure/partial pressure and wind profiles. This dual-band approach requires a new design for the optical bench to couple both frequencies into their respective receivers.
Synthetic profiles of polypeptides of human oocytes and normal and abnormal preimplantation embryos.
Capmany, G; Bolton, V N
1999-09-01
There is considerable variation in the rate of development in vitro of individual preimplantation human embryos. The relationship between the rate of development and patterns of polypeptide synthesis in individual embryos was examined using SDS-PAGE and autoradiography. After incubation in [35S]methionine, 19 polypeptide bands were identified that change between fertilization and the morula stage. Although changes in two of the bands occurred in embryos that were developing normally and in ageing oocytes, and are thus independent of fertilization, the changes identified in the remaining 17 bands occurred only after fertilization. In embryos that were developing abnormally, as assessed by delayed cleavage, cleavage arrest or extensive fragmentation, the alteration in polypeptide synthetic profiles increased with increasing abnormality.
NASA Technical Reports Server (NTRS)
Bortner, M. H.; Alyea, F. N.; Grenda, R. N.; Liebling, G. R.; Levy, G. M.
1973-01-01
The feasibility of measuring atmospheric carbon monoxide from a remote platform using the correlation interferometry technique was considered. It has been determined that CO data can be obtained with an accuracy of 10 percent using this technique on the first overtone band of CO at 2.3 mu. That band has been found to be much more suitable than the stronger fundamental band at 4.6 mu. Calculations for both wavelengths are presented which illustrate the effects of atmospheric temperature profiles, inversion layers, ground temperature and emissivity, CO profile, reflectivity, and atmospheric pressure. The applicable radiative transfer theory on which these calculations are based is described together with the principles of the technique.
Electron momentum density and band structure calculations of α- and β-GeTe
NASA Astrophysics Data System (ADS)
Vadkhiya, Laxman; Arora, Gunjan; Rathor, Ashish; Ahuja, B. L.
2011-12-01
We have measured isotropic experimental Compton profile of α-GeTe by employing high energy (662 keV) γ-radiation from a 137Cs isotope. To compare our experiment, we have also computed energy bands, density of states, electron momentum densities and Compton profiles of α- and β-phases of GeTe using the linear combination of atomic orbitals method. The electron momentum density is found to play a major role in understanding the topology of bands in the vicinity of the Fermi level. It is seen that the density functional theory (DFT) with generalised gradient approximation is relatively in better agreement with the experiment than the local density approximation and hybrid Hartree-Fock/DFT.
Lin, Long-Ze; Harnly, James M
2008-11-12
A screening method using LC-DAD-ESI/MS was developed for the identification of common hydroxycinnamoylquinic acids based on direct comparison with standards. A complete standard set for mono-, di-, and tricaffeoylquinic isomers was assembled from commercially available standards, positively identified compounds in common plants (artichokes, asparagus, coffee bean, honeysuckle flowers, sweet potato, and Vernonia amygdalina leaves) and chemically modified standards. Four C18 reversed phase columns were tested using the standardized profiling method (based on LC-DAD-ESI/MS) for 30 phenolic compounds, and their elution order and retention times were evaluated. Using only two columns under standardized LC condition and the collected phenolic compound database, it was possible to separate all of the hydroxycinnamoylquinic acid conjugates and to identify 28 and 18 hydroxycinnamoylquinic acids in arnica flowers (Arnica montana L.) and burdock roots (Arctium lappa L.), respectively. Of these, 22 are reported for the first time.
Pinto, Nuno D S; Uplekar, Shaunak D; Moreira, Antonio R; Rao, Govind; Frey, Douglas D
2017-01-01
Purification processes for monoclonal Immunoglobulin G (IgG) typically employ protein A chromatography as a capture step to remove most of the impurities. One major concern of the post-protein A chromatography processes is the co-elution of some of the host cell proteins (HCPs) with IgG in the capture step. In this work, a novel method for IgG elution in protein A chromatography that reduces the co-elution of HCPs is presented where a two-step pH gradient is self-formed inside a protein A chromatography column. The complexities involved in using an internally produced pH gradient in a protein A chromatography column employing adsorbed buffering species are discussed though equation-based modeling. Under the conditions employed, ELISA assays show a 60% reduction in the HCPs co-eluting with the IgG fraction when using the method as compared to conventional protein A elution without affecting the IgG yield. Evidence is also obtained which indicates that the amount of leached protein A present in free solution in the purified product is reduced by the new method. Biotechnol. Bioeng. 2017;114: 154-162. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.
Separation of mutagenic components in synthetic crudes
DOE Office of Scientific and Technical Information (OSTI.GOV)
Guerin, M. R.; Ho, C. H.; Clark, B. R.
1978-01-01
Mutagenic, basic constituents of a synthetic coal oil and a shale oil were isolated from the crude mixtures. In arriving at an efficient isolation procedure, several liquid chromatographic packing-eluent combinations were tried and the fractions bioassayed to determine the distributions of the mutagenic components. The most effective separation was achieved using a sequential elution scheme with first an alumina-benzene combination followed by a Sephadex LH-20 gel-isopropanol-acetone system. About 75 to 80% of an ether soluble base is eluted with benzene through alumina (activity I). Analysis of this fraction has revealed a wide range of alkyl substituted quinolines and pyridines. Materialmore » remaining on the alumina column was eluted with ethanol, dried and placed on the Sephadex column. Isopropanol (approximately 250 ml) and acetone (approximately 600 ml) were used in that order to elute the material quantitatively. About 12% of the ether-soluble base is eluted with the isopropanol while the rest (approximately 10%) is eluted with the acetone. Additional alkyl pyridine compounds are eluted with isopropanol while the acetone fractions are predominantly multi-ring nitrogen heterocyclic compounds, according to mass spectral analyses. Bioassay data show excellent isolation of the mutagenic activities into the acetone fractions. Negligible activity is found in the sum of the other (90% wt) fractions.« less
NASA Astrophysics Data System (ADS)
Prassanti, R.; Putra, D. S.; Kusuma, B. P.; Nawawi, F. W.
2018-01-01
Monazite is a natural mineral which contains abundant valuable element such as Radioactive Element and Rare Earth Element(REE). In this experiment, it is proven that solution of residual Thorium Sulfate from Monazite mineral process, can be seperated selectively by using extracting method of Solvent Impregnated Resin(SIR), with the elutant solution HNO3. In the earlier process, Thorium solution is conditioned at PH 1 by using H2SO4. Then REE, Thorium and Uranium elements are seperated. This seperation is conducted by using adsorption method by Amberlite XAD-16 Resin, which has been impregnated by Tributhyl Phosphate extractant. It is continued with elution process, which is aimed to obtain Thorium solution of a higher level of concentration. This elution process is conducted by using HNO3, with the elution variables of the lenght of mixing and amount concentration elutant. Based on this experiment, SIR extracting method is able to dissolve Thorium solution until 63,2%grade and a higher level of %grade about 92,40%. It can be concluded that this SIR method can extracted Thorium elements selectively, improve extracting process recovery, and determine optimum stripping condition in the 45th minutes with elutant concentration of 1,0M HNO3.
Kuivila, Kathryn; Crepeau, Kathryn L.
1999-01-01
A laboratory study was used to evaluate the response of select insecticides to toxicity identification evaluation procedures. Fourteen insecticides, one degradation product, and one synergist were spiked into organic-grade water and carried through toxicity identification evaluation procedures. Concentrations of each compound were analyzed by gas chromatography/mass spectrometry. During Phase I, the water sample was pumped through a C-8 solid-phase extraction cartridge and then eluted with methanol. Dimethoate was not removed by the extraction, but remained in the rinsate. In contrast, permethrin was removed by the extraction, but was not recovered by the methanol elution, and 80 percent of the permethrin remained on the cartridge, teflon tubing, and glassware. Chlorpyrifos also was not recovered completely with the methanol elution (only 62 percent was recovered). The other insecticides were extracted by C-8 solid-phase extraction cartridge and recovered by elution with methanol (80 percent or greater). During Phase II, a new spiked water sample was extracted by C-8 solid-phase extraction cartridge and then eluted with varying concentrations of methanol and water into different fractions. Each methanol:water fraction was analyzed for the added compounds. Most of the insecticides eluted in two fractions, with concentrations of 10 percent or greater. The largest number of insecticides eluted in the 75 percent methanol:water fraction.
Christiaens, B; Chiap, P; Rbeida, O; Cello, D; Crommen, J; Hubert, Ph
2003-09-25
A new fully automated method for the quantitative analysis of an antiandrogenic substance, cyproterone acetate (CPA), in plasma samples has been developed using on-line solid-phase extraction (SPE) prior to the determination by reversed-phase liquid chromatography (LC). The automated method was based on the use of a precolumn packed with an internal-surface reversed-phase packing material (LiChrospher RP-4 ADS) for sample clean-up coupled to LC analysis on an octadecyl stationary phase using a column-switching system. A 200-microL volume of plasma sample was injected directly on the precolumn packed with restricted access material using a mixture of water-acetonitrile (90:10, v/v) as washing liquid. The analyte was then eluted in the back-flush mode with the LC mobile phase which consisted of a mixture of phosphate buffer, pH 7.0-acetonitrile (54:46, v/v). The elution profiles of CPA and blank plasma samples on the precolumn and the time needed for analyte transfer from the precolumn to the analytical column were determined. Different compositions of washing liquid and mobile phase were tested to reduce the interference of plasma endogenous components. UV detection was achieved at 280 nm. Finally, the developed method was validated using a new approach, namely the application of the accuracy profile based on the interval confidence at 90% of the total measurement error (bias+standard deviation). The limit of quantification of cyproterone acetate in plasma was determined at 15 ng mL(-1). The validated method should be applicable to the determination of CPA in patients treated by at least 50 mg day(-1).
Mass transfer model of nanoparticle-facilitated contaminant transport in saturated porous media.
Johari, Wan Lutfi Wan; Diamessis, Peter J; Lion, Leonard W
2010-02-01
A one-dimensional model has been evaluated for transport of hydrophobic contaminants, such as polycyclic aromatic hydrocarbon (PAH) compounds, facilitated by synthetic amphiphilic polyurethane (APU) nanoparticles in porous media. APU particles synthesized from poly(ethylene glycol)-modified urethane acrylate (PMUA) precursor chains have been shown to enhance the desorption rate and mobility of phenanthrene (PHEN) in soil. A reversible process governed by attachment and detachment rates was considered to describe the PMUA binding in soil in addition to PMUA transport through advection and dispersion. Ultimately, an irreversible second-order PMUA attachment rate in which the fractional soil saturation capacity with PMUA was a rate control was found to be adequate to describe the retention of PMUA particles. A gamma-distributed site model (GS) was used to describe the spectrum of physical/chemical constraints for PHEN transfer from solid to aqueous phases. Instantaneous equilibrium was assumed for PMUA-PHEN interactions. The coupled model for PMUA and PHEN behavior successfully described the enhanced elution profile of PHEN by PMUA. Sensitivity analysis was performed to analyze the significance of model parameters on model predictions. The adjustable parameter alpha in the gamma-distribution shapes the contaminant desorption distribution profile as well as elution and breakthrough curves. Model simulations show the use of PMUA can be also expected to improve the release rate of PHEN in soils with higher organic carbon content. The percentage removal of PHEN mass over time is shown to be influenced by the concentration of PMUA added and this information can be used to optimize cost and time require to accomplish a desired remediation goal. Copyright 2009 Elsevier Ltd. All rights reserved.
NASA Astrophysics Data System (ADS)
Khodasevich, I. A.; Voitikov, S. V.; Orlovich, V. A.; Kosmyna, M. B.; Shekhovtsov, A. N.
2016-09-01
Unpolarized spontaneous Raman spectra of crystalline double calcium orthovanadates Ca10M(VO4)7 (M = Li, K, Na) in the range 150-1600 cm-1 were measured. Two vibrational bands with full-width at half-maximum (FWHM) of 37-50 cm-1 were found in the regions 150-500 and 700-1000 cm-1. The band shapes were approximated well by deconvolution into Voigt profiles. The band at 700-1000 cm-1 was stronger and deconvoluted into eight Voigt profiles. The frequencies of two strong lines were ~848 and ~862 cm-1 for Ca10Li(VO4)7; ~850 and ~866 cm-1 for Ca10Na(VO4)7; and ~844 and ~866 cm-1 for Ca10K(VO4)7. The Lorentzian width parameters of these lines in the Voigt profiles were ~5 times greater than those of the Gaussian width parameters. The FWHM of the Voigt profiles were ~18-42 cm-1. The two strongest lines had widths of 21-25 cm-1. The vibrational band at 300-500 cm-1 was ~5-6 times weaker than that at 700-1000 cm-1 and was deconvoluted into four lines with widths of 25-40 cm-1. The large FWHM of the Raman lines indicated that the crystal structures were disordered. These crystals could be of interest for Raman conversion of pico- and femtosecond laser pulses because of the intense vibrations with large FWHM in the Raman spectra.
NASA Astrophysics Data System (ADS)
Yankovsky, Valentine A.; Manuilova, Rada O.
2017-11-01
The altitude profiles of ozone concentration are retrieved from measurements of the volume emission rate in the 1.27 μm oxygen band in the TIMED-SABER experiment. In this study we compare the methods of retrieval of daytime [O3] altitude profile in the framework of two models: electronic-vibrational kinetics and a purely electronic kinetics of excited products of ozone and oxygen photolysis. In order to retrieve the [O3] altitude profile from the measurements of the intensity of the O2 band in the region of 1.27 μm correctly, it is necessary to use the photochemical model of the electronic-vibrational kinetics of excited products of ozone and oxygen photolysis in the mesosphere and lower thermosphere.
NASA Astrophysics Data System (ADS)
Wu, Ming-Chya; Forbes, Jeffrey G.; Wang, Kuan
2016-06-01
Nebulin is an about 1 μ m long intrinsically disordered scaffold for the thin filaments of skeletal muscle sarcomere. It is a multifunctional elastic protein that wraps around actin filament, stabilizes thin filaments, and regulates Ca-dependent actomyosin interactions. This study investigates whether the disorder profile of nebulin might encode guidelines for thin and thick filament interactions in the sarcomere of the skeletal muscle. The question was addressed computationally by analyzing the predicted disorder profile of human nebulin (6669 residues, ˜200 actin-binding repeats) by pondr and the periodicity of the A-band stripes (reflecting the locations of myosin-associated proteins) in the electron micrographs of the sarcomere. Using the detrended fluctuation analysis, a scale factor for the A-band stripe image data with respect to the nebulin disorder profile was determined to make the thin and thick filaments aligned to have maximum correlation. The empirical mode decomposition method was then applied to identify hidden periodicities in both the nebulin disorder profile and the rescaled A-band data. The decomposition reveals three characteristic length scales (45 nm, 100 nm, and 200 nm) that are relevant for correlational analysis. The dynamical cross-correlation analyses with moving windows at various sarcomere lengths depict a vernierlike design for both periodicities, thus enabling nebulin to sense position and fine tune sarcomere overlap. This shows that the disorder profile of scaffolding proteins may encode a guideline for cellular architecture.
Cassese, Salvatore; Byrne, Robert A; Ndrepepa, Gjin; Kufner, Sebastian; Wiebe, Jens; Repp, Janika; Schunkert, Heribert; Fusaro, Massimiliano; Kimura, Takeshi; Kastrati, Adnan
2016-02-06
Bioresorbable coronary stents might improve outcomes of patients treated with percutaneous coronary interventions. The everolimus-eluting bioresorbable vascular scaffold is the most studied of these stent platforms; however, its performance versus everolimus-eluting metallic stents remains poorly defined. We aimed to assess the efficacy and safety of everolimus-eluting bioresorbable vascular scaffolds versus everolimus-eluting metallic stents in patients with ischaemic heart disease treated with percutaneous revascularisation. We searched Medline, Embase, the Cochrane Central Register of Controlled Trials (CENTRAL), scientific sessions abstracts, and relevant websites for randomised trials investigating everolimus-eluting bioresorbable vascular scaffolds versus everolimus-eluting metallic stents published or posted between Nov 30, 2006, and Oct 12, 2015. The primary efficacy outcome was target lesion revascularisation and the primary safety outcome was definite or probable stent (scaffold) thrombosis. Secondary outcomes were target lesion failure (the composite of cardiac death, target-vessel myocardial infarction, or ischaemia-driven target lesion revascularisation), myocardial infarction, death, and in-device late lumen loss. We derived odds ratios (ORs) and weighted mean differences with 95% CIs, and calculated the risk estimates for the main outcomes according to a random-effects model. This study is registered with PROSPERO, number CRD42015026374. We included six trials, comprising data for 3738 patients randomised to receive percutaneous coronary intervention with either an everolimus-eluting bioresorbable vascular scaffold (n=2337) or an everolimus-eluting metallic stent (n=1401). Median follow-up was 12 months (IQR 9-12). Patients treated with bioresorbable vascular scaffolds had a similar risk of target lesion revascularisation (OR 0.97 [95% CI 0.66-1.43]; p=0.87), target lesion failure (1.20 [0.90-1.60]; p=0.21), myocardial infarction (1.36 [0.98-1.89]; p=0.06), and death (0.95 [0.45-2.00]; p=0.89) as those treated with metallic stents. Patients treated with a bioresorbable vascular scaffold had a higher risk of definite or probable stent thrombosis than those treated with a metallic stent (OR 1.99 [95% CI 1.00-3.98]; p=0.05), with the highest risk between 1 and 30 days after implantation (3.11 [1.24-7.82]; p=0.02). Lesions treated with a bioresorbable vascular scaffold had greater in-device late lumen loss than those treated with a metallic stent (weighted mean difference 0.08 [95% CI 0.05-0.12]; p<0.0001). Compared with everolimus-eluting metallic stents, everolimus-eluting bioresorbable vascular scaffolds had similar rates of repeat revascularisation at 1 year of follow-up, despite inferior mid-term angiographic performance. However, patients treated with a bioresorbable vascular scaffold had an increased risk of subacute stent thrombosis. Studies with extended follow-up in a larger number of patients are needed to fully assess the long-term advantages of everolimus-eluting bioresorbable vascular scaffolds. None. Copyright © 2016 Elsevier Ltd. All rights reserved.
Zodiacal emission. III - Dust near the asteroid belt
NASA Technical Reports Server (NTRS)
Reach, William T.
1992-01-01
Properties of the zodiacal dust bands are derived from fits to Infrared Astronomical Satellite profiles of the ecliptic. Three observations lead to the conclusion that the dust-band material is spread over a range of heliocentric distances between the asteroid belt and the sun: parallax, color temperature, and wavelength dependence of the band latitudes. The orientations of the midplanes of the bands are found to be typical of asteroids. A model of 'migrating bands', wherein dust is produced near the asteroid belt and spirals into the sun under the influence of Poynting-Robertson drag, is used to explain the range of heliocentric distances of dust-band material.
Tao, Pingyang; Poddar, Saumen; Sun, Zuchen; Hage, David S; Chen, Jianzhong
2018-02-02
Many biological processes involve solute-protein interactions and solute-solute competition for protein binding. One method that has been developed to examine these interactions is zonal elution affinity chromatography. This review discusses the theory and principles of zonal elution affinity chromatography, along with its general applications. Examples of applications that are examined include the use of this method to estimate the relative extent of solute-protein binding, to examine solute-solute competition and displacement from proteins, and to measure the strength of these interactions. It is also shown how zonal elution affinity chromatography can be used in solvent and temperature studies and to characterize the binding sites for solutes on proteins. In addition, several alternative applications of zonal elution affinity chromatography are discussed, which include the analysis of binding by a solute with a soluble binding agent and studies of allosteric effects. Other recent applications that are considered are the combined use of immunoextraction and zonal elution for drug-protein binding studies, and binding studies that are based on immobilized receptors or small targets. Copyright © 2018 Elsevier Inc. All rights reserved.
Kim, Joo Hyoung; Cha, Jung Yul; Hwang, Chung Ju
2012-12-01
This in vitro study was undertaken to evaluate the physical, chemical, and biological properties of commercially available metal orthodontic brackets in South Korea, because national standards for these products are lacking. FOUR BRACKET BRANDS WERE TESTED FOR DIMENSIONAL ACCURACY, (MANUFACTURING ERRORS IN ANGULATION AND TORQUE), CYTOTOXICITY, COMPOSITION, ELUTION, AND CORROSION: Archist (Daeseung Medical), Victory (3M Unitek), Kosaka (Tomy), and Confidence (Shinye Odontology Materials). The tested rackets showed no significant differences in manufacturing errors in angulation, but Confidence brackets showed a significant difference in manufacturing errors in torque. None of the brackets were cytotoxic to mouse fibroblasts. The metal ion components did not show a regular increasing or decreasing trend of elution over time, but the volume of the total eluted metal ions increased: Archist brackets had the maximal Cr elution and Confidence brackets appeared to have the largest volume of total eluted metal ions because of excessive Ni elution. Confidence brackets showed the lowest corrosion resistance during potentiodynamic polarization. The results of this study could potentially be applied in establishing national standards for metal orthodontic brackets and in evaluating commercially available products.
Contrasting Effects of Physical Wear on Elution of Two Antibiotics from Orthopedic Cement
Dodds, S.; Akid, R.; Stephenson, J.; Nichol, T.; Banerjee, R. D.; Stockley, I.; Townsend, R.
2012-01-01
The use of antibiotics as a supplement to bone cement for the purposes of providing a local release of antibiotics is common practice in arthroplasty surgery and the kinetics of elution of the antibiotics in such systems have been investigated previously. However, in these previous studies no account was taken of the potential effects that wear may have on the elution kinetics of the antibiotic. Here, we have modified an existing wear testing rig to allow the simultaneous study of the elution kinetics of bone cement samples containing antibiotics being subjected to immersion only and immersion and conjoint wear. The results show contrasting effects with two commonly used antibiotics. Bone cement containing daptomycin showed no substantial change in antibiotic elution due to wear, while cement containing gentamicin (the most commonly used antibiotic in this application) in contrast demonstrated a substantial reduction in the rate of antibiotic elution when wear was applied. Scanning electron microscopy revealed a possible explanation for these diverse results, due to wear-induced “sealing” of the surface in conjunction with the crystal morphology of the antibiotic. PMID:22155831
Dichroic Filter for Separating W-Band and Ka-Band
NASA Technical Reports Server (NTRS)
Epp, Larry W.; Durden, Stephen L.; Jamnejad, Vahraz; Long, Ezra M.; Sosnowski, John B.; Higuera, Raymond J.; Chen, Jacqueline C.
2012-01-01
The proposed Aerosol/Cloud/Ecosystems (ACEs) mission development would advance cloud profiling radar from that used in CloudSat by adding a 35-GHz (Ka-band) channel to the 94-GHz (W-band) channel used in CloudSat. In order to illuminate a single antenna, and use CloudSat-like quasi-optical transmission lines, a spatial diplexer is needed to add the Ka-band channel. A dichroic filter separates Ka-band from W-band by employing advances in electrical discharge machining (EDM) and mode-matching analysis techniques developed and validated for designing dichroics for the Deep Space Network (DSN), to develop a preliminary design that both met the requirements of frequency separation and mechanical strength. First, a mechanical prototype was built using an approximately 102-micron-diameter EDM process, and tolerances of the hole dimensions, wall thickness, radius, and dichroic filter thickness measured. The prototype validated the manufacturing needed to design a dichroic filter for a higher-frequency usage than previously used in the DSN. The initial design was based on a Ka-band design, but thicker walls are required for mechanical rigidity than one obtains by simply scaling the Ka-band dichroic filter. The resulting trade of hole dimensions for mechanical rigidity (wall thickness) required electrical redesign of the hole dimensions. Updates to existing codes in the linear solver decreased the analysis time using mode-matching, enabling the electrical design to be realized quickly. This work is applicable to missions and instruments that seek to extend W-band cloud profiling measurements to other frequencies. By demonstrating a dichroic filter that passes W-band, but reflects a lower frequency, this opens up the development of instruments that both compare to and enhance CloudSat.
Evaluation of three methods for the concentration of poliovirus from oysters.
Bouchriti, N; Goyal, S M
1992-10-01
Three methods for the concentration of poliovirus from oyster homogenates were compared. The adsorption-elution-precipitation method gave the lowest average virus recovery (24.1%), while the beef extract elution-acid precipitation method and the non-fat dry milk elution-acid precipitation methods gave recoveries of 47.2% and 39.6%, respectively. Although the overall recovery rates with these methods were lower than those reported in previous studies, recoveries of 40-47% obtained with the elution-precipitation methods used in the present study are considered to be above average in terms of recovery efficiency.
Palmerini, Tullio; Biondi-Zoccai, Giuseppe; Della Riva, Diego; Stettler, Christoph; Sangiorgi, Diego; D'Ascenzo, Fabrizio; Kimura, Takeshi; Briguori, Carlo; Sabatè, Manel; Kim, Hyo-Soo; De Waha, Antoinette; Kedhi, Elvin; Smits, Pieter C; Kaiser, Christoph; Sardella, Gennaro; Marullo, Antonino; Kirtane, Ajay J; Leon, Martin B; Stone, Gregg W
2012-04-14
The relative safety of drug-eluting stents and bare-metal stents, especially with respect to stent thrombosis, continues to be debated. In view of the overall low frequency of stent thrombosis, large sample sizes are needed to accurately estimate treatment differences between stents. We compared the risk of thrombosis between bare-metal and drug-eluting stents. For this network meta-analysis, randomised controlled trials comparing different drug-eluting stents or drug-eluting with bare-metal stents currently approved in the USA were identified through Medline, Embase, Cochrane databases, and proceedings of international meetings. Information about study design, inclusion and exclusion criteria, sample characteristics, and clinical outcomes was extracted. 49 trials including 50,844 patients randomly assigned to treatment groups were analysed. 1-year definite stent thrombosis was significantly lower with cobalt-chromium everolimus eluting stents (CoCr-EES) than with bare-metal stents (odds ratio [OR] 0·23, 95% CI 0·13-0·41). The significant difference in stent thrombosis between CoCr-EES and bare-metal stents was evident as early as 30 days (OR 0·21, 95% CI 0·11-0·42) and was also significant between 31 days and 1 year (OR 0·27, 95% CI 0·08-0·74). CoCr-EES were also associated with significantly lower rates of 1-year definite stent thrombosis compared with paclitaxel-eluting stents (OR 0·28, 95% CI 0·16-0·48), permanent polymer-based sirolimus-eluting stents (OR 0·41, 95% CI 0·24-0·70), phosphorylcholine-based zotarolimus-eluting stents (OR 0·21, 95% CI 0·10-0·44), and Resolute zotarolimus-eluting stents (OR 0·14, 95% CI 0·03-0·47). At 2-year follow-up, CoCr-EES were still associated with significantly lower rates of definite stent thrombosis than were bare-metal (OR 0·35, 95% CI 0·17-0·69) and paclitaxel-eluting stents (OR 0·34, 95% CI 0·19-0·62). No other drug-eluting stent had lower definite thrombosis rates compared with bare-metal stents at 2-year follow-up. In randomised studies completed to date, CoCr-EES has the lowest rate of stent thrombosis within 2 years of implantation. The finding that CoCr-EES also reduced stent thrombosis compared with bare-metal stents, if confirmed in future randomised trials, represents a paradigm shift. The Cardiovascular Research Foundation. Copyright © 2012 Elsevier Ltd. All rights reserved.
Paclitaxel Drug-Eluting Stents in Peripheral Arterial Disease: A Health Technology Assessment
2015-01-01
Background Peripheral arterial disease is a condition in which atherosclerotic plaques partially or completely block blood flow to the legs. Although percutaneous transluminal angioplasty and metallic stenting have high immediate success rates in treating peripheral arterial disease, long-term patency and restenosis rates in long and complex lesions remain unsatisfactory. Objective The objective of this analysis was to evaluate the clinical effectiveness, safety, cost-effectiveness and budget impact of Zilver paclitaxel self-expanding drug-eluting stents for the treatment of de novo or restenotic lesions in above-the-knee peripheral arterial disease. Data Sources Literature searches were performed using Ovid MEDLINE, Ovid MEDLINE In-Process and Other Non-Indexed Citations, Ovid Embase, EBSCO Cumulative Index to Nursing & Allied Health Literature (CINAHL), and EBM Reviews. For the economic review, a search filter was applied to limit search results to economics-related literature. Data sources for the budget impact analysis included expert opinion, published literature, and Ontario administrative data. Review Methods Systematic reviews, meta-analyses, randomized controlled trials, and observational studies were included in the clinical effectiveness review, and full economic evaluations were included in the economic literature review. Studies were included if they examined the effect of Zilver paclitaxel drug-eluting stents in de novo or restenotic lesions in above-the-knee arteries. For the budget impact analysis, 3 scenarios were constructed based on different assumptions. Results One randomized controlled trial reported a significantly higher patency rate with Zilver paclitaxel drug-eluting stents for lesions ≤ 14 cm than with angioplasty or bare metal stents. One observational study showed no difference in patency rates between Zilver paclitaxel drug-eluting stents and paclitaxel drug-coated balloons. Zilver paclitaxel drug-eluting stents were associated with a significantly higher event-free survival rate than angioplasty, but the event-free survival rate was similar for Zilver paclitaxel drug-eluting stents and paclitaxel drug-coated balloons. No economic evaluations compared Zilver paclitaxel drug-eluting stents with bare metal stents or angioplasty for peripheral arterial disease. A budget impact analysis showed that the cost savings associated with funding of Zilver paclitaxel drug-eluting stents would be $470,000 to $640,000 per year, assuming that the use of the Zilver paclitaxel drug-eluting stent was associated with a lower risk of subsequent revascularization. Conclusions Based on evidence of low to moderate quality, Zilver paclitaxel drug-eluting stents were associated with a higher patency rate than angioplasty or bare metal stents, and with fewer adverse events than angioplasty. The effectiveness and safety of Zilver paclitaxel drug-eluting stents and paclitaxel drug-coated balloons were similar. PMID:26719778
Pokrovskiy, Oleg I; Ustinovich, Konstantin B; Usovich, Oleg I; Parenago, Olga O; Lunin, Valeriy V; Ovchinnikov, Denis V; Kosyakov, Dmitry S
2017-01-06
A case of elution order inversion caused by cosolvent percentage change in supercritical fluid chromatography was observed and investigated in some detail. Z- and E-isomers of phenylisobutylketone oxime experience an elution order reversal on most columns if the mobile phase consists of CO 2 and alcohol. At lower percentages of alcohol Z-oxime is retained less, somewhere at 2-5% coelution occurs and at larger cosolvent volume elution order reverses - Z-oxime is eluted later than E-oxime. We suppose inversion with CO 2 -ROH phases happens due to a shift in balance between two main interactions governing retention. At low ROH percentages stationary phase surface is only slightly covered by ROH molecules so oximes primarily interact with adsorption sites via hydrogen bond formation. Due to intramolecular sterical hindrance Z-oxime is less able to form hydrogen bonds and consequently is eluted first. At higher percentages alcohols occupy most of strong hydrogen bonding sites on silica surface thus leaving non-specific electrostatic interactions predominantly responsible for Z/E selectivity. Z-oxime has a much larger dipole moment than E-oxime and at these conditions it is eluted later. Additional experimental data with CO 2 -CH 3 CN, hexane-iPrOH and CHF 3 -ROH mobile phases supporting this explanation are presented. Copyright © 2016 Elsevier B.V. All rights reserved.
Modeling of salt and pH gradient elution in ion-exchange chromatography.
Schmidt, Michael; Hafner, Mathias; Frech, Christian
2014-01-01
The separation of proteins by internally and externally generated pH gradients in chromatofocusing on ion-exchange columns is a well-established analytical method with a large number of applications. In this work, a stoichiometric displacement model was used to describe the retention behavior of lysozyme on SP Sepharose FF and a monoclonal antibody on Fractogel SO3 (S) in linear salt and pH gradient elution. The pH dependence of the binding charge B in the linear gradient elution model is introduced using a protein net charge model, while the pH dependence of the equilibrium constant is based on a thermodynamic approach. The model parameter and pH dependences are calculated from linear salt gradient elutions at different pH values as well as from linear pH gradient elutions at different fixed salt concentrations. The application of the model for the well-characterized protein lysozyme resulted in almost identical model parameters based on either linear salt or pH gradient elution data. For the antibody, only the approach based on linear pH gradients is feasible because of the limited pH range useful for salt gradient elution. The application of the model for the separation of an acid variant of the antibody from the major monomeric form is discussed. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Takimura, Celso K; Galon, Micheli Z; Gutierrez, Paulo S; Sojitra, Prakash; Vyas, Ashwin; Doshi, Manish; Lemos, Pedro A
2015-04-01
Permanent polymers in first generation drug-eluting stent (DES) have been imputed to be a possible cause of persistent inflammation, remodeling, malapposition and late stent thrombosis. We aim to describe the in vivo experimental result of a new polymer-free DES eluting sirolimus from stent-plus-balloon (Focus np stent, Envision Scientific) compared with a bare-metal stent (BMS) (Amazonia CroCo, Minvasys) and with a biolimus A9 eluting stent (Biomatrix, Biosensors). In 10 juvenile pigs, 23 coronary stents were implanted in the coronary arteries (8 Amazonia CroCo, 8 Focus np, and 7 Biomatrix). At 28-day follow-up, optical coherence tomography (OCT) and histology were used to evaluate neointimal hyperplasia and healing response. According to OCT analysis, Focus np stents had a greater lumen area and less neointimal hyperplasia response than BMS and Biomatrix had. Histomorphometry results showed less neointimal hyperplasia in Focus np than in BMS. Histology showed a higher fibrin deposition in Biomatrix stent compared to Focus np and BMS. The new polymer-free DES with sirolimus eluted from stent-plus-balloon demonstrated safety and reduced neointimal proliferation compared with the BMS and Biomatrix stents at 28-day follow-up in this porcine coronary model. This new polymer-free DES is promising and warrants further clinical studies.
Elution of lead from lead zirconate titanate ceramics to acid rain
NASA Astrophysics Data System (ADS)
Tsurumi, Takaaki; Takezawa, Shuhei; Hoshina, Takuya; Takeda, Hiroaki
2017-10-01
The amount of lead that eluted from lead zirconate titanate (PZT) ceramics to artificial acid rain was evaluated. Four kinds of PZT ceramics, namely, pure PZT at MPB composition, CuO-added PZT, PZT with 10 mol % substitution of Ba for Pb, and CuO-added PZT with 10 mol % substitution of Ba for Pb, were used as samples of the elution test. These PZT ceramics of 8 mm2 and 1.1-1.2 mm thickness were suspended in 300 ml of H2SO4 solution of pH 4.0. The concentration of lead eluted from PZT was in the range from 0.2 to 0.8 ppm. It was found that both liquid phase formation by the addition of CuO and the substitution of Ba for Pb were effective to reduce the amount of lead that eluted. By fitting the leaching out curve with a classical equation, a master curve assuming no sampling effect was obtained. The lead concentration evaluated from the amount of lead that eluted from a commercial PZT plate to H2SO4 solution of pH 5.3 was almost the same as the limit in city water. It is concluded that PZT is not harmful to health and the environment and the amount of lead that eluted from PZT can be controlled by modifying PZT composition.
NASA Astrophysics Data System (ADS)
McElroy, Kenneth L., Jr.
1992-12-01
A method is presented for the determination of neutral gas densities in the ionosphere from rocket-borne measurements of UV atmospheric emissions. Computer models were used to calculate an initial guess for the neutral atmosphere. Using this neutral atmosphere, intensity profiles for the N2 (0,5) Vegard-Kaplan band, the N2 Lyman-Birge-Hopfield band system, and the OI2972 A line were calculated and compared with the March 1990 NPS MUSTANG data. The neutral atmospheric model was modified and the intensity profiles recalculated until a fit with the data was obtained. The neutral atmosphere corresponding to the intensity profile that fit the data was assumed to be the atmospheric composition prevailing at the time of the observation. The ion densities were then calculated from the neutral atmosphere using a photochemical model. The electron density profile calculated by this model was compared with the electron density profile measured by the U.S. Air Force Geophysics Laboratory at a nearby site.
Characteristics of SnO2-based 68Ge/68Ga generator and aspects of radiolabelling DOTA-peptides.
de Blois, Erik; Sze Chan, Ho; Naidoo, Clive; Prince, Deidre; Krenning, Eric P; Breeman, Wouter A P
2011-02-01
PET scintigraphy with (68)Ga-labelled analogs is of increasing interest in Nuclear Medicine and performed all over the world. Here we report the characteristics of the eluate of SnO(2)-based (68)Ge/(68)Ga generators prepared by iThemba LABS (Somerset West, South Africa). Three purification and concentration techniques of the eluate for labelling DOTA-TATE and concordant SPE purifications were investigated. Characteristics of 4 SnO(2)-based generators (range 0.4-1 GBq (68)Ga in the eluate) and several concentration techniques of the eluate (HCl) were evaluated. The elution profiles of SnO(2)-based (68)Ge/(68)Ga generators were monitored, while [HCl] of the eluens was varied from 0.3-1.0 M. Metal ions and sterility of the eluate were determined by ICP. Fractionated elution and concentration of the (68)Ga eluate were performed using anion and cation exchange. Concentrated (68)Ga eluate, using all three concentration techniques, was used for labelling of DOTA-TATE. (68)Ga-DOTA-TATE-containing solution was purified and RNP increased by SPE, therefore also 11 commercially available SPE columns were investigated. The amount of elutable (68)Ga activity varies when the concentration of the eluens, HCl, was varied, while (68)Ge activity remains virtually constant. SnO(2)-based (68)Ge/(68)Ga generator elutes at 0.6 M HCl >100% of the (68)Ga activity at calibration time and ±75% after 300 days. Eluate at discharge was sterile and Endotoxins were <0.5 EU/mL, RNP was always <0.01%. Metal ions in the eluate were <10 ppm (in total). Highest desorption for anion purification was obtained with the 30 mg Oasis WAX column (>80%). Highest desorption for cation purification was obtained using a solution containing 90% acetone at increasing molarity of HCl, resulted in a (68)Ga desorption of 68±8%. With all (68)Ge/(68)Ga generators and for all 3 purification methods a SA up to 50 MBq/nmol with >95% incorporation (ITLC) and RCP (radiochemical purity) by HPLC ±90% could be achieved. Purification and concentration of the eluate with anion exchange has the benefit of more elutable (68)Ga with 1 M HCl as eluens. The additional washing step of the anion column with NaCl and ethanol, resulted in a lower and less variable [H(+)] in the eluate, and, as a result the pH in the reaction vial is better controlled, more constant, and less addition of buffer is required and concordant smaller reaction volumes. Desorption of (68)Ga-DOTA-TATE of SPE columns varied, highest desorption was obtained with Baker C(18) 100 mg (84%). Purification of (68)Ga-DOTA-TATE by SPE resulted in an RNP of <10(-4)%. Eluate of SnO(2)-based (68)Ge/(68)Ga generator, either by fractionated elution as by ion exchange can be used for labelling DOTA-peptides with (68)Ga at a SA of 50 MBq/nmol at >95% incorporation and a RCP of ±90%. SPE columns are very effective to increase RNP. Copyright © 2010 Elsevier Ltd. All rights reserved.
Golo, Patrícia Silva; Dos Santos, Alessa Siqueira de Oliveira; Monteiro, Caio Marcio Oliveira; Perinotto, Wendell Marcelo de Souza; Quinelato, Simone; Camargo, Mariana Guedes; de Sá, Fillipe Araujo; Angelo, Isabele da Costa; Martins, Marta Fonseca; Prata, Marcia Cristina de Azevedo; Bittencourt, Vânia Rita Elias Pinheiro
2016-09-01
In the present study, lab-on-a-chip electrophoresis (LoaC) was suggested as an alternative method to the conventional polyacrylamide gel electrophoresis under denaturing conditions (SDS-PAGE) to analyze raw cell-free tick hemolymph. Rhipicephalus microplus females were exposed to the entomopathogenic fungus Metarhizium anisopliae senso latu IBCB 116 strain and/or to the entomopathogenic nematode Heterorhabditis indica LPP1 strain. Hemolymph from not exposed or exposed ticks was collected 16 and 24 h after exposure and analyze by SDS-PAGE or LoaC. SDS-PAGE yielded 15 bands and LoaC electrophoresis 17 bands. Despite the differences in the number of bands, when the hemolymph protein profiles of exposed or unexposed ticks were compared in the same method, no suppressing or additional bands were detected among the treatments regardless the method (i.e., SDS-PAGE or chip electrophoresis using the Protein 230 Kit®). The potential of LoaC electrophoresis to detect protein bands from tick hemolymph was considered more efficient in comparison to the detection obtained using the traditional SDS-PAGE method, especially when it comes to protein subunits heavier than 100 KDa. LoaC electrophoresis provided a very good reproducibility, and is much faster than the conventional SDS-PAGE method, which requires several hours for one analysis. Despite both methods can be used to analyze tick hemolymph composition, LoaC was considered more suitable for cell-free hemolymph protein separation and detection. LoaC hemolymph band percent data reported changes in key proteins (i.e., HeLp and vitellogenin) exceptionally important for tick embryogenesis. This study reported, for the first time, tick hemolymph protein profile using LoaC.
Application of acidic elution to virus concentration using electropositive filters.
Haramoto, Eiji; Katayama, Hiroyuki
2013-03-01
The effect of the type and pH of an elution solution on the recovery of poliovirus from water by a virus concentration method using an electropositive filter was evaluated. The experimental results obtained indicated the potential usefulness of H2SO4 (pH 1.5-3.5) as a novel solution for virus elution.
Qualitative Beam Profiling of Light Curing Units for Resin Based Composites.
Haenel, Thomas; Hausnerová, Berenika; Steinhaus, Johannes; Moeginger, Ing Bernhard
2016-12-01
This study investigates two technically simple methods to determine the irradiance distribution of light curing units that governs the performance of a visible-light curing resin-based composites. Insufficient light irradiation leads to under-cured composites with poor mechanical properties and elution of residual monomers. The unknown irradiance distribution and its effect on the final restoration are the main critical issues requiring highly sophisticated experimental equipment. The study shows that irradiance distributions of LCUs can easily be determined qualitatively with generally available equipment. This significantly helps dentists in practices to be informed about the homogeneity of the curing lights. Copyright© 2016 Dennis Barber Ltd.
Planer, David; Smits, Pieter C; Kereiakes, Dean J; Kedhi, Elvin; Fahy, Martin; Xu, Ke; Serruys, Patrick W; Stone, Gregg W
2011-10-01
This study sought to compare the clinical outcomes of everolimus-eluting stents (EES) versus paclitaxel-eluting stents (PES) in patients with acute coronary syndromes (ACS) and stable coronary artery disease (CAD). Although randomized trials have shown superiority of EES to PES, the safety and efficacy of EES in ACS is unknown. We performed a patient-level pooled analysis from the prospective, randomized SPIRIT (Clinical Evaluation of the XIENCE V Everolimus Eluting Coronary Stent System) II, III, IV, and COMPARE (A Trial of Everolimus-Eluting Stents and Paclitaxel-Eluting Stents for Coronary Revascularization in Daily Practice) trials in which 2,381 patients with ACS and 4,404 patients with stable CAD were randomized to EES or to PES. Kaplan-Meier estimates of death, myocardial infarction (MI), ischemia-driven target lesion revascularization, and stent thrombosis were assessed at 2 years and stratified by clinical presentation (ACS vs. stable CAD). At 2 years, patients with ACS compared with stable CAD had higher rates of death (3.2% vs. 2.4%, hazard ratio [HR]: 1.37 [95% confidence interval (CI): 1.02 to 1.85], p = 0.04) and MI (4.9% vs. 3.4%, HR: 1.45 [95% CI: 1.14 to 1.85], p = 0.02). In patients with ACS, EES versus PES reduced the rate of death or MI (6.6% vs. 9.3%, HR: 0.70 [95% CI: 0.52 to 0.94], p = 0.02), stent thrombosis (0.7% vs. 2.9%, HR: 0.25 [95% CI: 0.12 to 0.52], p = 0.0002), and ischemia-driven target lesion revascularization (4.7% vs. 6.2%, HR: 0.69 [95% CI: 0.48 to 0.99], p = 0.04). In patients with stable CAD, EES reduced the rate of death or MI (4.5% vs. 7.1%, HR: 0.62 [95% CI: 0.48 to 0.80], p = 0.0002), stent thrombosis (0.7% vs. 1.8%, HR: 0.34 [95% CI: 0.19 to 0.62], p = 0.0002), and ischemia-driven target lesion revascularization (3.9% vs. 6.9%, HR: 0.55 [95% CI: 0.42 to 0.73], p < 0.0001). Treatment with EES versus PES provides enhanced safety and efficacy regardless of the acuity of the clinical syndrome being treated and appears to mitigate the increased risk of stent thrombosis associated with ACS. (A Clinical Evaluation of the XIENCE V Everolimus Eluting Coronary Stent System in the Treatment of Patients With de Novo Native Coronary Artery Lesions [SPIRIT II]; NCT00180310; SPIRIT III: A Clinical Evaluation of the Investigational Device XIENCE V Everolimus Eluting Coronary Stent System [EECSS] in the Treatment of Subjects With de Novo Native Coronary Artery Lesions [SPIRIT III]; NCT00180479; SPIRIT IV Clinical Trial: Clinical Evaluation of the XIENCE V Everolimus Eluting Coronary Stent System in the Treatment of Subjects With de Novo Native Coronary Artery Lesions [SPIRIT IV]; NCT00307047; A Trial of Everolimus-Eluting Stents and Paclitaxel-Eluting Stents for Coronary Revascularization in Daily Practice: the COMPARE Trial [COMPARE]; NCT01016041). Copyright © 2011 American College of Cardiology Foundation. Published by Elsevier Inc. All rights reserved.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Walsh, D. A., E-mail: david.walsh@stfc.ac.uk; Snedden, E. W.; Jamison, S. P.
The time-resolved detection of ultrashort pulsed THz-band electric field temporal profiles without an ultrashort laser probe is demonstrated. A non-linear interaction between a narrow-bandwidth optical probe and the THz pulse transposes the THz spectral intensity and phase information to the optical region, thereby generating an optical pulse whose temporal electric field envelope replicates the temporal profile of the real THz electric field. This optical envelope is characterised via an autocorrelation based FROG (frequency resolved optical gating) measurement, hence revealing the THz temporal profile. The combination of a narrow-bandwidth, long duration, optical probe, and self-referenced FROG makes the technique inherently immunemore » to timing jitter between the optical probe and THz pulse and may find particular application where the THz field is not initially generated via ultrashort laser methods, such as the measurement of longitudinal electron bunch profiles in particle accelerators.« less
Retrieval of the Nitrous Oxide Profiles using the AIRS Data in China
NASA Astrophysics Data System (ADS)
Chen, L.; Ma, P.; Tao, J.; Li, X.; Zhang, Y.; Wang, Z.; Li, S.; Xiong, X.
2014-12-01
As an important greenhouse gas and ozone-depleting substance, the 100-year global warming potential of Nitrous Oxide (N2O) is almost 300 times higher than that of carbon dioxide. However, there are still large uncertainties about the quantitative N2O emission and its feedback to climate change due to the coarse ground-based network. This approach attempts to retrieve the N2O profiles from the Atmospheric InfraRed Sounder (AIRS) data. First, the sensitivity of atmospheric temperature and humidity profiles and surface parameters between two spectral absorption bands were simulated by using the radiative transfer model. Second, the eigenvector regression algorithm is used to construct a priori state. Third, an optimal estimate method was developed based on the band selection of N2O. Finally, we compared our retrieved AIRS profiles with HIPPO data, and analyzed the seasonal and annual N2O distribution in China from 2004 to 2013.
Differential absorption lidar measurements of atmospheric temperature and pressure profiles
NASA Technical Reports Server (NTRS)
Korb, C. L.
1981-01-01
The theory and methodology of using differential absorption lidar techniques for the remote measurement of atmospheric pressure profiles, surface pressure, and temperature profiles from ground, air, and space-based platforms are presented. Pressure measurements are effected by means of high resolution measurement of absorption at the edges of the oxygen A band lines where absorption is pressure dependent due to collisional line broadening. Temperature is assessed using measurements of the absorption at the center of the oxygen A band line originating from a quantum state with high ground state energy. The population of the state is temperature dependent, allowing determination of the temperature through the Boltzmann term. The results of simulations of the techniques using Voigt profile and variational analysis are reported for ground-based, airborne, and Shuttle-based systems. Accuracies in the 0.5-1.0 K and 0.1-0.3% range are projected.
Partial Purification of a Megadalton DNA Replication Complex by Free Flow Electrophoresis.
Li, Caroline M; Miao, Yunan; Lingeman, Robert G; Hickey, Robert J; Malkas, Linda H
2016-01-01
We describe a gentle and rapid method to purify the intact multiprotein DNA replication complex using free flow electrophoresis (FFE). In particular, we applied FFE to purify the human cell DNA synthesome, which is a multiprotein complex that is fully competent to carry-out all phases of the DNA replication process in vitro using a plasmid containing the simian virus 40 (SV40) origin of DNA replication and the viral large tumor antigen (T-antigen) protein. The isolated native DNA synthesome can be of use in studying the mechanism by which mammalian DNA replication is carried-out and how anti-cancer drugs disrupt the DNA replication or repair process. Partially purified extracts from HeLa cells were fractionated in a native, liquid based separation by FFE. Dot blot analysis showed co-elution of many proteins identified as part of the DNA synthesome, including proliferating cell nuclear antigen (PCNA), DNA topoisomerase I (topo I), DNA polymerase δ (Pol δ), DNA polymerase ɛ (Pol ɛ), replication protein A (RPA) and replication factor C (RFC). Previously identified DNA synthesome proteins co-eluted with T-antigen dependent and SV40 origin-specific DNA polymerase activity at the same FFE fractions. Native gels show a multiprotein PCNA containing complex migrating with an apparent relative mobility in the megadalton range. When PCNA containing bands were excised from the native gel, mass spectrometric sequencing analysis identified 23 known DNA synthesome associated proteins or protein subunits.
Zhang, Zhenbin; Yan, Xiaojing; Sun, Liangliang; Zhu, Guijie; Dovichi, Norman J
2015-04-21
A detachable sulfonate-silica hybrid strong cation-exchange monolith was synthesized in a fused silica capillary, and used for solid phase extraction with online pH gradient elution during capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) proteomic analysis. Tryptic digests were prepared in 50 mM formic acid and loaded onto the strong cation-exchange monolith. Fractions were eluted using a series of buffers with lower concentration but higher pH values than the 50 mM formic acid background electrolyte. This combination of elution and background electrolytes results in both sample stacking and formation of a dynamic pH junction and allows use of relatively large elution buffer volumes while maintaining reasonable peak efficiency and resolution. A series of five pH bumps were applied to elute E. coli tryptic peptides from the monolith, followed by analysis using CZE coupled to an LTQ-Orbitrap Velos mass spectrometer; 799 protein groups and 3381 peptides were identified from 50 ng of the digest in a 2.5 h analysis, which approaches the identification rate for this organism that was obtained with an Orbitrap Fusion. We attribute the improved numbers of peptide and protein identifications to the efficient fractionation by the online pH gradient elution, which decreased the complexity of the sample in each elution step and improved the signal intensity of low abundance peptides. We also performed a comparative analysis using a nanoACQUITY UltraPerformance LCH system. Similar numbers of protein and peptide identifications were produced by the two methods. Protein identifications showed significant overlap between the two methods, whereas peptide identifications were complementary.
Multiplexed electrokinetic sample fractionation, preconcentration and elution for proteomics.
Hua, Yujuan; Jemere, Abebaw B; Dragoljic, Jelena; Harrison, D Jed
2013-07-07
Both 6 and 8-channel integrated microfluidic sample pretreatment devices capable of performing "in space" sample fractionation, collection, preconcentration and elution of captured analytes via sheath flow assisted electrokinetic pumping are described. Coatings and monolithic polymer beds were developed for the glass devices to provide cationic surface charge and anodal electroosmotic flow for delivery to an electrospray emitter tip. A mixed cationic ([2-(methacryloyloxy)ethyl] trimethylammonium chloride) (META) and hydrophobic butyl methacrylate-based monolithic porous polymer, photopolymerized in the 6- or 8-fractionation channels, was used to capture and preconcentrate samples. A 0.45 wt% META loaded bed generated comparable anodic electroosmotic flow to the cationic polymer PolyE-323 coated channel segments in the device. The balanced electroosmotic flow allowed stable electrokinetic sheath flow to prevent cross contamination of separated protein fractions, while reducing protein/peptide adsorption on the channel walls. Sequential elution of analytes trapped in the SPE beds revealed that the monolithic columns could be efficiently used to provide sheath flow during elution of analytes, as demonstrated for neutral carboxy SNARF (residual signal, 0.08% RSD, n = 40) and charged fluorescein (residual signal, 2.5% n = 40). Elution from monolithic columns showed reproducible performance with peak area reproducibility of ~8% (n = 6 columns) in a single sequential elution and the run-to-run reproducibility was 2.4-6.7% RSD (n = 4) for elution from the same bed. The demonstrated ability of this device design and operation to elute from multiple fractionation beds into a single exit channel for sample analysis by fluorescence or electrospray mass spectrometry is a crucial component of an integrated fractionation and assay system for proteomics.
Effectiveness and safety of drug-eluting stents in Ontario.
Tu, Jack V; Bowen, James; Chiu, Maria; Ko, Dennis T; Austin, Peter C; He, Yaohua; Hopkins, Robert; Tarride, Jean-Eric; Blackhouse, Gord; Lazzam, Charles; Cohen, Eric A; Goeree, Ron
2007-10-04
The placement of drug-eluting stents decreases the frequency of repeat revascularization procedures in patients undergoing percutaneous coronary intervention (PCI) in randomized clinical trials. However, there is uncertainty about the effectiveness of drug-eluting stents, and increasing concern about their safety, in routine clinical practice. From the Cardiac Care Network of Ontario's population-based clinical registry of all patients undergoing PCI in Ontario, Canada, we identified a well-balanced cohort of 3751 pairs of patients, matched on the basis of propensity score, who received either bare-metal stents alone or drug-eluting stents alone during an index PCI procedure between December 1, 2003, and March 31, 2005. The primary outcomes of the study were the rates of target-vessel revascularization, myocardial infarction, and death. The 2-year rate of target-vessel revascularization was significantly lower among patients who received drug-eluting stents than among those who received bare-metal stents (7.4% vs. 10.7%, P<0.001). Drug-eluting stents were associated with significant reductions in the rate of target-vessel revascularization among patients with two or three risk factors for restenosis (i.e., presence of diabetes, small vessels [<3 mm in diameter], and long lesions [> or =20 mm]) but not among lower-risk patients. The 3-year mortality rate was significantly higher in the bare-metal-stent group than in the drug-eluting-stent group (7.8% vs. 5.5%, P<0.001), whereas the 2-year rate of myocardial infarction was similar in the two groups (5.2% and 5.7%, respectively; P=0.95). Drug-eluting stents are effective in reducing the need for target-vessel revascularization in patients at highest risk for restenosis, without a significantly increased rate of death or myocardial infarction. Copyright 2007 Massachusetts Medical Society.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Song, Zhi-Gang; State Key Laboratory of Superlattices and Microstructures, Institute of Semiconductors, Chinese Academy of Sciences, P.O. Box 912, Beijing 100083; Bose, Sumanta
The electronic band structure and optical gain of GaN{sub x}Bi{sub y}As{sub 1−x−y}/GaAs pyramidal quantum dots (QDs) are investigated using the 16-band k ⋅ p model with constant strain. The optical gain is calculated taking both homogeneous and inhomogeneous broadenings into consideration. The effective band gap falls as we increase the composition of nitrogen (N) and bismuth (Bi) and with an appropriate choice of composition we can tune the emission wavelength to span within 1.3 μm–1.55 μm, for device application in fiber technology. The extent of this red shift is more profound in QDs compared with bulk material due to quantum confinement. Othermore » factors affecting the emission characteristics include virtual crystal, strain profile, band anticrossing (BAC), and valence band anticrossing (VBAC). The strain profile has a profound impact on the electronic structure, specially the valence band of QDs, which can be determined using the composition distribution of wave functions. All these factors eventually affect the optical gain spectrum. With an increase in QD size, we observe a red shift in the emission energy and emergence of secondary peaks owing to transitions or greater energy compared with the fundamental transition.« less
NASA Astrophysics Data System (ADS)
Sockalingam, Komathi; Misnan, Rosmilah; Yadzir, Zailatul Hani Mohd
2017-05-01
Prawn allergy is certainly the most frequent cause of allergic reactions in countries where this crustacean is a popular dish of seafood. The aim of this study was to determine the protein profiles of giant river prawn which scientifically known as Macrobrachium rosenbergii. Raw and cooked extracts (boiled, steamed and fried) of prawn samples were prepared and then resolved by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). 27 protein bands between 6 to 207 kDa were detected in the SDS-PAGE gel of raw extracts while boiled, steamed and fried extracts revealed fewer protein bands. Steamed and boiled prawns presented higher numbers of protein bands compared to fried prawn. A prominent heat-resistant band between 32 to 38 kDa was seen in all extracts, might hypothesized to be tropomyosin. Other prominent bands between 17 to 20 kDa were also seen in all treated prawn extracts while bands of 24 to 27 kDa were seen in steamed and boiled prawn extracts. These positions are consistent with the known shellfish allergens myosin light chain, sacroplasmic calcium binding protein and troponin C respectively. Several other heat-sensitive protein bands at various molecular weights were also not detected in boiled, steamed and fried extracts of this prawn. This study showed that M. rosenbergii contains numerous heat-sensitive and heat-resistant proteins, which may play an important role in prawn allergy.
Elimination of surface band bending on N-polar InN with thin GaN capping
DOE Office of Scientific and Technical Information (OSTI.GOV)
Kuzmík, J., E-mail: Jan.Kuzmik@savba.sk; Haščík, Š.; Kučera, M.
2015-11-09
0.5–1 μm thick InN (0001) films grown by molecular-beam epitaxy with N- or In-polarity are investigated for the presence of native oxide, surface energy band bending, and effects introduced by 2 to 4 monolayers of GaN capping. Ex situ angle-resolved x-ray photo-electron spectroscopy is used to construct near-surface (GaN)/InN energy profiles, which is combined with deconvolution of In3d signal to trace the presence of InN native oxide for different types of polarity and capping. Downwards surface energy band bending was observed on bare samples with native oxide, regardless of the polarity. It was found that the In-polar InN surface is mostmore » readily oxidized, however, with only slightly less band bending if compared with the N-polar sample. On the other hand, InN surface oxidation was effectively mitigated by GaN capping. Still, as confirmed by ultra-violet photo-electron spectroscopy and by energy band diagram calculations, thin GaN cap layer may provide negative piezoelectric polarization charge at the GaN/InN hetero-interface of the N-polar sample, in addition to the passivation effect. These effects raised the band diagram up by about 0.65 eV, reaching a flat-band profile.« less
Alendronate-Eluting Biphasic Calcium Phosphate (BCP) Scaffolds Stimulate Osteogenic Differentiation
Kim, Sung Eun; Lee, Deok-Won; Kang, Eun Young; Jeong, Won Jae; Lee, Boram; Jeong, Myeong Seon; Kim, Hak Jun; Park, Kyeongsoon; Song, Hae-Ryong
2015-01-01
Biphasic calcium phosphate (BCP) scaffolds have been widely used in orthopedic and dental fields as osteoconductive bone substitutes. However, BCP scaffolds are not satisfactory for the stimulation of osteogenic differentiation and maturation. To enhance osteogenic differentiation, we prepared alendronate- (ALN-) eluting BCP scaffolds. The coating of ALN on BCP scaffolds was confirmed by scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), and attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR). An in vitro release study showed that release of ALN from ALN-eluting BCP scaffolds was sustained for up to 28 days. In vitro results revealed that MG-63 cells grown on ALN-eluting BCP scaffolds exhibited increased ALP activity and calcium deposition and upregulated gene expression of Runx2, ALP, OCN, and OPN compared with the BCP scaffold alone. Therefore, this study suggests that ALN-eluting BCP scaffolds have the potential to effectively stimulate osteogenic differentiation. PMID:26221587
DOE Office of Scientific and Technical Information (OSTI.GOV)
Pan, Horng-Bin; Wai, Chien M.; Kuo, Li-Jung
Uranium adsorbed on amidoxime-based polyethylene fibers in simulated seawater can be quantitatively eluted using 3 M KHCO3 at 40°C. Thermodynamic calculations are in agreement with the experimental observation that at high bicarbonate concentrations (3 M) uranyl ions bound to amidoxime molecules are converted to uranyl tris-carbonato complex in the aqueous solution. The elution process is basically the reverse reaction of the uranium adsorption process which occurs at a very low bicarbonate concentration (~10-3 M) in seawater. In real seawater experiments, the bicarbonate elution is followed by a NaOH treatment to remove natural organic matter adsorbed on the polymer adsorbent. Usingmore » the sequential bicarbonate and NaOH elution, the adsorbent is reusable after rinsing with deionized water and the recycled adsorbent shows no loss of uranium loading capacity based on real seawater experiments.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Pan, Horng-Bin; Wai, Chien M.; Kuo, Li-Jung
Uranium adsorbed on amidoxime-based polyethylene fibers in simulated seawater can be quantitatively eluted using 3 M KHCO 3 at 40°C. Thermodynamic calculations are in agreement with the experimental observation that at high bicarbonate concentrations (3 M) uranyl ions bound to amidoxime molecules are converted to uranyl tris-carbonato complex in the aqueous solution. The elution process is basically the reverse reaction of the uranium adsorption process which occurs at a very low bicarbonate concentration (~10 -3 M) in seawater. The bicarbonate elution is followed by a NaOH treatment to remove natural organic matter adsorbed on the polymer adsorbent, in real seawatermore » experiments. Furthermore, by using the sequential bicarbonate and NaOH elution, the adsorbent is reusable after rinsing with deionized water and the recycled adsorbent shows no loss of uranium loading capacity based on real seawater experiments.« less
Technetium-99m generator system
Mirzadeh, Saed; Knapp, Jr., Furn F.; Collins, Emory D.
1998-01-01
A .sup.99 Mo/.sup.99m Tc generator system includes a sorbent column loaded with a composition containing .sup.99 Mo. The sorbent column has an effluent end in fluid communication with an anion-exchange column for concentrating .sup.99m Tc eluted from the sorbent column. A method of preparing a concentrated solution of .sup.99m Tc includes the general steps of: a. providing a sorbent column loaded with a composition containing .sup.99 Mo, the sorbent column having an effluent end in fluid communication with an anion-exchange column; b. eluting the sorbent column with a salt solution to elute .sup.99m Tc from the sorbent and to trap and concentrate the eluted .sup.99m Tc on the ion-exchange column; and c. eluting the concentrated .sup.99m Tc from the ion-exchange column with a solution comprising a reductive complexing agent.
Technetium-99m generator system
Mirzadeh, S.; Knapp, F.F. Jr.; Collins, E.D.
1998-06-30
A {sup 99}Mo/{sup 99m}Tc generator system includes a sorbent column loaded with a composition containing {sup 99}Mo. The sorbent column has an effluent end in fluid communication with an anion-exchange column for concentrating {sup 99m}Tc eluted from the sorbent column. A method of preparing a concentrated solution of {sup 99m}Tc includes the general steps of: (a) providing a sorbent column loaded with a composition containing {sup 99}Mo, the sorbent column having an effluent end in fluid communication with an anion-exchange column; (b) eluting the sorbent column with a salt solution to elute {sup 99m}Tc from the sorbent and to trap and concentrate the eluted {sup 99m}Tc on the ion-exchange column; and (c) eluting the concentrated {sup 99m}Tc from the ion-exchange column with a solution comprising a reductive complexing agent. 1 fig.
Pan, Horng-Bin; Wai, Chien M.; Kuo, Li-Jung; ...
2017-05-02
Uranium adsorbed on amidoxime-based polyethylene fibers in simulated seawater can be quantitatively eluted using 3 M KHCO 3 at 40°C. Thermodynamic calculations are in agreement with the experimental observation that at high bicarbonate concentrations (3 M) uranyl ions bound to amidoxime molecules are converted to uranyl tris-carbonato complex in the aqueous solution. The elution process is basically the reverse reaction of the uranium adsorption process which occurs at a very low bicarbonate concentration (~10 -3 M) in seawater. The bicarbonate elution is followed by a NaOH treatment to remove natural organic matter adsorbed on the polymer adsorbent, in real seawatermore » experiments. Furthermore, by using the sequential bicarbonate and NaOH elution, the adsorbent is reusable after rinsing with deionized water and the recycled adsorbent shows no loss of uranium loading capacity based on real seawater experiments.« less
Resonant beam behavior studies in the Proton Storage Ring
NASA Astrophysics Data System (ADS)
Cousineau, S.; Holmes, J.; Galambos, J.; Fedotov, A.; Wei, J.; Macek, R.
2003-07-01
We present studies of space-charge-induced beam profile broadening at high intensities in the Proton Storage Ring (PSR) at Los Alamos National Laboratory. We investigate the profile broadening through detailed particle-in-cell simulations of several experiments and obtain results in good agreement with the measurements. We interpret these results within the framework of coherent resonance theory. With increasing intensity, our simulations show strong evidence for the presence of a quadrupole-mode resonance of the beam envelope with the lattice in the vertical plane. Specifically, we observe incoherent tunes crossing integer values, and large amplitude, nearly periodic envelope oscillations. At the highest operating intensities, we observe a continuing relaxation of the beam through space charge forces leading to emittance growth. The increase of emittance commences when the beam parameters encounter an envelope stop band. Once the stop band is reached, the emittance growth balances the intensity increase to maintain the beam near the stop band edge. Additionally, we investigate the potential benefit of a stop band correction to the high intensity PSR beam.
NASA Technical Reports Server (NTRS)
Mumma, M. J.; Stone, E. J.; Zipf, E. C.
1975-01-01
Measurements were made of the rotational profiles of specific bands of the CO fourth-positive group (4PG). The CO 4PG bands were excited by electron impact dissociative excitation of CO2. The results are applicable to analysis of the Mariner observations of the CO 4PG in the dayglow of Mars. The results indicate that dissociative excitation of CO2 by electron impact leads to CO(A 1Pi) fragments with a rotational distribution that is highly nonthermal. The parent CO2 temperature was about 300 K in the experiment, while the fragment CO(A 1Pi) showed emission band profiles consistent with a rotational temperature greater than about 1500 K. Laboratory measurement of the reduced transmission of the hot bands by thermal CO appears to be the most direct way of determining the column density responsible for the CO(v',0) absorption of Mars.
NASA Astrophysics Data System (ADS)
Deshpande, Sachin M.; Dhangar, N.; Das, S. K.; Kalapureddy, M. C. R.; Chakravarty, K.; Sonbawne, S.; Konwar, M.
2015-11-01
Single Doppler analysis techniques known as velocity azimuth display (VAD) and volume velocity processing (VVP) are used to analyze kinematics of mesoscale flow such as horizontal wind and divergence using X-band Doppler weather radar observations, for selected cases of convective, stratiform, and shallow cloud systems near tropical Indian sites Pune (18.58°N, 73.92°E, above sea level (asl) 560 m) and Mandhardev (18.51°N, 73.85°E, asl 1297 m). The vertical profiles of horizontal wind estimated from radar VVP/VAD methods agree well with GPS radiosonde profiles, with the low-level jet at about 1.5 km during monsoon season well depicted in both. The vertical structure and temporal variability of divergence and reflectivity profiles are indicative of the dynamical and microphysical characteristics of shallow convective, deep convective, and stratiform cloud systems. In shallow convective systems, vertical development of reflectivity profiles is limited below 5 km. In deep convective systems, reflectivity values as large as 55 dBZ were observed above freezing level. The stratiform system shows the presence of a reflectivity bright band (~35 dBZ) near the melting level. The diagnosed vertical profiles of divergence in convective and stratiform systems are distinct. In shallow convective conditions, convergence was seen below 4 km with divergence above. Low-level convergence and upper level divergence are observed in deep convective profiles, while stratiform precipitation has midlevel convergence present between lower level and upper level divergence. The divergence profiles in stratiform precipitation exhibit intense shallow layers of "melting convergence" at 0°C level, near 4.5 km altitude, with a steep gradient on the both sides of the peak. The level of nondivergence in stratiform situations is lower than that in convective situations. These observed vertical structures of divergence are largely indicative of latent heating profiles in the atmosphere, an important ingredient of monsoon dynamics.
From AFF to CCNT : JPL's evolving family of multifunction constellation transceivers
NASA Technical Reports Server (NTRS)
Bar-Sever, Yoaz; Srinivasan, Jeff; Farrington, Allen
2001-01-01
This paper describes the profiles and requirements of the ST-3 and ST-5 missions, and discusses the unique technological challenges each of them presents. Bothe the AFF and CCNT trace their heritage to GPS receivers, using measurements of both RF carrier phase and a ranging code. They will operate, however, at very different frequency bands; the ADD at Ka-band, and the CCNT at S-band.
Stone, Gregg W; Teirstein, Paul S; Meredith, Ian T; Farah, Bruno; Dubois, Christophe L; Feldman, Robert L; Dens, Joseph; Hagiwara, Nobuhisa; Allocco, Dominic J; Dawkins, Keith D
2011-04-19
We sought to evaluate the clinical outcomes with a novel platinum chromium everolimus-eluting stent (PtCr-EES) compared with a predicate cobalt chromium everolimus-eluting stent (CoCr-EES) in patients undergoing percutaneous coronary intervention (PCI). Randomized trials have demonstrated an excellent safety and efficacy profile for the CoCr-EES. The PtCr-EES uses the identical antiproliferative agent and polymer but with a novel platinum chromium scaffold designed for enhanced deliverability, vessel conformability, side-branch access, radiopacity, radial strength, and fracture resistance. A total of 1,530 patients undergoing PCI of 1 or 2 de novo native lesions were randomized at 132 worldwide sites to CoCr-EES (n = 762) or PtCr-EES (n = 768). The primary endpoint was the 12-month rate of target lesion failure (TLF), the composite of target vessel-related cardiac death, target vessel-related myocardial infarction (MI), or ischemia-driven target lesion revascularization (TLR) in the per-protocol population (patients who received ≥1 assigned study stent), powered for noninferiority. The 12-month rate of TLF in the per-protocol population occurred in 2.9% versus 3.4% of patients assigned to CoCr-EES versus PtCr-EES, respectively (difference: 0.5%, 95% confidence interval: -1.3% to 2.3%, p(noninferiority) = 0.001, p(superiority) = 0.60). By intention-to-treat, there were no significant differences between CoCr-EES and PtCr-EES in the 12-month rates of TLF (3.2% vs. 3.5%, p = 0.72), cardiac death or MI (2.5% vs. 2.0%, p = 0.56), TLR (1.9% vs. 1.9%, p = 0.96), or Academic Research Consortium definite or probable stent thrombosis (0.4% vs. 0.4%, p = 1.00). In this large-scale, prospective, single-blind randomized trial, a novel PtCr-EES was noninferior to the predicate CoCr-EES for TLF, with nonsignificant differences in measures of safety and efficacy through 12-month follow-up after PCI. Copyright © 2011 American College of Cardiology Foundation. Published by Elsevier Inc. All rights reserved.
Drug-eluting stents and acute myocardial infarction: A lethal combination or friends?
Otsuki, Shuji; Sabaté, Manel
2014-01-01
Primary percutaneous coronary intervention is the preferred reperfusion strategy for patients presenting with ST-segment elevation myocardial infarction (STEMI). First generation drug-eluting stents (DES), (sirolimus drug-eluting stents and paclitaxel drug-eluting stents), reduce the risk of restenosis and target vessel revascularization compared to bare metal stents. However, stent thrombosis emerged as a major safety concern with first generation DES. In response to these safety issues, second generation DES were developed with different drugs, improved stent platforms and more biocompatible durable or bioabsorbable polymeric coating. This article presents an overview of safety and efficacy of the first and second generation DES in STEMI. PMID:25276295
NASA Astrophysics Data System (ADS)
Kalachev, L. V.
2016-06-01
We present a simple model of experimental setup for in vitro study of drug release from drug eluting stents and drug propagation in artificial tissue samples representing blood vessels. The model is further reduced using the assumption on vastly different characteristic diffusion times in the stent coating and in the artificial tissue. The model is used to derive a relationship between the times at which the measurements have to be taken for two experimental platforms, with corresponding artificial tissue samples made of different materials with different drug diffusion coefficients, to properly compare the drug release characteristics of drug eluting stents.
Parodi, S; Balbi, C; Abelmoschi, M L; Pala, M; Russo, P; Santi, L
1983-12-01
Alkaline elution is a well-known method for detecting DNA damage. Recently we have developed a viscosimetric method that is even more sensitive than alkaline elution. Here we report that the two methods, although apparently both revealing alkaline DNA fragmentation, can give dramatically different results for a significant series of compounds. We suspect that alkaline elution might reveal not only DNA fragmentation but also the extent of disentanglement of chromatin structure, whereas this DNA disentanglement rate, when evaluated viscosimetrically , is more strictly correlated with the initiation of DNA unwinding.
Drug eluting biliary stents to decrease stent failure rates: A review of the literature
Shatzel, Joseph; Kim, Jisoo; Sampath, Kartik; Syed, Sharjeel; Saad, Jennifer; Hussain, Zilla H; Mody, Kabir; Pipas, J Marc; Gordon, Stuart; Gardner, Timothy; Rothstein, Richard I
2016-01-01
Biliary stenting is clinically effective in relieving both malignant and non-malignant obstructions. However, there are high failure rates associated with tumor ingrowth and epithelial overgrowth as well as internally from biofilm development and subsequent clogging. Within the last decade, the use of prophylactic drug eluting stents as a means to reduce stent failure has been investigated. In this review we provide an overview of the current research on drug eluting biliary stents. While there is limited human trial data regarding the clinical benefit of drug eluting biliary stents in preventing stent obstruction, recent research suggests promise regarding their safety and potential efficacy. PMID:26839648
Lemasson, Elise; Bertin, Sophie; Hennig, Philippe; Boiteux, Hélène; Lesellier, Eric; West, Caroline
2015-08-21
Impurity profiling of organic products that are synthesized as possible drug candidates requires complementary analytical methods to ensure that all impurities are identified. Supercritical fluid chromatography (SFC) is a very useful tool to achieve this objective, as an adequate selection of stationary phases can provide orthogonal separations so as to maximize the chances to see all impurities. In this series of papers, we have developed a method for achiral SFC-MS profiling of drug candidates, based on a selection of 160 analytes issued from Servier Research Laboratories. In the first part of this study, focusing on mobile phase selection, a gradient elution with carbon dioxide and methanol comprising 2% water and 20mM ammonium acetate proved to be the best in terms of chromatographic performance, while also providing good MS response [1]. The objective of this second part was the selection of an orthogonal set of ultra-high performance stationary phases, that was carried out in two steps. Firstly, a reduced set of analytes (20) was used to screen 23 columns. The columns selected were all 1.7-2.5μm fully porous or 2.6-2.7μm superficially porous particles, with a variety of stationary phase chemistries. Derringer desirability functions were used to rank the columns according to retention window, column efficiency evaluated with peak width of selected analytes, and the proportion of analytes successfully eluted with good peak shapes. The columns providing the worst performances were thus eliminated and a shorter selection of columns (11) was obtained. Secondly, based on 160 tested analytes, the 11 columns were ranked again. The retention data obtained on these columns were then compared to define a reduced set of the best columns providing the greatest orthogonality, to maximize the chances to see all impurities within a limited number of runs. Two high-performance columns were thus selected: ACQUITY UPC(2) HSS C18 SB and Nucleoshell HILIC. Copyright © 2015 Elsevier B.V. All rights reserved.
Fan, Wenzhe; Zhang, Yu; Carr, Peter W.; Rutan, Sarah C.; Dumarey, Melanie; Schellinger, Adam P.; Pritts, Wayne
2011-01-01
Fourteen judiciously selected reversed-phase columns were tested with 18 cationic drug solutes under the isocratic elution conditions advised in the Snyder-Dolan (S-D) hydrophobic subtraction method of column classification. The standard errors (S.E.) of the least squares regressions of log k′ vs. log k′REF were obtained for a given column against a reference column and used to compare and classify columns based on their selectivity. The results are consistent with those obtained with a study of the 16 test solutes recommended by Snyder and Dolan. To the extent that these drugs are representative these results show that the S-D classification scheme is also generally applicable to pharmaceuticals under isocratic conditions. That is, those columns judged to be similar based on the S-D 16 solutes were similar based on the 18 drugs; furthermore those columns judged to have significantly different selectivities based on the 16 S-D probes appeared to be quite different for the drugs as well. Given that the S-D method has been used to classify more than 400 different types of reversed phases the extension to cationic drugs is a significant finding. PMID:19698948
Anuradha, S; Kumar, K Shravan; Bhama, S; Kishan, V
2016-09-01
Tuberculosis, caused by Mycobacterium tuberculosis, continues to be a serious public health problem around the world, and it urges the need for development of new antitubercular drugs. An antibiotic producing strain, Streptomyces luridus (MTCC 4402) was earlier isolated from soil by our group. In this work, the phylogenic status was established by 16S rRNA gene sequence analysis. The strain was found to be active against clinically resistant strains. The culture was grown in shake flasks in a medium containing cornsteep liquor, glucose, CaCO(3), soyabean meal and starch. Antibiotic production reached maximum at the end of 72 h. and fermentation profile was obtained. The active compound was extracted into ethyl acetate and was subjected to activity guided purification by column chromatography using silica gel, TLC and HPLC methods. The pure compound eluted at 16.7 min. by gradient elution was subjected to (1)H, (13)C NMR and mass spectral analyses. The acquired data was compared with that of natural products’ data base and found to be a known antibiotic, spiramycin. The purified compound was studied for mutagenic, cytotoxicity, antitubercular activities. It was non mutagenic at the concentration of 1000 μg/mL, non cytotoxic and active as antitubercular agent at a concentration of 64 mg/mL and was comparable to rifampicin.
Salman, D; Peron, J-M R; Goronga, T; Barton, S; Swinden, J; Nabhani-Gebara, S
2016-03-01
The aim of this study is to conduct a forced degradation study on ifosfamide under several stress conditions to investigate the robustness of the developed HPLC method. It also aims to provide further insight into the stability of ifosfamide and its degradation profile using both HPLC and NMR. Ifosfamide solutions (20mg/mL; n=15, 20mL) were stressed in triplicate by heating (70°C), under acidic (pH 1 & 4) and alkaline (pH 10 & 12) conditions. Samples were analysed periodically using HPLC and FT-NMR. Ifosfamide was most stable under weakly acidic conditions (pH 4). NMR results suggested that the mechanism of ifosfamide degradation involves the cleavage of the PN bond. For all stress conditions, HPLC was not able to detect ifosfamide degradation products that were detected by NMR. These results suggest that the developed HPLC method for ifosfamide did not detect the degradation products shown by NMR. It is possible that degradation products co-elute with ifosfamide, do not elute altogether or are not amenable to the detection method employed. Therefore, investigation of ifosfamide stability requires additional techniques that do not suffer from the aforementioned shortcomings. Copyright © 2015 Académie Nationale de Pharmacie. Published by Elsevier Masson SAS. All rights reserved.
NASA Astrophysics Data System (ADS)
Salem, Mohamed Shaker; Abdelaleem, Asmaa Mohamed; El-Gamal, Abear Abdullah; Amin, Mohamed
2017-01-01
One-dimensional silicon-based photonic crystals are formed by the electrochemical anodization of silicon substrates in hydrofluoric acid-based solution using an appropriate current density profile. In order to create a multi-band optical filter, two fabrication approaches are compared and discussed. The first approach utilizes a current profile composed of a linear combination of sinusoidal current waveforms having different frequencies. The individual frequency of the waveform maps to a characteristic stop band in the reflectance spectrum. The stopbands of the optical filter created by the second approach, on the other hand, are controlled by stacking multiple porous silicon rugate multilayers having different fabrication conditions. The morphology of the resulting optical filters is tuned by controlling the electrolyte composition and the type of the silicon substrate. The reduction of sidelobes arising from the interference in the multilayers is observed by applying an index matching current profile to the anodizing current waveform. In order to stabilize the resulting optical filters against natural oxidation, atomic layer deposition of silicon dioxide on the pore wall is employed.
Neuropsychological Profile of Children with Subcortical Band Heterotopia
ERIC Educational Resources Information Center
Spencer-Smith, Megan; Leventer, Richard; Jacobs, Rani; De Luca, Cinzia; Anderson, Vicki
2009-01-01
Aim: Subcortical band heterotopia (SBH) or "double cortex" is a malformation of cortical development resulting from impaired neuronal migration. So far, research has focused on the neurological, neuroimaging, and genetic correlates of SBH. More recently, clinical reports and small sample studies have documented neuropsychological dysfunction in…
Stent Coating Integrity of Durable and Biodegradable Coated Drug Eluting Stents.
Yazdani, Saami K; Sheehy, Alexander; Pacetti, Stephen; Rittlemeyer, Brandon; Kolodgie, Frank D; Virmani, Renu
2016-10-01
Coatings consisting of a polymer and drug are widely used in drug-eluting stents (DES) and are essential in providing programmable drug release kinetics. Among other factors, stent coating technologies can influence blood compatibility, affect acute and sub-acute healing, and potentially trigger a chronic inflammatory response. The aim of this study was to investigate the short-term (7 and 28 days) and long-term (90 and 180 days) coating integrity of the Xience Prime Everolimus-Eluting Stent (EES), Resolute Zotarolimus-Eluting Stent (ZES), Taxus Paclitaxel-Eluting Stent (PES), and Nobori Biolimus A9-Eluting Stent (BES) in a rabbit ilio-femoral stent model. Stented arteries (n = 48) were harvested and the tissue surrounding the implanted stents digested away with an enzymatic solution. Results demonstrated that the majority of struts of EES were without any coating defects with a few struts showing minor defects. Similarly, for the ZES, most of the struts were without coating defects at all time points except at 180 days. The majority of PES demonstrated mostly webbing and uneven coating. In the BES group, the majority of strut coating showed polymer cracking. Overall, the EES and ZES had fewer coating defects than the PES and BES. Coating defects, however increase over time for the ZES, whereas the percent of coating irregularities remained constant for the EES. These results provide, for the first time, a comparison of the long-term durability of these drug-eluting stent coatings in vivo. © 2016, Wiley Periodicals, Inc.
Galon, Micheli Z.; Gutierrez, Paulo S.; Sojitra, Prakash; Vyas, Ashwin; Doshi, Manish; Lemos, Pedro A.
2015-01-01
Background Permanent polymers in first generation drug-eluting stent (DES) have been imputed to be a possible cause of persistent inflammation, remodeling, malapposition and late stent thrombosis. We aim to describe the in vivo experimental result of a new polymer-free DES eluting sirolimus from stent-plus-balloon (Focus np stent, Envision Scientific) compared with a bare-metal stent (BMS) (Amazonia CroCo, Minvasys) and with a biolimus A9 eluting stent (Biomatrix, Biosensors). Methods In 10 juvenile pigs, 23 coronary stents were implanted in the coronary arteries (8 Amazonia CroCo, 8 Focus np, and 7 Biomatrix). At 28-day follow-up, optical coherence tomography (OCT) and histology were used to evaluate neointimal hyperplasia and healing response. Results According to OCT analysis, Focus np stents had a greater lumen area and less neointimal hyperplasia response than BMS and Biomatrix had. Histomorphometry results showed less neointimal hyperplasia in Focus np than in BMS. Histology showed a higher fibrin deposition in Biomatrix stent compared to Focus np and BMS. Conclusions The new polymer-free DES with sirolimus eluted from stent-plus-balloon demonstrated safety and reduced neointimal proliferation compared with the BMS and Biomatrix stents at 28-day follow-up in this porcine coronary model. This new polymer-free DES is promising and warrants further clinical studies. PMID:25984451
Padró, Juan M; Osorio-Grisales, Jaiver; Arancibia, Juan A; Olivieri, Alejandro C; Castells, Cecilia B
2015-07-01
Valuable quantitative information could be obtained from strongly overlapped chromatographic profiles of two enantiomers by using proper chemometric methods. Complete separation profiles where the peaks are fully resolved are difficult to achieve in chiral separation methods, and this becomes a particularly severe problem in case that the analyst needs to measure the chiral purity, i.e., when one of the enantiomers is present in the sample in very low concentrations. In this report, we explore the scope of a multivariate chemometric technique based on unfolded partial least-squares regression, as a mathematical tool to solve this quite frequent difficulty. This technique was applied to obtain quantitative results from partially overlapped chromatographic profiles of R- and S-ketoprofen, with different values of enantioresolution factors (from 0.81 down to less than 0.2 resolution units), and also at several different S:R enantiomeric ratios. Enantiomeric purity below 1% was determined with excellent precision even from almost completely overlapped signals. All these assays were tested on the most demanding condition, i.e., when the minor peak elutes immediately after the main peak. The results were validated using univariate calibration of completely resolved profiles and the method applied to the determination of enantiomeric purity of commercial pharmaceuticals. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Thul, Sanjog T; Srivastava, Ankit K; Singh, Subhash C; Shanker, Karuna
2011-09-01
A method was developed based on multiple approaches wherein DNA and chemical analysis was carried out toward differentiation of important species of Sida complex that is being used for commercial preparation. Isolated DNA samples were successfully performed through PCR amplification using ISSR markers and degree of genetic diversity among the different species of Sida is compared with that of chemical diversity. For genetic fingerprint investigation, selected 10 ISSR primers generating reproducible banding patterns were used. Among the total of 63 amplicons, 62 were recorded as polymorphic, genetic similarity index deduced from ISSR profiles ranged from 12 to 51%. Based on similarity index, S. acuta and S. rhombifolia found to be most similar (51%). High number of species-specific bands played pivotal role to delineate species at genetic level. Investigation based on HPTLC fingerprints analysis revealed 23 bands representing to characteristic chemicals and similarity index ranged from 73 to 91%. Prominent distinguishable bands were observed only in S. acuta, while S. cordifolia and S. rhombifolia shared most bands making them difficult to identify on chemical fingerprint basis. This report summarizes the genotypic and chemotypic diversity and the use of profiles for authentication of species of Sida complex.
NASA Astrophysics Data System (ADS)
Tapia, V.; González, A.; Finger, R.; Mena, F. P.; Monasterio, D.; Reyes, N.; Sánchez, M.; Bronfman, L.
2017-03-01
We present the design, implementation, and characterization of the optics of ALMA Band 1, the lowest frequency band in the most advanced radio astronomical telescope. Band 1 covers the broad frequency range from 35 to 50 GHz, with the goal of minor degradation up to 52 GHz. This is, up to now, the largest fractional bandwidth of all ALMA bands. Since the optics is the first subsystem of any receiver, low noise figure and maximum aperture efficiency are fundamental for best sensitivity. However, a conjunction of several factors (small cryostat apertures, mechanical constraints, and cost limitations) makes extremely challenging to achieve these goals. To overcome these problems, the optics presented here includes two innovative solutions, a compact optimized-profile corrugated horn and a modified Fresnel lens. The horn profile was optimized for optimum performance and easy fabrication by a single-piece manufacturing process in a lathe. In this way, manufacturability is eased when compared with traditional fabrication methods. To minimize the noise contribution of the optics, a one-step zoned lens was designed. Its parameters were carefully optimized to maximize the frequency coverage and reduce losses. The optical assembly reported here fully complies with ALMA specifications.
Elution of viruses by ionic and nonionic surfactants.
Fujito, B T; Lytle, C D
1996-01-01
The ionic and nonionic surfactants sodium dodecyl sulfate and Triton X-100, respectively, eluted two viruses, phi X174 and PRD1, which were adsorbed to the ionic and nonionic binding membranes cationic polysulfone and nitrocellulose, respectively. Results indicated that complete elution was readily achieved only when combinations of surfactants and binding membranes were matched (i.e., ionic-ionic or nonionic-nonionic). PMID:8795240
Vlachojannis, Georgios J; Smits, Pieter C; Hofma, Sjoerd H; Togni, Mario; Vázquez, Nicolás; Valdés, Mariano; Voudris, Vassilis; Slagboom, Ton; Goy, Jean-Jaques; den Heijer, Peter; van der Ent, Martin
2017-06-26
This analysis investigates the 5-year outcomes of the biodegradable polymer biolimus-eluting stent (BP-BES) and durable polymer everolimus-eluting stent (DP-EES) in an all-comers population undergoing percutaneous coronary intervention. Recent 1- and 3-year results from randomized trials have indicated similar safety and efficacy outcomes of BP-BES and DP-EES. Whether benefits of the biodegradable polymer device arise over longer follow-up is unknown. Moreover, in-depth, prospective, long-term follow-up data on metallic drug-eluting stents with durable or biodegradable polymers are scarce. The COMPARE II trial (Abluminal Biodegradable Polymer Biolimus-Eluting Stent Versus Durable Polymer Everolimus-Eluting Stent) was a prospective, randomized, multicenter, all-comers trial in which 2,707 patients were randomly allocated (2:1) to BP-BES or DP-EES. The pre-specified endpoint at 5 years was major adverse cardiac events, a composite of cardiac death, nonfatal myocardial infarction, or target vessel revascularization. Five-year follow-up was available in 2,657 patients (98%). At 5 years, major adverse cardiac events occurred in 310 patients (17.3%) in the BP-BES group and 142 patients (15.6%) in the DP-EES group (p = 0.26). The rate of the combined safety endpoint all-cause death or myocardial infarction was 15.0% in the BP-BES group versus 14.8% in the DP-EES group (p = 0.90), whereas the efficacy measure target vessel revascularization was 10.6% versus 9.0% (p = 0.18), respectively. Interestingly, definite stent thrombosis rates did not differ between groups (1.5% for BP-BES vs. 0.9% for DP-EES; p = 0.17). The 5-year analysis comparing biodegradable polymer-coated BES and the durable polymer-coated EES confirms the initial early- and mid-term results regarding similar safety and efficacy outcomes in this all-comers percutaneous coronary intervention population. Copyright © 2017 American College of Cardiology Foundation. Published by Elsevier Inc. All rights reserved.
Brunner-La Rocca, Hans Peter; Kaiser, Christoph; Bernheim, Alain; Zellweger, Michael J; Jeger, Raban; Buser, Peter T; Osswald, Stefan; Pfisterer, Matthias
2007-11-03
Our aim was to determine whether drug-eluting stents are good value for money in long-term, everyday practice. We did an 18-month cost-effectiveness analysis of the Basel Stent KostenEffektivitäts Trial (BASKET), which randomised 826 patients 2:1 to drug-eluting stents (n=545) or to bare-metal stents (281). We used non-parametric bootstrap techniques to determine incremental cost-effectiveness ratios (ICERs) of drug-eluting versus bare-metal stents, to compare low-risk (> or =3.0 mm stents in native vessels; n=558, 68%) and high-risk patients (<3.0 mm stents/bypass graft stenting; n=268, 32%), and to do sensitivity analyses by altering costs and event rates in the whole study sample and in predefined subgroups. Quality-adjusted life-years (QALYs) were assessed by EQ-5D questionnaire (available in 703/826 patients). Overall costs were higher for patients with drug-eluting stents than in those with bare-metal stents (11,808 euros [SD 400] per patient with drug-eluting stents and 10,450 euros [592] per patient with bare-metal stents, mean difference 1358 euros [717], p<0.0001), due to higher stent costs. We calculated an ICER of 64,732 euros to prevent one major adverse cardiac event, and of 40,467 euros per QALY gained. Stent costs, number of events, and QALYs affected ICERs most, but unrealistic alterations would have been required to achieve acceptable cost-effectiveness. In low-risk patients, the probability of drug-eluting stents achieving an arbitrary ICER of 10,000 euros or less to prevent one major adverse cardiac event was 0.016; by contrast, it was 0.874 in high-risk patients. If used in all patients, drug-eluting stents are not good value for money, even if prices were substantially reduced. Drug-eluting stents are cost effective in patients needing small vessel or bypass graft stenting, but not in those who require large native vessel stenting.
Involvement of COX-2 in nickel elution from a wire implanted subcutaneously in mice.
Sato, Taiki; Kishimoto, Yu; Asakawa, Sanki; Mizuno, Natsumi; Hiratsuka, Masahiro; Hirasawa, Noriyasu
2016-07-01
Many types of medical alloys include nickel (Ni), and the elution of Ni ions from these materials causes toxicities and inflammation. We have previously reported that inflammation enhances Ni elution, although the molecular mechanisms underlying this effect remain unclear. In this study, we investigated how inflammatory responses enhanced Ni elution in a wire-implantation mouse model. Subcutaneous implantation of Ni wire induced the expression of cyclooxygenase-2 (COX-2) and microsomal prostaglandin E synthase-1 (mPGES-1) mRNA in the surrounding tissues. Immunostaining analysis showed that cells expressing COX-2 were mainly fibroblast-like cells 8h after implantation of a Ni wire, but were mainly infiltrated leukocytes at 24h. NiCl2 induced the expression of COX-2 mRNA in primary fibroblasts, neutrophils, RAW 264 cells, and THP-1 cells, indicating that Ni ions can induce COX-2 expression in various types of cells. The elution of Ni ions from the implanted Ni wire at 8h was reduced by dexamethasone (Dex), indomethacin (Ind), or celecoxib (Cel) treatment. Ni wire implantation induced an increase in mRNA levels for anaerobic glycolytic pathway components glucose transporter 1 (GLUT1), hexokinase 2 (HK2), lactate dehydrogenase A (LDHA), and monocarboxylate transporter 4 (MCT4); the expression of these genes was also inhibited by Dex, Ind, and Cel. In primary fibroblasts, the expression of these mRNAs and the production of lactate were induced by NiCl2 and further potentiated by PGE2. Furthermore, Ni wire-induced infiltration of inflammatory leukocytes was significantly reduced by Dex, Ind, or Cel. Depletion of neutrophils with a specific antibody caused reduction of both leukocyte infiltration and Ni elution. These results indicate that Ni ions eluted from wire induced COX-2 expression, which further promoted elution of Ni ions by increasing lactate production and leukocyte infiltration. Since COX inhibitors and Dex reduced the elution of Ni ions, these drugs may be useful for prevention of metal-related inflammation and allergy. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.
NASA Astrophysics Data System (ADS)
Long, D. A.; Wójtewicz, S.; Miller, C. E.; Hodges, J. T.
2015-08-01
We present new high accuracy measurements of the (30012)←(00001) CO2 band near 1575 nm recorded with a frequency-agile, rapid scanning cavity ring-down spectrometer. The resulting spectra were fit with the partially correlated, quadratic-speed-dependent Nelkin-Ghatak profile with line mixing. Significant differences were observed between the fitted line shape parameters and those found in existing databases, which are based upon more simplistic line profiles. Absolute transition frequencies, which were referenced to an optical frequency comb, are given, as well as the other line shape parameters needed to model this line profile. These high accuracy measurements should allow for improved atmospheric retrievals of greenhouse gas concentrations by current and future remote sensing missions.
NASA Technical Reports Server (NTRS)
Anikouchine, W. A. (Principal Investigator)
1973-01-01
The author has identified the following significant results. Radiance profiles drawn along cruise tracks have been examined for use in correlating digital radiance levels with ground truth data. Preliminary examination results are encouraging. Adding weighted levels from the 4 MSS bands appears to enhance specular surface reflections while rendering sensor noise white. Comparing each band signature to the added specular signature ought to enhance non-specular effects caused by ocean turbidity. Preliminary examination of radiance profiles and ground truth turbidity measurements revealed substantial correlation.
Denburg, J A; Behmann, S A
1994-01-01
OBJECTIVE--To examine specific lymphocyte or neuronal antigens immuno-precipitated by systemic lupus erythematosus (SLE) sera. METHOD--SLE sera were screened for the presence of antibodies binding to surface antigens of CD4(+) HUT-78 or SK-N-SH and IMR-6 neuroblastoma cells using Western blotting or radioimmunoprecipitation. RESULTS--IgG eluates from both lymphocytes and neuroblastoma cells recognised a 52 kd band in HUT 78 cell lysates. Eight sera studied further using radioimmunoprecipitation also demonstrated binding to a 52 kd antigen (4/8 on HUT-78, 8/8 on SK-N-SH cells), partially depleted by absorption with viable HUT-78. CONCLUSION--A 52 kd antigen recognised by SLE sera on lymphocytes and neuronal cells may play a role in the pathogenesis of neuropsychiatric-SLE. Images PMID:8017983
Influence of ablation impurities on blunt body re-entry ionization
NASA Technical Reports Server (NTRS)
Schexnayder, C. J., Jr.; Evans, J. S.
1974-01-01
Electron density profiles which include the effect of an ablated sodium impurity were computed for the boundary layer on a blunt-nosed body re-entering the atmosphere at 7.62 km/sec. Profiles are computed from the nose to a distance of four diameters along the RAM C-payload. A finite-difference, laminar, nonequilibrium chemistry boundary-layer program was used. Comparison of theory with S-band diagnostic antenna results, electron concentration deduced from X- and C-band attenuation data, and Langmuir probe data at several different aft body locations show that agreement is good at high altitude. At the lower altitudes there is disagreement between theory and S-band antenna data where the apparent discrepancy is attributed to the three-body recombination rate constant used for deionization of sodium coupled with the effect of angle of attack.
Stortecky, Stefan; Stefanini, Giulio G; daCosta, Bruno R; Rutjes, Anne Wilhelmina; Di Nisio, Marcello; Siletta, Maria G; Maione, Ausilia; Alfonso, Fernando; Clemmensen, Peter M; Collet, Jean-Philippe; Cremer, Jochen; Falk, Volkmar; Filippatos, Gerasimos; Hamm, Christian; Head, Stuart; Kappetein, Arie Pieter; Kastrati, Adnan; Knuuti, Juhani; Landmesser, Ulf; Laufer, Günther; Neumann, Franz-Joseph; Richter, Dimitri; Schauerte, Patrick; Sousa Uva, Miguel; Taggart, David P; Torracca, Lucia; Valgimigli, Marco; Wijns, William; Witkowski, Adam; Kolh, Philippe; Juni, Peter
2014-01-01
Objective To investigate whether revascularisation improves prognosis compared with medical treatment among patients with stable coronary artery disease. Design Bayesian network meta-analyses to combine direct within trial comparisons between treatments with indirect evidence from other trials while maintaining randomisation. Eligibility criteria for selecting studies A strategy of initial medical treatment compared with revascularisation by coronary artery bypass grafting or Food and Drug Administration approved techniques for percutaneous revascularization: balloon angioplasty, bare metal stent, early generation paclitaxel eluting stent, sirolimus eluting stent, and zotarolimus eluting (Endeavor) stent, and new generation everolimus eluting stent, and zotarolimus eluting (Resolute) stent among patients with stable coronary artery disease. Data sources Medline and Embase from 1980 to 2013 for randomised trials comparing medical treatment with revascularisation. Main outcome measure All cause mortality. Results 100 trials in 93 553 patients with 262 090 patient years of follow-up were included. Coronary artery bypass grafting was associated with a survival benefit (rate ratio 0.80, 95% credibility interval 0.70 to 0.91) compared with medical treatment. New generation drug eluting stents (everolimus: 0.75, 0.59 to 0.96; zotarolimus (Resolute): 0.65, 0.42 to 1.00) but not balloon angioplasty (0.85, 0.68 to 1.04), bare metal stents (0.92, 0.79 to 1.05), or early generation drug eluting stents (paclitaxel: 0.92, 0.75 to 1.12; sirolimus: 0.91, 0.75 to 1.10; zotarolimus (Endeavor): 0.88, 0.69 to 1.10) were associated with improved survival compared with medical treatment. Coronary artery bypass grafting reduced the risk of myocardial infarction compared with medical treatment (0.79, 0.63 to 0.99), and everolimus eluting stents showed a trend towards a reduced risk of myocardial infarction (0.75, 0.55 to 1.01). The risk of subsequent revascularisation was noticeably reduced by coronary artery bypass grafting (0.16, 0.13 to 0.20) followed by new generation drug eluting stents (zotarolimus (Resolute): 0.26, 0.17 to 0.40; everolimus: 0.27, 0.21 to 0.35), early generation drug eluting stents (zotarolimus (Endeavor): 0.37, 0.28 to 0.50; sirolimus: 0.29, 0.24 to 0.36; paclitaxel: 0.44, 0.35 to 0.54), and bare metal stents (0.69, 0.59 to 0.81) compared with medical treatment. Conclusion Among patients with stable coronary artery disease, coronary artery bypass grafting reduces the risk of death, myocardial infarction, and subsequent revascularisation compared with medical treatment. All stent based coronary revascularisation technologies reduce the need for revascularisation to a variable degree. Our results provide evidence for improved survival with new generation drug eluting stents but no other percutaneous revascularisation technology compared with medical treatment. PMID:24958153
Low altitude wind shear statistics derived from measured and FAA proposed standard wind profiles
NASA Technical Reports Server (NTRS)
Dunham, R. E., Jr.; Usry, J. W.
1984-01-01
Wind shear statistics were calculated for a simulated data set using wind profiles proposed as a standard and compared to statistics derived from measured wind profile data. Wind shear values were grouped in altitude bands of 100 ft between 100 and 1400 ft, and in wind shear increments of 0.025 kt/ft between + or - 0.600 kt/ft for the simulated data set and between + or - 0.200 kt/ft for the measured set. No values existed outside the + or - 0.200 kt/ft boundaries for the measured data. Frequency distributions, means, and standard deviations were derived for each altitude band for both data sets, and compared. Also, frequency distributions were derived for the total sample for both data sets and compared. Frequency of occurrence of a given wind shear was about the same for both data sets for wind shears, but less than + or 0.10 kt/ft, but the simulated data set had larger values outside these boundaries. Neglecting the vertical wind component did not significantly affect the statistics for these data sets. The frequency of occurrence of wind shears for the flight measured data was essentially the same for each altitude band and the total sample, but the simulated data distributions were different for each altitude band. The larger wind shears for the flight measured data were found to have short durations.
Woolfolk, C A
1985-01-01
The isolation of a xanthine dehydrogenase from Pseudomonas putida 40 which utilizes ferricyanide as an electron acceptor at high efficiency is presented. The new activity is separate from the NAD+ and oxygen-utilizing activities of the same organism but displays a broad pattern for reducing substrates typical of those of previously studied xanthine-oxidizing enzymes. Unlike the previously studied enzymes, the new enzyme appears to lack flavin but possess heme and is resistant to cyanide treatment. However, sensitivity of the purified enzyme to methanol and the selective elimination of the activity when tungstate is added to certain growth media suggest a role for molybdenum. The enzyme is subject to a selective proteolytic action during processing which is not accompanied by denaturation or loss of activity and which is minimized by the continuous exposure of the activity to EDTA and phenylmethylsulfonyl fluoride. Electrophoresis of the denatured enzyme in the presence of sodium dodecyl sulfate suggests that the enzyme is constructed of subunits with a molecular weight of approximately 72,000. Electrophoresis under native conditions of a purified enzyme previously exposed to magnesium ion reveals a series of major and minor activity bands which display some selectivity toward both electron donors and acceptors. An analysis of the effect of gel concentration on this pattern suggests that the enzyme forms a series of charge and size isomers with a pair of trimeric forms predominating. Comparison of the rate of sedimentation of the enzyme in sucrose gradients with its elution profile from standardized Sepharose 6B columns suggests a molecular weight of 255,000 for the major form of the native enzyme. Images PMID:3860496
Size-exclusion chromatography-based enrichment of extracellular vesicles from urine samples
Lozano-Ramos, Inés; Bancu, Ioana; Oliveira-Tercero, Anna; Armengol, María Pilar; Menezes-Neto, Armando; Del Portillo, Hernando A.; Lauzurica-Valdemoros, Ricardo; Borràs, Francesc E.
2015-01-01
Renal biopsy is the gold-standard procedure to diagnose most of renal pathologies. However, this invasive method is of limited repeatability and often describes an irreversible renal damage. Urine is an easily accessible fluid and urinary extracellular vesicles (EVs) may be ideal to describe new biomarkers associated with renal pathologies. Several methods to enrich EVs have been described. Most of them contain a mixture of proteins, lipoproteins and cell debris that may be masking relevant biomarkers. Here, we evaluated size-exclusion chromatography (SEC) as a suitable method to isolate urinary EVs. Following a conventional centrifugation to eliminate cell debris and apoptotic bodies, urine samples were concentrated using ultrafiltration and loaded on a SEC column. Collected fractions were analysed by protein content and flow cytometry to determine the presence of tetraspanin markers (CD63 and CD9). The highest tetraspanin content was routinely detected in fractions well before the bulk of proteins eluted. These tetraspanin-peak fractions were analysed by cryo-electron microscopy (cryo-EM) and nanoparticle tracking analysis revealing the presence of EVs. When analysed by sodium dodecyl sulphate–polyacrylamide gel electrophoresis, tetraspanin-peak fractions from urine concentrated samples contained multiple bands but the main urine proteins (such as Tamm–Horsfall protein) were absent. Furthermore, a preliminary proteomic study of these fractions revealed the presence of EV-related proteins, suggesting their enrichment in concentrated samples. In addition, RNA profiling also showed the presence of vesicular small RNA species. To summarize, our results demonstrated that concentrated urine followed by SEC is a suitable option to isolate EVs with low presence of soluble contaminants. This methodology could permit more accurate analyses of EV-related biomarkers when further characterized by -omics technologies compared with other approaches. PMID:26025625
FTA card utility for PCR detection of Mycobacterium leprae.
Aye, Khin Saw; Matsuoka, Masanori; Kai, Masanori; Kyaw, Kyaw; Win, Aye Aye; Shwe, Mu Mu; Thein, Min; Htoo, Maung Maung; Htoon, Myo Thet
2011-01-01
The suitability of the FTA® elute card for the collection of slit skin smear (SSS) samples for PCR detection of Mycobacterium leprae was evaluated. A total of 192 SSS leprosy samples, of bacillary index (BI) 1 to 5, were collected from patients attending two skin clinics in Myanmar and preserved using both FTA® elute cards and 70% ethanol tubes. To compare the efficacy of PCR detection of DNA from each BI class, PCR was performed to amplify an M. leprae-specific repetitive element. Of the 192 samples, 116 FTA® elute card and 112 70% ethanol samples were PCR positive for M. leprae DNA. When correlated with BI, area under the curve (AUC) values of the respective receiver-operating characteristic curves were similar for the FTA® elute card and ethanol collection methods (AUC=0.6). Taken together, our results indicate that the FTA® elute card, which enables the collection, transport, and archiving of clinical samples, is an attractive alternative to ethanol preservation for the detection of M. leprae DNA.
Zhang, Jie; Wang, Yue-Hai; Wei, Quan-Yuan; Du, Xiao-Jia; Qu, Yong-Shui
2018-02-01
As the most representative of lignocellulosic materials, corn stalk (CS) will be a great candidate to produce xylo-oligosaccharides (XOS). Owing to the high impurity content of the XOS produced by directly enzymatic hydrolysis of xylan extracted from CS, subsequent refining steps are essential. The present study was aimed to investigate desorption during ethanol elution to improve the quality and antioxidant activity of XOS from CS. The desorption was systematically investigated after optimizing the elution conditions. The results showed that it had an elution watershed when the volume ratio was 2:1. More interestingly, XOS had a obvious priorities of desorption during ethanol gradient elution. The highest purity of XOS was 98.12% from 30% ethanol eluate. Antioxidant activity assay showed that the highest radical scavenging activity of XOS was 89.89% obtained from 70% ethanol eluate at a concentration of 3 mg/mL, which could be used in antioxidant food, feed additives. Copyright © 2017 Elsevier Ltd. All rights reserved.
Yang, Yang; Gong, Hai-Huan; Song, Ai-Yang; Feng, Dan; Jin, Jie; Zhu, Song
2015-02-01
To determine the influence of denture base resins coated with antibacterial coating on water sorption, solubility and monomer elution. The values of water sorption and solubility were measured according to YY 0270-2003 and gas chromatography was used to examine the leachability of 4 commercially available heat-cured acrylic resins between experimental group and control group. Degree of crosslinking of the experimental heat-cured acrylic denture bases we remeasured by soxhlet extraction method. The data was analyzed by 17.0 software package. The values of water sorption, solubility and monomer elution of experimental group were lower compared to the control group. Degree of crosslinking of Heraeus reins was the highest among the experimental heat-cured acrylic denture bases. There is a same trend among water sorption, degree of crosslinking and the monomer elution. When the degree of crosslinking increases, the values of water sorption and monomer elution decrease. Antibacterial coating can improve the comprehensive properties of the denture base resins.
Wei, Huaibin; Yu, Huibin; Pan, Hongwei; Gao, Hongjie
2018-05-01
UV-visible absorption spectroscopy combined with principal component analysis (PCA) and two-dimensional correlation (2D correlation) is used to trace components of dissolved organic matter (DOM) extracted from soils in a larger estuarine delta and to investigate spatial variations of DOM fractions. Soil samples of different depths were collected from native halophyte soils along a saline gradient, i.e., Suaeda salsa Comm. (SSC), Chenopodium album Comm. (CAC), Phragmites australis Comm. (PAC), and Artemisia selengensis Comm. (ASC). Molecular weights of DOM within the SSC soil profile were the lowest, followed by the CAC, PAC, and ASC soil profiles. Humification degree of DOM within the ASC soil profile was the highest, followed by the PAC, SSC, and CAC soil profiles. DOM within the soil profiles mainly contained phenolic, carboxylic, microbial products, and aromatic and alkyl groups through the PCA, which presented the significant differentiation among the four native halophyte soil profiles. The 2D UV correlation spectra of DOM within the SSC soil profile indicated that the variations of the phenolic groups were the largest, followed by the carboxylic groups, microbial products, and humified organic materials according to the band changing order of 285 → 365 → 425 → 520 nm. The 2D UV correlation spectra of DOM within the CAC soil profiles determined that the decreasing order of the variations was phenolic groups > carboxylic groups > microbial products according the band changing order of 285 → 365 → 425 nm. The 2D UV correlation spectra of DOM within the PAC soil profile proved that the variations of the phenolic groups were larger than those of the carboxylic groups according to the band changing order of 285 → 365 nm. The 2D UV correlation spectra of DOM within the ASC soil profile demonstrated that the variations of the phenolic groups were larger than those of the other DOM fractions according to the broad cross-peak at 285/365-700 nm.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Wai, Chien M.
Amidoxime-based polymer fibers are considered one of the most promising materials for sequestering uranium from seawater. The high-surface-area polymer fibers containing amidoxime and carboxylate groups synthesized by Oak Ridge National Lab (ORNL-AF1) show very high uranium adsorption capacities known in the literature. Effective elution of uranium and repeated use of the adsorbent are important factors affecting the cost of producing uranium from seawater using this material. Traditional acid leaching of uranium followed by KOH conditioning of the fiber causes chemical changes and physical damage to the ORNL-AF1 adsorbent. Two alkaline solution leaching methods were developed by this project, one usesmore » a highly concentrated (3 M) potassium bicarbonate solution at pH 8.3 and 40 °C; the other uses a mixture of sodium carbonate and hydrogen peroxide at pH 10.4. Both elution methods do not require KOH conditioning prior to reusing the fiber adsorbent. The conditions of eluting uranium from the amidoxime-based adsorbent using these alkaline solutions are confirmed by thermodynamic calculations. The bicarbonate elution method is selective for uranium recovery compared to other elution methods and causes no chemical change to the fiber material based on FTIR spectroscopy« less
Sun, Xiaoli; Hao, Weiqiang; Wang, Junde; Di, Bin; Chen, Qiang; Zhuang, Wei; Yu, Qiang; Zhang, Peipei
2013-08-01
By not explicitly specifying the type of solvent strength model, the features of ladder-like gradient elution were studied based on the general retention time formula that was derived in our previous work. For the case where the solute is eluted at like gradient, we derived the expression that connects the mobile phase composition (phiR), at which the solute is eluted from the column, with the gradient slope (B). It was shown that phiR will increase with the increase of B in this case. For the case where the solute is eluted at the last isocratic segment of the ladder-like gradient, it was proven that the retention time (tR) will correlate linearly with the reciprocal of the gradient slope (1/B) when the initial and final mobile phase compositions are set to be constant. In experiments, by taking biphenyl as the sample, the values of retention time in isocratic and gradient elution were measured on a C18 column by using a mixture of methanol and water as the mobile phase. The experimental values were found to be well consistent with the theoretical values that were calculated from the expressions. These expressions will be helpful to understand the features of the ladder-like gradient in practice.
Ji, Guodong; Sui, Xin
2010-07-15
An ultrasound-enhanced elution system employing water at a temperature of 70 degrees C was used to remedy weathered soils contaminated with severely biodegraded heavy oil (SBHO). The effect of varying the ultrasonic irradiation time from 0 to 1800 s on the elution of SBHO and three characteristic biomarkers (C(26-34) 17alpha 25-norhopanes, C(26-28) TAS, and C(27-29) MTAS) was analyzed using GC/MS, scanning electron microscopy (SEM), and X-ray diffraction (XRD). Elution of the three biomarkers was closely related to the carbon number of the marker. C(26-34) 17alpha 25-norhopanes and C(26-28) TAS species with higher carbon numbers and C(27-29) MTAS species with lower carbon numbers were more readily eluted using sonication times of 1080-1800 s, while smaller TAS homologs were more readily eluted after sonication times of 0-360 s. SEM images of samples treated for longer periods revealed larger "bare patches" on the soil surface. The results of XRD and energy spectroscopy experiments indicated that ultrasound irradiation for 1080 s negatively affected the deposition of CaCO(3), but overall improved the mineral and chemical compositions of treated soils and removal of SBHO. 2010 Elsevier B.V. All rights reserved.
Drug elution from high-dose antibiotic-loaded acrylic cement: a comparative, in vitro study.
Gasparini, Giorgio; De Gori, Marco; Calonego, Giovanni; Della Bora, Tommaso; Caroleo, Benedetto; Galasso, Olimpio
2014-11-01
High-dose antibiotic-loaded acrylic cement (ALAC) is used for managing peri-prosthetic joint infections (PJIs). The marked increase in resistant high-virulence bacteria is drawing the attention of physicians toward alternative antimicrobial formulations loaded into acrylic bone cement. The aim of this in vitro study was to determine the elution kinetics of 14 different high-dose ALACs. All ALAC samples showed a burst release of antibiotics in the first hour, progressively decreasing over time, and elution curves strictly adhered to a nonlinear regression analysis formula. Among aminoglycosides, commonly seen as the most appropriate antibiotics to be loaded into the bone cement, the highest elution rate was that of tobramycin. Among the glycopeptides, a class of antibiotics that should be considered to treat PJIs because of the prevalence of aminoglycoside resistance, vancomycin showed better elution than teicoplanin. Clindamycin, which can be associated with aminoglycosides to prepare ALACs and represents a useful option against the most common pathogens responsible for PJIs, showed the highest absolute and relative elutions among all the tested formulations. A noticeable elution was also detected for colistin, an antibiotic of last resort for treating multidrug-resistant bacteria. The current study demonstrates theoretical advantages in the preparation of ALAC for some antibiotics not routinely used in the clinical setting for PJIs. The use of these antibiotics based on the infecting bacteria sensitivity may represent a useful option for physicians to eradicate PJIs. In vivo testing should be considered in the future to confirm the results of this study. Copyright 2014, SLACK Incorporated.
Identification and Characterization of Memecylon Species Using Isozyme Profiling
Bharathi, T. R.; Sekhar, Shailasree; Geetha, N.; Niranjana, S. R.; Prakash, H. S.
2017-01-01
Background: The protein/isozyme fingerprint is useful in differentiating the species and acts as a biochemical marker for identification and systematic studies of medicinal plant species. Objective: In the present study, protein and isozyme profiles for peroxidase, esterase, acid phosphatase, polyphenol oxidase, alcohol dehydrogenase, and alkaline phosphatase of five species of Memecylon (Melastomataceae), Memecylon umbellatum, Memecylon edule, Memecylon talbotianum, Memecylon malabaricum, and Memecylon wightii were investigated. Materials and Methods: Fresh leaves were used to prepare crude enzyme extract for analyzing the five enzymes isozyme variations. Separation of isozymes was carried out using polyacrylamide gel electrophoresis (PAGE) and the banding patterns of protein were scored. Pair-wise comparisons of genotypes, based on the presence or absence of unique and shared polymorphic products, were used to regenerate similarity coefficients. The similarity coefficients were then used to construct dendrograms, using the unweighted pair group method with arithmetic averages. Results: A total of 50 bands with various Rf values and molecular weight were obtained through PAGE analysis. Among the five Memecylon species, more number of bands was produced in M. wightii and less number of bands was observed in M. edule. The results of similarity indices grouped M. malabaricum and M. wightii in one cluster with 98% similarity and M. umbellatum, M. edule, and M. talbotianum are grouped in another cluster with 79% similarity showing close genetic similarities which is in accordance with the morphological identification of Memecylon species. Conclusion: The protein/isozyme fingerprint is useful in differentiating the species and acts as a biochemical marker for identification of Memecylon species. SUMMARY Biochemical characterization of Memecylon species was evaluated by SDS-PAGE of extracted protein and isozyme profiling on native PAGE.After electrophoresis, each gel was stained with specific stains. Genetic distance relationships were evaluated based on the banding patterns of protein on isozymes.Unique banding pattern of esterase, peroxidase, acid phosphatase, alcohol dehydrogenase and polyphenol oxidase are observed in all the five species of Memecylon, which represent the fingerprint of Memecylon species.SDS-PAGE and isozyme profiling of five Memecylon species revealed that M. malabaricum and M. wightii grouped in one cluster and M. umbellatum, M. edule and M. talbotianum grouped in another cluster showing close genetic similarities which is in accordance with the morphological identification of Memecylon species.This is the first report on the comparison of protein and isozyme profile of five different Memecylon species. Abbreviations Used: SDS-PAGE: Sodium docecyl sulfate polyacrylamide gel electrophoresis; NTSYS PC2: Numerical taxonomy system, version 2.2 for Windows XP, Vista, Win7, Win 8 and Win10 including 64 bit PMID:29263637
Effect of layer thickness on the elution of bulk-fill composite components.
Rothmund, Lena; Reichl, Franz-Xaver; Hickel, Reinhard; Styllou, Panorea; Styllou, Marianthi; Kehe, Kai; Yang, Yang; Högg, Christof
2017-01-01
An increment layering technique in a thickness of 2mm or less has been the standard to sufficiently convert (co)monomers. Bulk fill resin composites were developed to accelerate the restoration process by enabling up to 4mm thick increments to be cured in a single step. The aim of the present study is to investigate the effect of layer thickness on the elution of components from bulk fill composites. The composites ELS Bulk fill, SDR Bulk fill and Venus Bulkfill were polymerized according to the instruction of the manufacturers. For each composite three groups with four samples each (n=4) were prepared: (1) samples with a layer thickness of 2mm; (2) samples with a layer thickness of 4mm and (3) samples with a layer thickness of 6mm. The samples were eluted in methanol and water for 24h and 7 d. The eluates were analyzed by gas chromatography/mass spectrometry (GC/MS). A total of 11 different elutable substances have been identified from the investigated composites. Following methacrylates showed an increase of elution at a higher layer thickness: TEGDMA (SDR Bulk fill, Venus Bulk fill), EGDMA (Venus Bulk fill). There was no significant difference in the elution of HEMA regarding the layer thickness. The highest concentration of TEGDMA was 146μg/mL for SDR Bulk fill at a layer thickness of 6mm after 7 d in water. The highest HEMA concentration measured at 108μg/mL was detected in the methanol eluate of Venus Bulk fill after 7 d with a layer thickness of 6mm. A layer thickness of 4mm or more can lead to an increased elution of some bulk fill components, compared to the elution at a layer thickness of 2mm. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Moses, Jeffrey W; Mehran, Roxana; Nikolsky, Eugenia; Lasala, John M; Corey, Woodrow; Albin, Glenn; Hirsch, Cary; Leon, Martin B; Russell, Mary E; Ellis, Stephen G; Stone, Gregg W
2005-04-19
We sought to investigate the outcomes of paclitaxel-eluting stent implantation in patients with unstable angina or non-ST-segment elevation myocardial infarction undergoing percutaneous coronary intervention (PCI). Whether the paclitaxel-eluting stent is safe and effective in patients with acute coronary syndromes (ACS) is unknown. In the TAXUS-IV trial, 1,314 patients with stable or unstable ischemic syndromes undergoing PCI were randomized to treatment with either the slow-release, polymer-based, paclitaxel-eluting TAXUS stent or a bare-metal EXPRESS stent (Boston Scientific Corp., Natick, Massachusetts). The results were stratified by the acuity of the presenting clinical syndrome. Acute coronary syndromes were present in 450 patients (34.2%), 237 of whom were assigned to paclitaxel-eluting stents and 213 to bare-metal stents. The baseline and procedural characteristics were well matched between the groups. Clinical outcomes at 30 days were similar with both stents. At one-year follow-up, patients with ACS assigned to the paclitaxel-eluting stent compared to the control stent had strikingly lower rates of target lesion revascularization (TLR) (3.9% vs. 16.0%, p < 0.0001) and major adverse cardiac events (11.1 vs. 21.7%, p = 0.002). By multivariate analysis, ACS was an independent predictor of in-stent restenosis in the cohort treated with bare-metal stents (hazard ratio [HR] = 2.03 [95% confidence interval (CI) 1.05 to 3.92], p = 0.035), while among patients randomized to the paclitaxel-eluting stents, ACS was an independent predictor of freedom from restenosis (HR = 0.27 [95% CI 0.08 to 0.97], p = 0.04). The use of the paclitaxel-eluting TAXUS stent was safe in patients with unstable ischemic syndromes, and was associated with marked reduction of ischemia-driven TLR and adverse cardiac events at one year.
ANIONIC EXCHANGE PROCESS FOR THE RECOVERY OF URANIUM AND VANADIUM FROM CARBONATE SOLUTIONS
Bailes, R.H.; Ellis, D.A.; Long, R.S.
1958-12-16
Uranium and vanadium can be economically purified and recovered from non- salt roast carbonate leach liquors by adsorption on a strongly basic anionic exchange resin and subsequent selective elution by one of three alternative methods. Method 1 comprises selectively eluting uranium from the resin with an ammonium sulfate solution followed by eluting vanadium from the resin with either 5 M NaCl, saturated (NH/sub 4/)/sub 2/CO/sub 3/, saturated NaHCO/sub 3/, 1 M NaOH, or saturated S0/sub 2/ solutions. Method II comprises selectively eluting vanadium from the resin with either concentrated NaCl or S0/sub 2/ solutions subsequent to pretreatment of the column with either S0/sub 2/ gas, 1 N HCl, or 0.1 N H/sub 2/8O/sub 4/ followed by eluting uranium from the resin with solutions containing 0.9 M NH/sub 4/Cl or NaCl and 0.1 Cl. Method III comprises flowing the carbonate leac solutlon through a first column of a strongly basic anlonlc exchange resin untll vanadium breakthrough occurs, so that the effluent solution is enriched ln uranium content and the vanadium is chiefly retalned by the resln, absorbing the uranlum from the enriched effluent solution on a second column of a strongly basic anionic exchange resin, pretreating the first column with either 0.1 N HCl, 0.1 H/sub 2/SO/sub 4/, C0/sub 2/ gas, or ammonium sulfate, selectively eluting the vanadlum from the column with saturated S0/sub 2/ solution, pretreatlng the second column with either 0.1 N HCl or S0/sub 2/ gas, selectively eluting residual vanadium from the column with saturated S0/sub 2/ solution, and then eluting the uranium from the column with either 0.1 N HCl and 1 N NaCl orO.l N HCl and 1 N NH/sub 4/Cl.
Error analyses of JEM/SMILES standard products on L2 operational system
NASA Astrophysics Data System (ADS)
Mitsuda, C.; Takahashi, C.; Suzuki, M.; Hayashi, H.; Imai, K.; Sano, T.; Takayanagi, M.; Iwata, Y.; Taniguchi, H.
2009-12-01
SMILES (Superconducting Submillimeter-wave Limb-Emission Sounder) , which has been developed by Japan Aerospace Exploration Agency (JAXA) and National Institute of Information and Communications Technology (NICT), is planned to be launched in September, 2009 and will be on board the Japanese Experiment Module (JEM) of the International Space Station (ISS). The SMILES measures the atmospheric limb emission from stratospheric minor constituents in 640 GHz band. Target species on L2 operational system are O3, ClO, HCl, HNO3, HOCl, CH3CN, HO2, BrO, and O3 isotopes (18OOO, 17OOO and O17OO). The SMILES carries 4 K cooled Superconductor-Insulator-Superconductor mixers to carry out high-sensitivity observations. In sub-millimeter band, water vapor absorption is an important factor to decide the tropospheric and stratospheric brightness temperature. The uncertainty of water vapor absorption influences the accuracy of molecular vertical profiles. Since the SMILES bands are narrow and far from H2O lines, it is a good approximation to assume this uncertainly as linear function of frequency. We include 0th and 1st coefficients of ‘baseline’ function, not water vapor profile, in state vector and retrieve them to remove influence of the water vapor uncertainty. We performed retrieval simulations using spectra computed by L2 operatinal forward model for various H2O conditions (-/+ 5, 10% difference between true profile and a priori profile in the stratosphere and -/+ 10, 20% one in the troposphere). The results show that the incremental errors of molecules are smaller than 10% of measurements errors when height correlation of baseline coefficients and temperature are assumed to be 10 km. In conclusion, the retrieval of the baseline coefficients effectively suppresses profile error due to bias of water vapor profile.
Alfonso, Fernando; Pérez-Vizcayno, María José; García Del Blanco, Bruno; García-Touchard, Arturo; Masotti, Mónica; López-Minguez, José R; Iñiguez, Andrés; Zueco, Javier; Velazquez, Maite; Cequier, Angel; Lázaro-García, Rosa; Martí, Vicens; Moris, César; Urbano-Carrillo, Cristobal; Bastante, Teresa; Rivero, Fernando; Cárdenas, Alberto; Gonzalo, Nieves; Jiménez-Quevedo, Pilar; Fernández, Cristina
2016-02-15
Treatment of patients with in-stent restenosis (ISR) remains a challenge. This study sought to compare the efficacy of everolimus-eluting stents (EESs) and drug-eluting balloons (DEBs) with paclitaxel in patients with ISR. A pooled analysis of the Restenosis Intra-Stent of Drug-Eluting Stents: Drug-Eluting Balloon vs Everolimus-Eluting Stent (RIBS IV) and Restenosis Intra-Stent of Bare-Metal Stents: Drug-Eluting Balloon vs Everolimus-Eluting Stent (RIBS V) randomized trials was performed using patient-level data. In both trials, EESs were compared with DEBs in patients with ISR (RIBS V included 189 patients with bare-metal ISR; RIBS IV included 309 patients with drug-eluting ISR). Inclusion and exclusion criteria were identical in both trials. A total of 249 patients were allocated to EES and 249 to DEB. Clinical follow-up at 1 year was obtained in all (100%) patients and late angiography (median 249 days) in 91% of eligible patients. Compared with patients treated with DEBs, patients treated with EESs obtained better short-term results (postprocedural minimal lumen diameter 2.28 ± 0.5 vs 2.12 ± 0.4 mm, p <0.0001). At follow-up, patients treated with EESs had larger in-segment minimal lumen diameter (primary end point 2.16 ± 0.7 vs 1.88 ± 0.6 mm, p <0.0001; absolute mean difference 0.28 mm; 95% confidence interval [CI] 0.16 to 0.40) and net lumen gain (1.33 ± 0.6 vs 1.00 ± 0.7 mm, p <0.0001) and had lower %diameter stenosis (19 ± 21% vs 28 ± 22%, p <0.0001) and binary restenosis rate (8.7% vs 15.7%, p = 0.02). Consistent results were observed in the in-lesion analysis. No interactions were found between the underlying stent type and treatment effects. At 1-year clinical follow-up, the composite of cardiac death, myocardial infarction, and target vessel revascularization was significantly reduced in the EES arm (8.8% vs 14.5%, p = 0.03; hazard ratio 0.59, 95% CI 0.31 to 0.94) mainly driven by a lower need for target vessel revascularization (6% vs 12.4%, p = 0.01, hazard ratio 0.46, 95% CI 0.25 to 0.86). This pooled analysis of the RIBS IV and RIBS V randomized trials demonstrates the superiority of EES over DEB in the treatment of patients with ISR. Copyright © 2016 Elsevier Inc. All rights reserved.
Selective enrichment and desalting of hydrophilic peptides using graphene oxide.
Jiang, Miao; Qi, Linyu; Liu, Peiru; Wang, Zijun; Duan, Zhigui; Wang, Ying; Liu, Zhonghua; Chen, Ping
2016-08-01
The wide variety and low abundance of peptides in tissue brought great difficulties to the separation and identification of peptides, which is not in favor of the development of peptidomics. RP-HPLC, which could purify small molecules based on their hydrophobicity, has been widely used in the separation and enrichment of peptide due to its fast, good reproducibility and high resolution. However, RP-HPLC requires the instrument and expensive C18 column and its sample capacity is also limited. Recently, graphene oxide has been applied to the adsorption of amino acids. However, the enrichment efficiency and selectivity of graphene oxide for peptides remain unclear. In this study, the adsorption efficiency and selectivity of graphene oxide and RP-C18 matrix were compared on trypsinized α-actin and also on tissue extracts from pituitary gland and hippocampus. For α-actin, there exhibit similar elution peaks for total trypsinized products and those adsorpted by GO and C18 matrix. But peptides adsorbed by GO showed the higher hydrophilic peaks than which adsorbed by C18 matrix. The resulted RP-HPLC profile showed that most of peptides enriched by graphene oxide were eluted at low concentration of organic solvent, while peptides adsorbed by RP-C18 matrix were mostly eluted at relatively high concentration. Moreover, mass spectrometry analysis suggested that, in pituitary sample, there were 495 peptides enriched by graphene oxide, 447 peptides enriched by RP-C18 matrix while in hippocampus sample 333 and 243 peptides respectively. The GRAVY value analysis suggested that the graphene oxide has a stronger adsorption for highly hydrophilic peptides compared to the RP-C18 matrix. Furthermore, the combination of these two methods could notably increase the number of identification peptides but also the number of predicted protein precursors. Our study provided a new thought to the role of graphene oxide during the enrichment of peptides from tissue which should be useful for peptidomics study. Copyright © 2016 Elsevier B.V. All rights reserved.
Kemp, Brian M; Winters, Misa; Monroe, Cara; Barta, Jodi Lynn
2014-01-01
The success in recovering genetic profiles from aged and degraded biological samples is diminished by fundamental aspects of DNA extraction, as well as its long-term preservation, that are not well understood. While numerous studies have been conducted to determine whether one extraction method was superior to others, nearly all of them were initiated with no knowledge of the actual starting DNA quantity in the samples prior to extraction, so they ultimately compared the outcome of all methods relative to the best. Using quantitative PCR to estimate the copy count of synthetic standards before (i.e., "copies in") and after (i.e., "copies out") purification by the Qiagen MinElute PCR Purification Kit, we documented DNA loss within a pool of 16 different-sized fragments ranging from 106 to 409 bp in length, corresponding to those targeted by the PowerPlex 16 System (Promega, Madison, WI). Across all standards from 10(4) to 10(7) copies/μL, loss averaged between 21.75% and 60.56% (mean, 39.03%), which is not congruent with Qiagen's claim that 80% of 70 bp to 4 kb fragments are retained using this product (i.e., 20% loss). Our study also found no clear relationship either between DNA strand length and retention or between starting copy number and retention. This suggests that there is no molecule bias across the MinElute column membrane and highlights the need for manufacturers to clearly and accurately describe on what their claims are based, and should also encourage researchers to document DNA retention efficiencies of their own methods and protocols. Understanding how and where to reduce loss of molecules during extraction and purification will serve to generate clearer and more accurate data, which will enhance the utility of ancient and low-copy-number DNA as a tool for closing forensic cases or in reconstructing the evolutionary history of humans and other organisms.
Xu, Zhihao; Li, Jason; Zhou, Joe X
2012-01-01
Aggregate removal is one of the most important aspects in monoclonal antibody (mAb) purification. Cation-exchange chromatography (CEX), a widely used polishing step in mAb purification, is able to clear both process-related impurities and product-related impurities. In this study, with the implementation of quality by design (QbD), a process development approach for robust removal of aggregates using CEX is described. First, resin screening studies were performed and a suitable CEX resin was chosen because of its relatively better selectivity and higher dynamic binding capacity. Second, a pH-conductivity hybrid gradient elution method for the CEX was established, and the risk assessment for the process was carried out. Third, a process characterization study was used to evaluate the impact of the potentially important process parameters on the process performance with respect to aggregate removal. Accordingly, a process design space was established. Aggregate level in load is the critical parameter. Its operating range is set at 0-3% and the acceptable range is set at 0-5%. Equilibration buffer is the key parameter. Its operating range is set at 40 ± 5 mM acetate, pH 5.0 ± 0.1, and acceptable range is set at 40 ± 10 mM acetate, pH 5.0 ± 0.2. Elution buffer, load mass, and gradient elution volume are non-key parameters; their operating ranges and acceptable ranges are equally set at 250 ± 10 mM acetate, pH 6.0 ± 0.2, 45 ± 10 g/L resin, and 10 ± 20% CV respectively. Finally, the process was scaled up 80 times and the impurities removal profiles were revealed. Three scaled-up runs showed that the size-exclusion chromatography (SEC) purity of the CEX pool was 99.8% or above and the step yield was above 92%, thereby proving that the process is both consistent and robust.
NASA Astrophysics Data System (ADS)
Yedukondalu, N.; Kunduru, Lavanya; Roshan, S. C. Rakesh; Sainath, M.
2018-04-01
Assessment of band gaps for nine alkaline-earth chalcogenides namely MX (M = Ca, Sr, Ba and X = S, Se Te) compounds are reported using Tran Blaha-modified Becke Johnson (TB-mBJ) potential and its new parameterization. From the computed electronic band structures at the equilibrium lattice constants, these materials are found to be indirect band gap semiconductors at ambient conditions. The calculated band gaps are improved using TB-mBJ and its new parameterization when compared to local density approximation (LDA) and Becke Johnson potentials. We also observe that TB-mBJ new parameterization for semiconductors below 7 eV reproduces the experimental trends very well for the small band gap semiconducting alkaline-earth chalcogenides. The calculated band profiles look similar for MX compounds (electronic band structures are provided for BaS for representation purpose) using LDA and new parameterization of TB-mBJ potentials.
Johanson, Helene C; Hyland, Valentine; Wicking, Carol; Sturm, Richard A
2009-04-01
We describe here a method for DNA elution from buccal cells and whole blood both collected onto Whatman FTA technology, using methanol fixation followed by an elution PCR program. Extracted DNA is comparable in quality to published Whatman FTA protocols, as judged by PCR-based genotyping. Elution of DNA from the dried sample is a known rate-limiting step in the published Whatman FTA protocol; this method enables the use of each 3-mm punch of sample for several PCR reactions instead of the standard, one PCR reaction per sample punch. This optimized protocol therefore extends the usefulness and cost effectiveness of each buccal swab sample collected, when used for nucleic acid PCR and genotyping.
NASA Technical Reports Server (NTRS)
Salas, W. A.; Ranson, K. J.; Rock, B. N.; Moss, D. M.
1991-01-01
The diurnal characteristics of microwave dielectric properties and water potential of two conifer species were investigated in July and September, 1990. P-band and C-band radial dielectric profiles of hemlock and red spruce, as well as hemlock diurnal water potential and dielectric profiles, are presented. The resulting radial dielectric profiles matched the regions of the functional sapwood (water transport component of the active xylem) in both species such that the sapwood was characterized by a higher dielectric than the bark and heartwood tissues. This is probably due to characteristic differences in the water content of each tissue. As the hemlocks progressed through their diurnal water potential pattern, the dielectric profile remained static until mid-afternoon. As the tension in the water column relaxed (2 to 3 bars) the dielectric constant decreased by 30 to 40 percent. There are several possible explanations for this phenomenon, and these may relate to the dependency of the dielectric measurements on temperature, salinity, and volumetric water content.
UV resonance Raman finds peptide bond-Arg side chain electronic interactions.
Sharma, Bhavya; Asher, Sanford A
2011-05-12
We measured the UV resonance Raman excitation profiles and Raman depolarization ratios of the arginine (Arg) vibrations of the amino acid monomer as well as Arg in the 21-residue predominantly alanine peptide AAAAA(AAARA)(3)A (AP) between 194 and 218 nm. Excitation within the π → π* peptide bond electronic transitions result in UVRR spectra dominated by amide peptide bond vibrations. The Raman cross sections and excitation profiles indicate that the Arg side chain electronic transitions mix with the AP peptide bond electronic transitions. The Arg Raman bands in AP exhibit Raman excitation profiles similar to those of the amide bands in AP which are conformation specific. These Arg excitation profiles distinctly differ from the Arg monomer. The Raman depolarization ratios of Arg in monomeric solution are quite simple with ρ = 0.33 indicating enhancement by a single electronic transition. In contrast, we see very complex depolarization ratios of Arg in AP that indicate that the Arg residues are resonance enhanced by multiple electronic transitions.
NASA Technical Reports Server (NTRS)
Cravens, T. E.; Gerard, J.-C.; Lecompte, M.; Stewart, A. I.; Rusch, D. W.
1985-01-01
The ultraviolet nitric oxide spectrometer (UVNO) experiment on the Atmosphere Explorer D (AE-D) satellite measured thermospheric nitric oxide during the winter of 1974-1975 using resonant fluorescence from the 1-0 gamma band of the molecule. Almost complete latitude coverage was obtained, but the observations were confined to morning local times close to 0900. The 1-0 gamma band intensity profiles measured by the instrument were inverted to provide vertical profiles of the NO number density between about 90 and 200 km. Typically, the measured NO concentrations reached a maximum between altitudes of 100 and 110 km, and more NO was observed at higher latitudes than at low latitudes, in agreement with previous observational studies. The shape of the NO profile was also found to be a function of latitude, with a plateau appearing in the profile near 130 km for low latitudes and mid-latitudes in the winter hemisphere.
Laser heterodyne system for obtaining height profiles of minor species in the atmosphere
NASA Technical Reports Server (NTRS)
Jain, S. L.; Saha, A. K.
1986-01-01
An infrared laser heterodyne system for obtaining height profiles of minor constituents of the atmosphere was developed and erected. A brief discription of the system is given. The system consists of a tunable CO2 waveguide laser in the 9 to 11 micrometer band, that is used as a local oscillator and a heliostat that follows the sun and brings in solar radiation, that is mixed with the laser beam in a high speed liquid nitrogen cooled mercury cadmium telluride detector. The detected signal is analysed in a RF spectrum analyser that allows tracing absorption line profiles. Absorption lines of a number of minor constituents in the troposphere and stratosphere, such as O3, NH3, H2O, SO2, ClO, N2O, are in the 9 to 11 micrometer band and overlap with that of CO2 laser range. The experimental system has been made operational and trial observations taken. Current measurements are limited to ozone height profiles. Results are presented.
Observational analysis of the well-correlated diffuse bands: 6196 and 6614 Å
NASA Astrophysics Data System (ADS)
Krełowski, J.; Galazutdinov, G. A.; Bondar, A.; Beletsky, Y.
2016-08-01
We confirm, using spectra from seven observatories, that the diffuse bands 6196 and 6614 are very tightly correlated. However, their strength ratio is not constant as well as profile shapes. Apparently, the two interstellar features do not react in unison to the varying physical conditions of different interstellar clouds.
Taga, C; Tsuji, M; Nakajima, T
1989-05-01
A reversed phase HPLC method with fluorometric detection for the analysis of beta-phenylethylamine has been developed using p-methoxyphenylethylamine as an internal standard. Two columns, containing 200 microL of Dowex 50-X8 and Amberlite CG-50 respectively, were used to prepare a fraction containing beta-phenylethylamine. The recoveries of beta-phenylethylamine and p-methoxyphenylethylamine were 53.9 +/- 9.4% and 68.1 +/- 12.4%, respectively, and elution profile of p-methoxyphenylethylamine was sufficiently well correlated with that of beta-phenylethylamine. Regional distributions of beta-phenylethylamine in rat and mouse brains were determined. The highest concentrations were found in hypothalamus and hippocampus in both animals.
Effects of melting layer on Ku-band signal depolarization
NASA Astrophysics Data System (ADS)
Sarkar, Thumree; Das, Saurabh; Maitra, Animesh
2014-09-01
Propagation effects on Ku-band over an earth-space path is carried out at Kolkata, India, a tropical location, by receiving a Ku-band signal with horizontal plane polarization transmitted from the geostationary satellite NSS-6 (at 95°E). The amplitude of co-polar attenuation has been monitored along with the measurements of rain rate, rain drop size distribution and height profile of rain rate. The cross-polar enhancement of the signal is also monitored by receiving the same signal in orthogonal direction with another identical receiver. The experimental observations are used to study the effect of melting layer on both co-polar attenuation and cross-polar enhancement for the rain events observed during 2012-2013. Melting layer is indicated by the bright band signature in vertical profile of rain rate. The ground based drop size measurements indicate that the stratiform rain has more number of small drops whereas convective rain composed of large rain drops. The results indicate that the depolarization due to melting layer is more dominant compared to that due to the drop deformation mechanism at low rain rates.
Subclasses of immunoglobulins and autoantibodies in autoimmune diseases.
Outschoorn, I; Rowley, M J; Cook, A D; Mackay, I R
1993-01-01
The differing capacity of subclasses of IgG to bind to protein A and protein G was used in a sequential affinity purification procedure to examine immunoglobulin isotypes and subclasses in autoimmune disease. The utility of the procedure is that affinity-purified fractions containing particular isotypes and subclasses of immunoglobulin can be analyzed for their content of autoantibodies using standard techniques. For each of four autoimmune diseases studied, chronic active hepatitis, Sjogren's syndrome, primary biliary cirrhosis, and rheumatoid arthritis, there were characteristic protein elution profiles and the various disease-specific autoantibodies showed preferential distributions among the isotypes and subclasses. Moreover there was not an absolute correlation between an increased level of a particular subclass and the occurrence of antibodies of that subclass. The occurrence of highly disease-specific immunoglobulin subclass profiles suggests that the hypergammaglobulinemia associated with autoimmunity cannot be attributed entirely to polyclonal B-cell activation. Rather, there are disease-specific alterations in isotype subclass switching which may reflect different cytokine-dependent influences on autoimmune B cells and their products.
Turner, Dee A; Goodpaster, John V
2011-07-01
Biodegradation can result in selective removal of many of the compounds required for the identification of an ignitable liquid. In this study, the effects of microbial degradation on tiki torch fuel, lamp oil, and turpentine are reported. Samples of soil spiked with 20 μL of the liquids were stored at room temperature for up to 7 days. The ignitable liquids were then recovered using passive headspace concentration onto charcoal strips followed by solvent elution using pentane. Microbial degradation of tiki torch fuel resulted in the loss of the n-alkanes relative to the branched alkanes. Changes in the profile of the lamp oil were minor due to the highly branched nature of its alkanes. Microbial degradation of turpentine resulted in the selective loss of limonene and o-cymene. Overall, significant degradation by microbial action could result in the inability to identify the presence of an ignitable liquid or misclassify the ignitable liquid found. © 2011 American Academy of Forensic Sciences.
Jahnen, W; Batterham, M P; Clarke, A E; Moritz, R L; Simpson, R J
1989-05-01
S-Gene-associated glycoproteins (S-glycoproteins) from styles of Nicotiana alata, identified by non-equilibrium two-dimensional electrophoresis, were purified by cation exchange fast protein liquid chromatography with yields of 0.5 to 8 micrograms of protein per style, depending on the S-genotype of the plant. The method relies on the highly basic nature of the S-glycoproteins. The elution profiles of the different S-glycoproteins from the fast protein liquid chromatography column were characteristic of each S-glycoprotein, and could be used to establish the S-genotype of plants in outbreeding populations. In all cases, the S-genotype predicted from the style protein profile corresponded to that predicted from DNA gel blot analysis using S-allele-specific DNA probes and to that established by conventional breeding tests. Amino-terminal sequences of five purified S-glycoproteins showed a high degree of homology with the previously published sequences of N. alata and Lycopersicon esculentum S-glycoproteins.
Jin, Hui; Lao, Yong Min; Zhou, Jin; Zhang, Huai Jin; Cai, Zhong Hua
2017-03-10
A simple ultra-high-pressure liquid chromatography (UHPLC) method for rapidly and simultaneously identifying thirteen carotenoids in Haematococcus pluvialis was developed in this study. The method is capable of effectively separating two astaxanthin isomers, two ζ-carotene isomers, and three phytoene isomers on two simple C18 columns within 9 and 12min only by using methanol and acetonitrile, respectively. To our best knowledge, this is the rapidest method for these carotenoid isomers, currently. Using this method, carotenoid profiling in the astaxanthin-accumulating H. pluvialis under environmental stresses was successfully carried out. Results indicated that carotenoid biosynthesis was differentially perturbed by environmental stresses, indicating that this simple and rapid method is suitable to not only bacterial but also algal samples, with potential applications for a wide range of samples from plant to animal. Finally, possible reasons for the elution order of carotenoids were studied. Copyright © 2017 Elsevier B.V. All rights reserved.
Vold, Barbara S.
1973-01-01
Differences between the transfer ribonucleic acid (tRNA) of spores and exponentially growing cells of Bacillus subtilis 168 were compared by co-chromatography on reversed-phase column RPC-5. This system gave excellent resolution of isoaccepting species in 1 to 2 hr using a 200-ml gradient. Two methods were used to extract spore tRNAs, a procedure using a Braun homogenizer and a pretreatment with dithiothreitol followed by lysis with lysozyme. Where changes were observed, column elution profiles of spore tRNAs were independent of the extraction method used. Three kinds of changes between the profiles of vegetative cell tRNA and spore tRNA were observed: (i) no change; phe-, val-, ala-, asp-, ileu-, pro-, met-, fmet-, and his-tRNAs, (ii) a change in the ratio of existing peaks; gly-, tyr-, leu-, ser-, thr-, aspn-, and arg-tRNAs, and (iii) the appearance or disappearance of unique peaks; lys-, glu-, and trp-tRNAs. PMID:4632322
Information retrieval from wide-band meteorological data - An example
NASA Technical Reports Server (NTRS)
Adelfang, S. I.; Smith, O. E.
1983-01-01
The methods proposed by Smith and Adelfang (1981) and Smith et al. (1982) are used to calculate probabilities over rectangles and sectors of the gust magnitude-gust length plane; probabilities over the same regions are also calculated from the observed distributions and a comparison is also presented to demonstrate the accuracy of the statistical model. These and other statistical results are calculated from samples of Jimsphere wind profiles at Cape Canaveral. The results are presented for a variety of wavelength bands, altitudes, and seasons. It is shown that wind perturbations observed in Jimsphere wind profiles in various wavelength bands can be analyzed by using digital filters. The relationship between gust magnitude and gust length is modeled with the bivariate gamma distribution. It is pointed out that application of the model to calculate probabilities over specific areas of the gust magnitude-gust length plane can be useful in aerospace design.
Magnetospectroscopy of double HgTe/CdHgTe quantum wells
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bovkun, L. S.; Krishtopenko, S. S.; Ikonnikov, A. V., E-mail: antikon@ipmras.ru
2016-11-15
The magnetoabsorption spectra in double HgTe/CdHgTe quantum wells (QWs) with normal and inverted band structures are investigated. The Landau levels in symmetric QWs with a rectangular potential profile are calculated based on the Kane 8 × 8 model. The presence of a tunnel-transparent barrier is shown to lead to the splitting of states and “doubling” of the main magnetoabsorption lines. At a QW width close to the critical one the presence of band inversion and the emergence of a gapless band structure, similar to bilayer graphene, are shown for a structure with a single QW. The shift of magnetoabsorption linesmore » as the carrier concentration changes due to the persistent photoconductivity effect associated with a change in the potential profile because of trap charge exchange is detected. This opens up the possibility for controlling topological phase transitions in such structures.« less
G-Band Vapor Radiometer Profiler (GVRP) Handbook
DOE Office of Scientific and Technical Information (OSTI.GOV)
Caddeau, MP
2010-06-23
The G-Band Vapor Radiometer Profiler (GVRP) provides time-series measurements of brightness temperatures from 15 channels between 170 and 183.310 GHz. Atmospheric emission in this spectral region is primarily due to water vapor, with some influence from liquid water. Channels between 170.0 and 176.0 GHz are particularly sensitive to the presence of liquid water. The sensitivity to water vapor of the 183.31-GHz line is approximately 30 times higher than at the frequencies of the two-channel microwave radiometer (MWR) for a precipitable water vapor (PWV) amount of less than 2.5 mm. Measurements from the GVRP instrument are therefore especially useful during low-humiditymore » conditions (PWV < 5 mm). In addition to integrated water vapor and liquid water, the GVRP can provide low-resolution vertical profiles of water vapor in very dry conditions.« less
Wang, Zhi-Guo; Chen, Zeng-Ping; Gong, Fan; Wu, Hai-Long; Yu, Ru-Qin
2002-05-01
The chromatographic peak located inside another peak in the time direction is called an embedded or inner peak in contradistinction with the embedding peak, which is called an outer peak. The chemical components corresponding to inner and outer peaks are called inner and outer components, respectively. This special case of co-eluting chromatograms was investigated using chemometric approaches taking GC-MS as an example. A novel method, named inner chromatogram projection (ICP), for resolution of GC-MS data with embedded chromatographic peaks is derived. Orthogonal projection resolution is first utilized to obtain the chromatographic profile of the inner component. Projection of the two-way data matrix columnwise-normalized along the time direction to the normalized profile of the inner component found is subsequently performed to find the selective m/z points, if they exist, which represent the chromatogram of the outer component by itself. With the profiles obtained, the mass spectra can easily be found by means of a least-squares procedure. The results for both simulated data and real samples demonstrate that the proposed method is capable of achieving satisfactory resolution performance not affected by the shapes of chromatograms and the relative positions of the components involved.
Development of softcopy environment for primary color banding visibility assessment
NASA Astrophysics Data System (ADS)
Min, Byungseok; Pizlo, Zygmunt; Allebach, Jan P.
2008-01-01
Fine-pitch banding is one of the most unwanted artifacts in laser electrophotographic (EP) printers. It is perceived as a quasiperiodic fluctuation in the process direction. Therefore, it is essential for printer vendors to know how banding is perceived by humans in order to improve print quality. Monochrome banding has been analyzed and assessed by many researchers; but there is no literature that deals with the banding of color laser printers as measured from actual prints. The study of color banding is complicated by the fact that the color banding signal is physically defined in a three-dimensional color space, while banding perception is described in a one-dimensional sense such as more banding or less banding. In addition, the color banding signal arises from the independent contributions of the four primary colorant banding signals. It is not known how these four distinct signals combine to give rise to the perception of color banding. In this paper, we develop a methodology to assess the banding visibility of the primary colorant cyan based on human visual perception. This is our first step toward studying the more general problem of color banding in combinations of two or more colorants. According to our method, we print and scan the cyan test patch, and extract the banding profile as a one dimensional signal so that we can freely adjust the intensity of banding. Thereafter, by exploiting the pulse width modulation capability of the laser printer, the extracted banding profile is used to modulate a pattern consisting of periodic lines oriented in the process direction, to generate extrinsic banding. This avoids the effect of the halftoning algorithm on the banding. Furthermore, to conduct various banding assessments more efficiently, we also develop a softcopy environment that emulates a hardcopy image on a calibrated monitor, which requires highly accurate device calibration throughout the whole system. To achieve the same color appearance as the hardcopy, we perform haploscopic matching experiments that allow each eye to independently adapt to different viewing conditions; and we find an appearance mapping function in the adapted XYZ space. Finally, to validate the accuracy of the softcopy environment, we conduct a banding matching experiment at three different banding levels by the memory matching method, and confirm that our softcopy environment produces the same banding perception as the hardcopy. In addition, we perform two more separate psychophysical experiments to measure the differential threshold of the intrinsic banding in both the hardcopy and softcopy environments, and confirm that the two thresholds are statistically identical. The results show that with our target printer, human subjects can see a just noticeable difference with a 9% reduction in the banding magnitude for the cyan colorant.
NASA Astrophysics Data System (ADS)
Moriondo, G.; Baffa, C.; Casertano, S.; Chincarini, G.; Gavazzi, G.; Giovanardi, C.; Hunt, L. K.; Pierini, D.; Sperandio, M.; Trinchieri, G.
1999-05-01
We present near-infrared, H-band (1.65 $() μm), surface photometry of 174 spiral galaxies in the area of the Pisces-Perseus supercluster. The images, acquired with the ARNICA camera mounted on various telescopes, are used to derive radial profiles of surface brightness, ellipticities, and position angles, together with global parameters such as H-band magnitudes and diameters Radial profiles in tabular form and images FITS files are also available upon request from gmorio@arcetri.astro.it.}. The mean relation between H-band isophotal diameter D_{21.5} and the B-band D25 implies a B-H color of the outer disk bluer than 3.5; moreover, D_{21.5}/D25 depends on (global) color and absolute luminosity. The correlations among the various photometric parameters suggest a ratio between isophotal radius D_{21.5}/2 and disk scale length of ~ m3.5 and a mean disk central brightness ~ meq 17.5 H-mag arcsec^{-2}. We confirm the trend of the concentration index C31$ with absolute luminosity and, to a lesser degree, with morphological type. We also assess the influence of non-axisymmetric structures on the radial profiles and on the derived parameters. Based on observations at the TIRGO, NOT, and VATT telescopes. TIRGO (Gornergrat, CH) is operated by CAISMI-CNR, Arcetri, Firenze. NOT (La Palma, Canary Islands) is operated by NOTSA, the Nordic Observatory Scientific Association. VATT (Mt. Graham, Az) is operated by VORG, the Vatican Observatory Research Group Table 3 and Fig. 4 are only available in electronic form at the CDS via anonymous ftp to cdsarc.u-strasbg.fr (130.79.128.5) or via http://cdsweb.u-strasbg.fr/Abstract.html.
Effects of Agronomic Treatments on Structure and Function of Ammonia-Oxidizing Communities
Phillips, Carol J.; Harris, Dave; Dollhopf, Sherry L.; Gross, Katherine L.; Prosser, James I.; Paul, Eldor A.
2000-01-01
The aim of this study was to determine the effects of different agricultural treatments and plant communities on the diversity of ammonia oxidizer populations in soil. Denaturing gradient gel electrophoresis (DGGE), coupled with specific oligonucleotide probing, was used to analyze 16S rRNA genes of ammonia oxidizers belonging to the β subgroup of the division Proteobacteria by use of DNA extracted from cultivated, successional, and native deciduous forest soils. Community profiles of the different soil types were compared with nitrification rates and most-probable-number (MPN) counts. Despite significant variation in measured nitrification rates among communities, there were no differences in the DGGE banding profiles of DNAs extracted from these soils. DGGE profiles of DNA extracted from samples of MPN incubations, cultivated at a range of ammonia concentrations, showed the presence of bands not amplified from directly extracted DNA. Nitrosomonas-like bands were seen in the MPN DNA but were not detected in the DNA extracted directly from soils. These bands were detected in some samples taken from MPN incubations carried out with medium containing 1,000 μg of NH4+-N ml−1, to the exclusion of bands detected in the native DNA. Cell concentrations of ammonia oxidizers determined by MPN counts were between 10- and 100-fold lower than those determined by competitive PCR (cPCR). Although no differences were seen in ammonia oxidizer MPN counts from the different soil treatments, cPCR revealed higher numbers in fertilized soils. The use of a combination of traditional and molecular methods to investigate the activities and compositions of ammonia oxidizers in soil demonstrates differences in fine-scale compositions among treatments that may be associated with changes in population size and function. PMID:11097922
Alfonso, Fernando; Pérez-Vizcayno, María José; García Del Blanco, Bruno; García-Touchard, Arturo; López-Mínguez, José-Ramón; Masotti, Mónica; Zueco, Javier; Melgares, Rafael; Mainar, Vicente; Moreno, Raul; Domínguez, Antonio; Sanchís, Juan; Bethencourt, Armando; Moreu, José; Cequier, Angel; Martí, Vicens; Otaegui, Imanol; Bastante, Teresa; Gonzalo, Nieves; Jiménez-Quevedo, Pilar; Cárdenas, Alberto; Fernández, Cristina
2016-07-01
Treatment of patients with drug-eluting stent (DES) in-stent restenosis (ISR) is more challenging than that of patients with bare-metal stent ISR. However, the results of everolimus-eluting stents (EES) in these distinct scenarios remain unsettled. A pooled analysis of the RIBS IV (Restenosis Intra-Stent of Drug-Eluting Stents: Paclitaxel-Eluting Balloon vs Everolimus-Eluting Stent) and RIBS V (Restenosis Intra-Stent of Bare Metal Stents: Paclitaxel-Eluting Balloon vs Everolimus-Eluting Stent) randomized trials was performed using patient-level data to compare the efficacy of EES in bare-metal stent ISR and DES-ISR. Inclusion and exclusion criteria were identical in both trials. Results of 94 patients treated with EES for bare-metal stent ISR were compared with those of 155 patients treated with EES for DES-ISR. Baseline characteristics were more adverse in patients with DES-ISR, although they presented later and more frequently with a focal pattern. After intervention, minimal lumen diameter (2.22±0.5 versus 2.38±0.5 mm, P=0.01) was smaller in the DES-ISR group. Late angiographic findings (89.3% of eligible patients), including minimal lumen diameter (2.03±0.7 versus 2.36±0.6 mm, P<0.001) and diameter stenosis (23±22 versus 13±17%, P<0.001) were poorer in patients with DES-ISR. Results were consistent in the in-segment and in-lesion analyses. On multiple linear regression analysis, minimal lumen diameter at follow-up remained significantly smaller in patients with DES-ISR. Finally, at 1-year clinical follow-up (100% of patients), mortality (2.6 versus 0%, P<0.01) and need for target vessel revascularization (8 versus 2%, P=0.03) were higher in the DES-ISR group. This patient-level pooled analysis of the RIBS IV and RIBS V randomized clinical trials suggests that EES provide favorable outcomes in patients with ISR. However, the results of EES are less satisfactory in patients with DES-ISR than in those with bare-metal stent ISR. URL: http://www.clinicaltrials.gov. Unique identifiers: NCT01239953 and NCT01239940. © 2016 American Heart Association, Inc.
NASA Astrophysics Data System (ADS)
Noll, Stefan
2016-07-01
Rotational temperatures derived from hydroxyl (OH) line emission are frequently used to study atmospheric temperatures at altitudes of about 87 km. While the measurement only requires intensities of a few bright lines of an OH band, the interpretation can be complicated. Ground-based temperatures are averages for the entire, typically 8 km wide emission layer. Variations in the rotational temperature are then caused by changes of the kinetic temperature and the OH emission profile. The latter can also be accompanied by differences in the layer-averaged efficiency of the thermalisation of the OH rotational level populations. Since this especially depends on the frequency of collisions with O_2, which is low at high altitudes, the non-local thermodynamic equilibrium (non-LTE) contribution to the measured temperatures can be significant and variable. In order to understand the impact of the different sources of OH rotational temperature variations from time scales of hours to a solar cycle, we have studied spectra from the astronomical echelle spectrographs X-shooter and UVES located at Cerro Paranal in Chile. While the X-shooter data spanning 3.5 years allowed us to measure temperatures for 25 OH and two O_2 bands, the UVES spectra cover no more than 10 OH bands simultaneously but a period of about 15 years. These data have been complemented by kinetic temperature and OH and O_2 emission profiles from the multi-channel radiometer SABER on the TIMED satellite. Taking the O_2 and SABER kinetic temperatures as reference and considering the different band-dependent emission profiles, we could evaluate the contribution of non-LTE effects to the measured OH rotational temperatures depending on line set, band, and time. Non-LTE contributions are significant for most bands and can exceed 10 K. The amplitudes of their average nocturnal and seasonal variation are of the order of 1 to 2 K.
Atmospheric pressure and temperature profiling using near IR differential absorption lidar
NASA Technical Reports Server (NTRS)
Korb, C. L.; Schwemmer, G. K.; Dombrowski, M.; Weng, C. Y.
1983-01-01
The present investigation is concerned with differential absorption lidar techniques for remotely measuring the atmospheric temperature and pressure profile, surface pressure, and cloud top pressure-height. The procedure used in determining the pressure is based on the conduction of high-resolution measurements of absorption in the wings of lines in the oxygen A band. Absorption with respect to these areas is highly pressure sensitive in connection with the mechanism of collisional line broadening. The method of temperature measurement utilizes a determination of the absorption at the center of a selected line in the oxygen A band which originates from a quantum state with high ground state energy.
A geodemographic analysis of the Denplan patient population in the North West Region.
Tickle, M; Blinkhorn, A S; Brown, P J; Matthews, R
2000-11-11
To provide a preliminary descriptive investigation of Denplan patients in the North West Region, by plotting the age/gender and payment banding distribution, and to identify the area types where Denplan patients live and the areas in the North West Region where Denplan practices are most likely to thrive. North West Region of England The study included Denplan patients resident in the North West Region. Age/gender and payment banding frequency distributions were constructed. A market penetration ranking report using the Target Market level of the Super Profiles geodemographic classification was produced by a spreadsheet analysis in Microsoft Excel. A Lorenz curve was plotted to graphically represent the output of the market penetration analysis. Following the market penetration analysis the enumeration districts (EDs) of the six top ranked Target Markets in the North West Region were identified and mapped out across the Region. Finally, the number and percentage of EDs in the six top ranked Target Markets were identified for each health authority in the Region. 47,106 patients were registered with Denplan. In all but one 5-year age band (16-20-year-olds) female patients were in the majority. Patients were concentrated (40.5%) into the 40-55 age group. Nearly 50% (22,329) of patients were allocated to the second lowest payment banding. Under 0.5% of patients (N = 199) were categorised into the highest payment band. The Target Markets at the top of the penetration ranking were more affluent in nature, with a strong rural element and an older demographic profile as part of their descriptive titles. At the bottom of the ranking deprived area types with young demographic profiles predominated. About one half (49.9%) of Denplan patients were present in just over a quarter (25.7%) of the total population of the North West Region. The Lorenz curve demonstrated that Super Profiles at Target Market level had an effectiveness of 37.9% in segmenting the population of the North West Region according to Denplan registration status. The population using this service in the North West Region tend to be from more mature, rural and affluent populations. The Super Profiles classification was moderately successful in segmenting the population of the North West Region according to their Denplan registration status.
NASA Astrophysics Data System (ADS)
Kirchengast, G.; Schweitzer, S.
2008-12-01
The ACCURATE (Atmospheric Climate and Chemistry in the UTLS Region And climate Trends Explorer) mission was conceived at the Wegener Center in late 2004 and subsequently proposed in 2005 by an international team of more than 20 scientific partners from more than 12 countries to an ESA selection process for next Earth Explorer Missions. While the mission was not selected for formal pre-phase A study, it received very positive evaluation and was recommended for further development and demonstration. ACCURATE employs the occultation measurement principle, known for its unique combination of high vertical resolution, accuracy and long-term stability, in a novel way. It systematically combines use of highly stable signals in the MW 17-23/178-196 GHz bands (LEO-LEO MW crosslink occultation) with laser signals in the SWIR 2-2.5 μm band (LEO-LEO IR laser crosslink occultation) for exploring and monitoring climate and chemistry in the atmosphere with focus on the UTLS region (upper troposphere/lower stratosphere, 5-35 km). The MW occultation is an advanced and at the same time compact version of the LEO-LEO MW occultation concept, studied in 2002-2004 for the ACE+ mission project of ESA for frequencies including the 17-23 GHz band, complemented by U.S. study heritage for frequencies including the 178-196 GHz bands (R. Kursinski et al., Univ. of Arizona, Tucson). The core of ACCURATE is tight synergy of the IR laser crosslinks with the MW crosslinks. The observed parameters, obtained simultaneously and in a self-calibrated manner based on Doppler shift and differential log-transmission profiles, comprise the fundamental thermodynamic variables of the atmosphere (temperature, pressure/geopotential height, humidity) retrieved from the MW bands, complemented by line-of-sight wind, six greenhouse gases (GHGs) and key species of UTLS chemistry (H2O, CO2, CH4, N2O, O3, CO) and four CO2 and H2O isotopes (HDO, H218O, 13CO2, C18OO) from the SWIR band. Furthermore, profiles of aerosol extinction, cloud layering, and turbulence are obtained. All profiles come with accurate height knowledge (< 10 m uncertainty), since measuring height as a function of time is intrinsic to the MW occultation part of ACCURATE. The presentation will introduce ACCURATE along the lines above, with emphasis on the climate science value and the new IR laser occultation capability. The focus will then be on retrieval performance analysis results obtained so far, in particular regarding the profiles of GHGs, isotopes, and wind. The results provide evidence that the GHG and isotope profiles can generally be retrieved within 5-35 km outside clouds with < 1% to 5% rms accuracy at 1-2 km vertical resolution, and wind with < 2 m/s accuracy. Monthly mean climatological profiles, assuming ~40 profiles per climatologic grid box per month, are found unbiased (free of time-varying biases) and at < 0.2% to 0.5% rms accuracy. These encouraging results are discussed in light of the potential of the ACCURATE technique to provide benchmark data for future monitoring of climate, GHGs, and chemistry variability and change. European science and demonstration activities are outlined, including international participation opportunities.
Saieg, Mauro Ajaj; Geddie, William R; Boerner, Scott L; Liu, Ni; Tsao, Ming; Zhang, Tong; Kamel-Reid, Suzanne; da Cunha Santos, Gilda
2012-06-25
Novel high-throughput molecular technologies have made the collection and storage of cells and small tissue specimens a critical issue. The FTA card provides an alternative to cryopreservation for biobanking fresh unfixed cells. The current study compared the quality and integrity of the DNA obtained from 2 types of FTA cards (Classic and Elute) using 2 different extraction protocols ("Classic" and "Elute") and assessed the feasibility of performing multiplex mutational screening using fine-needle aspiration (FNA) biopsy samples. Residual material from 42 FNA biopsies was collected in the cards (21 Classic and 21 Elute cards). DNA was extracted using the Classic protocol for Classic cards and both protocols for Elute cards. Polymerase chain reaction for p53 (1.5 kilobase) and CARD11 (500 base pair) was performed to assess DNA integrity. Successful p53 amplification was achieved in 95.2% of the samples from the Classic cards and in 80.9% of the samples from the Elute cards using the Classic protocol and 28.5% using the Elute protocol (P = .001). All samples (both cards) could be amplified for CARD11. There was no significant difference in the DNA concentration or 260/280 purity ratio when the 2 types of cards were compared. Five samples were also successfully analyzed by multiplex MassARRAY spectrometry, with a mutation in KRAS found in 1 case. High molecular weight DNA was extracted from the cards in sufficient amounts and quality to perform high-throughput multiplex mutation assays. The results of the current study also suggest that FTA Classic cards preserve better DNA integrity for molecular applications compared with the FTA Elute cards. Copyright © 2012 American Cancer Society.
Kostanyan, Artak E; Erastov, Andrey A; Shishilov, Oleg N
2014-06-20
The multiple dual mode (MDM) counter-current chromatography separation processes consist of a succession of two isocratic counter-current steps and are characterized by the shuttle (forward and back) transport of the sample in chromatographic columns. In this paper, the improved MDM method based on variable duration of alternating phase elution steps has been developed and validated. The MDM separation processes with variable duration of phase elution steps are analyzed. Basing on the cell model, analytical solutions are developed for impulse and non-impulse sample loading at the beginning of the column. Using the analytical solutions, a calculation program is presented to facilitate the simulation of MDM with variable duration of phase elution steps, which can be used to select optimal process conditions for the separation of a given feed mixture. Two options of the MDM separation are analyzed: 1 - with one-step solute elution: the separation is conducted so, that the sample is transferred forward and back with upper and lower phases inside the column until the desired separation of the components is reached, and then each individual component elutes entirely within one step; 2 - with multi-step solute elution, when the fractions of individual components are collected in over several steps. It is demonstrated that proper selection of the duration of individual cycles (phase flow times) can greatly increase the separation efficiency of CCC columns. Experiments were carried out using model mixtures of compounds from the GUESSmix with solvent systems hexane/ethyl acetate/methanol/water. The experimental results are compared to the predictions of the theory. A good agreement between theory and experiment has been demonstrated. Copyright © 2014 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Tick, G. R.; Wei, S.; Sun, H.; Zhang, Y.
2016-12-01
Pore-scale heterogeneity, NAPL distribution, and sorption/desorption processes can significantly affect aqueous phase elution and mass flux in porous media systems. The application of a scale-independent fractional derivative model (tFADE) was used to simulate elution curves for a series of columns (5 cm, 7 cm, 15 cm, 25 cm, and 80 cm) homogeneously packed with 20/30-mesh sand and distributed with uniform saturations (7-24%) of NAPL phase trichloroethene (TCE). An additional set of columns (7 cm and 25 cm) were packed with a heterogeneous distribution of quartz sand upon which TCE was emplaced by imbibing the immiscible liquid, under stable displacement conditions, to simulate a spill-type process. The tFADE model was able to better represent experimental elution behavior for systems that exhibited extensive long-term concentration tailing requiring much less parameters compared to typical multi-rate mass transfer models (MRMT). However, the tFADE model was not able to effectively simulate the entire elution curve for such systems with short concentration tailing periods since it assumes a power-law distribution for the dissolution rate for TCE. Such limitations may be solved using the tempered fractional derivative model, which can capture the single-rate mass transfer process and therefore the short elution concentration tailing behavior. Numerical solution for the tempered fractional-derivative model in bounded domains however remains a challenge and therefore requires further study. However, the tFADE model shows excellent promise for understanding impacts on concentration elution behavior for systems in which physical heterogeneity, non-uniform NAPL distribution, and pronounced sorption-desorption effects dominate or are present.
Berthod, Alain; Hassoun, Mahmoud
2006-05-26
The retention volumes of solutes in countercurrent chromatography (CCC) are directly proportional to their distribution coefficients, K(D) in the biphasic liquid system used as mobile and stationary phase in the CCC column. The cocurrent CCC method consists in putting the liquid "stationary" phase in slow motion in the same direction as the mobile phase. A mixture of five steroid compounds of widely differing polarities was used as a test mixture to evaluate the capabilities of the method with the biphasic liquid system made of water/methanol/ethyl acetate/heptane 6/5/6/5 (v/v) and a 53 mL CCC column of the coil planet centrifuge type. It is shown that the chromatographic resolution obtained in cocurrent CCC is very good because the solute band broadening is minimized as long as the solute is located inside the "stationary" phase. Pushing the method at its limits, it is demonstrated that the five steroids can still be (partly) separated when the flow rate of the two liquid phases is the same (2 mL/min). This is due to the higher volume of upper phase (72% of the column volume) contained inside the CCC column producing a lower linear speed compared to the aqueous lower phase linear speed. The capabilities of the cocurrent CCC method compare well with those of the gradient elution method in HPLC. Continuous detection is a problem due to the fact that two immiscible liquid phases elute from the column. It was partly solved using an evaporative light scattering detector.
Electrophoretic fractional elution apparatus employing a rotational seal fraction collector
NASA Technical Reports Server (NTRS)
Bier, M. (Inventor)
1977-01-01
Electrophoretic fractional elution apparatus which has a column with a rotating seal joint is described. A thin jet of eluting buffer is directed across the lumen of the electrophoretic column in a direction perpendicular to that of electrophoretic migration. Either the content of the column is rotated with respect to the stationary jet, or the jet is rotated with respect to the column. The system may employ electrophoresis either in free solution or in packed columns.
Neo, Shu Hui; Chung, Ka Yan; Quek, Jia Min; Too, Heng-Phon
2017-11-30
The preservation of nucleic acids from clinical samples is critical to facilitate accurate molecular diagnosis. The use of a paper matrix, Flinders Technology Associates (FTA) Elute cards, to archive DNA and viral RNA is well-documented. However, the feasibility of FTA Elute cards for archiving serum and serum exosomal microRNAs (miRNAs) remains unclear. Here, we performed a comprehensive evaluation of FTA Elute cards for miRNA storage and recovery in different pre-analytical conditions. The recovery of serum miRNA dry-spotted on FTA Elute cards by direct elution with water at high temperature was poor. However, serum miRNAs dry-spotted on the cards were isolated with about 40% yield when using QIAzol lysis reagent and recovery was improved remarkably (>80%) upon extraction from cards pre-treated with trehalose. miRNAs stored on the cards remained stable at room temperature and can be kept for prolonged periods. Furthermore, miRNAs could be similarly recovered from serum exosomes dry-spotted on the cards. Importantly, when using sera from gastric cancer (GC) patients, the miRNAs were efficiently recovered from trehalose pre-treated cards without affecting their representation. Collectively, we have demonstrated the potential of FTA Elute cards to archive serum and serum exosomal miRNAs, making it useful for biomarker discovery and diagnostics.
DNA adsorption to and elution from silica surfaces: influence of amino acid buffers.
Vandeventer, Peter E; Mejia, Jorge; Nadim, Ali; Johal, Malkiat S; Niemz, Angelika
2013-09-19
Solid phase extraction and purification of DNA from complex samples typically requires chaotropic salts that can inhibit downstream polymerase amplification if carried into the elution buffer. Amino acid buffers may serve as a more compatible alternative for modulating the interaction between DNA and silica surfaces. We characterized DNA binding to silica surfaces, facilitated by representative amino acid buffers, and the subsequent elution of DNA from the silica surfaces. Through bulk depletion experiments, we found that more DNA adsorbs to silica particles out of positively compared to negatively charged amino acid buffers. Additionally, the type of the silica surface greatly influences the amount of DNA adsorbed and the final elution yield. Quartz crystal microbalance experiments with dissipation monitoring (QCM-D) revealed multiphasic DNA adsorption out of stronger adsorbing conditions such as arginine, glycine, and glutamine, with DNA more rigidly bound during the early stages of the adsorption process. The DNA film adsorbed out of glutamate was more flexible and uniform throughout the adsorption process. QCM-D characterization of DNA elution from the silica surface indicates an uptake in water mass during the initial stage of DNA elution for the stronger adsorbing conditions, which suggests that for these conditions the DNA film is partly dehydrated during the prior adsorption process. Overall, several positively charged and polar neutral amino acid buffers show promise as an alternative to methods based on chaotropic salts for solid phase DNA extraction.
Buza, V V; Karpov, Iu A; Samko, A N; Deev, A D; Lopukhova, V V; Levitskiĭ, I V; Sozykin, A V
2009-01-01
The placement of sirolimus-eluting stents decreases the frequency of repeat revascularization procedures in patients undergoing percutaneous coronary intervention (PCI) in randomized clinical trials. However, there is uncertainty about the effectiveness of sirolimus-eluting stents, and increasing concern about their safety in routine clinical practice. From the prof. Samko PCI laboratory in Moscow, Russia, we identified 426 patients, who received either bare-metal stents alone or sirolimus-eluting stents alone during an index PCI procedure between March 1, 2002, and September 31, 2004.The primary outcomes of the study were the rates of target-lesion revascularization, myocardial infarction, death, late stent thrombosis. The 3-year rate of target-lesion revascularization was significantly lower among patients who received sirolimus-eluting stents than among those who received bare-metal stents (3.1% vs. 19 %, p=0.001). The 3-year mortality rate was not different between the bare-metal stent group and the sirolimus eluting stent group (5.9% vs. 7.2%, p=0.68), the 3-year rate of all ARC late stent thrombosis was similar in the two groups (5.9% and 7.2%, respectively; p=0.95). Sirolimus-eluting stents are effective in reducing the need for target-vessel revascularization without significantly increased rates of death, late stent thrombosis, myocardial infarction.
Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming
2015-03-01
A simple and efficient integrated microwave processing system (IMPS) was firstly assembled and validated for the extraction of organophosphorus pesticides in fresh vegetables. Two processes under microwave irradiation, dynamic microwave-assisted extraction (DMAE) and microwave-accelerated solvent elution (MASE), were integrated for simplifying the pretreatment of the sample. Extraction, separation, enrichment and elution were finished in a simple step. The organophosphorus pesticides were extracted from the fresh vegetables into hexane with DMAE, and then the extract was directly introduced into the enrichment column packed with active carbon fiber (ACF). Subsequently, the organophosphorus pesticides trapped on the ACF were eluted with ethyl acetate under microwave irradiation. No further filtration or cleanup was required before analysis of the eluate by gas chromatography-mass spectrometry. Some experimental parameters affecting extraction efficiency were investigated and optimized, such as microwave output power, kind and volume of extraction solvent, extraction time, amount of sorbent, elution microwave power, kind and volume of elution solvent, elution solvent flow rate. Under the optimized conditions, the recoveries were in the range of 71.5-105.2%, and the relative standard deviations were lower than 11.6%. The experiment results prove that the present method is a simple and effective sample preparation method for the determination of pesticides in solid samples. Copyright © 2014 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Chen, Liang-Chia; Ho, Hsuan-Wei; Nguyen, Xuan-Loc
2010-02-01
This article presents a novel band-pass filter for Fourier transform profilometry (FTP) for accurate 3-D surface reconstruction. FTP can be employed to obtain 3-D surface profiles by one-shot images to achieve high-speed measurement. However, its measurement accuracy has been significantly influenced by the spectrum filtering process required to extract the phase information representing various surface heights. Using the commonly applied 2-D Hanning filter, the measurement errors could be up to 5-10% of the overall measuring height and it is unacceptable to various industrial application. To resolve this issue, the article proposes an elliptical band-pass filter for extracting the spectral region possessing essential phase information for reconstructing accurate 3-D surface profiles. The elliptical band-pass filter was developed and optimized to reconstruct 3-D surface models with improved measurement accuracy. Some experimental results verify that the accuracy can be effectively enhanced by using the elliptical filter. The accuracy improvement of 44.1% and 30.4% can be achieved in 3-D and sphericity measurement, respectively, when the elliptical filter replaces the traditional filter as the band-pass filtering method. Employing the developed method, the maximum measured error can be kept within 3.3% of the overall measuring range.
Pavlidou, Anastasia; Schnitzler, Alfons; Lange, Joachim
2014-05-01
The neural correlates of action recognition have been widely studied in visual and sensorimotor areas of the human brain. However, the role of neuronal oscillations involved during the process of action recognition remains unclear. Here, we were interested in how the plausibility of an action modulates neuronal oscillations in visual and sensorimotor areas. Subjects viewed point-light displays (PLDs) of biomechanically plausible and implausible versions of the same actions. Using magnetoencephalography (MEG), we examined dynamic changes of oscillatory activity during these action recognition processes. While both actions elicited oscillatory activity in visual and sensorimotor areas in several frequency bands, a significant difference was confined to the beta-band (∼20 Hz). An increase of power for plausible actions was observed in left temporal, parieto-occipital and sensorimotor areas of the brain, in the beta-band in successive order between 1650 and 2650 msec. These distinct spatio-temporal beta-band profiles suggest that the action recognition process is modulated by the degree of biomechanical plausibility of the action, and that spectral power in the beta-band may provide a functional interaction between visual and sensorimotor areas in humans. Copyright © 2014 Elsevier Ltd. All rights reserved.
Identification of geometrical isomers and comparison of different isomeric samples of astaxanthin.
Qiu, Dan; Wu, Yue-Chan; Zhu, Wen-Li; Yin, Hong; Yi, Long-Tao
2012-09-01
A high-performance liquid chromatographic (HPLC) analysis system for isomeric astaxanthin was developed. The separation system consisted of a C(30) column and an elution system of methanol/MTBE/water/dichloromethane (77:13:8:2, v/v/v/v). Using the combination of HPLC diode array detector and HPLC atmospheric pressure chemical ionization mass spectrometry, 11 geometrical isomers and 4 epoxides of astaxanthin were successfully identified. Referred to crystal, only isomerization with different degrees was found for solvent dissolving and iodine catalysis, while melting of astaxanthin caused isomerization, slight oxidation, and more noticeable polymerization confirmed by gel permeation chromatography. Chemical changes in isomeric samples all caused a decrease in UV content. The vibrational spectra (infrared and Raman) showed that epoxide was the only new functional group generated for melting. Changes of several key bands and formations of new bands were found in iodine catalysis and melting samples because of isomerization. Practical Application: Eleven geometrical isomers and 4 epoxides, which were normally generated for solvent dissolving, iodine catalysis, and melting of astaxanthin, have been identified by C(30) -HPLC-MS technology. Furthermore, different samples were measured by gel permeation chromatography, UV, infrared, and Raman, based on the analysis of messages, the effect of each processing was well understood. © 2012 Institute of Food Technologists®
Macko, Tibor; Pasch, Harald; Brüll, Robert
2006-05-19
The adsorption of polyethylene and polypropylene on zeolites depends on the nature of zeolite, the solvent as well as the molar mass of the polymer sample. For example, linear polyethylene is strongly retained on zeolite SH-300 from decalin, while isotactic, syndiotactic or atactic polypropylene is fully eluted in this system. On the other hand, polypropylene is retained on zeolite CBV-780 from diphenylether, while linear polyethylene is eluted. These differences in the elution behaviour have been utilised for selective removal of either linear polyethylene or polypropylene from blends of both polymers. The desorption of the retained polymer is difficult, or at times impossible. However, the selected adsorption systems have complimentary character, i.e. either one or second component is eluted or fully retained. Thus these sorbent/solvent systems, identified herein, are the first isocratic chromatographic systems, which enable selectively to remove polyethylene or polypropylene from their mixture. Moreover, decalin/SH-300 enables the removal of both linear and branched polyethylene from mixtures with random ethylene/propylene copolymers (polyethylene fully retained, ethylene/propylene copolymers eluted).
Optimized pH method for DNA elution from buccal cells collected in Whatman FTA cards.
Lema, Carolina; Kohl-White, Kendra; Lewis, Laurie R; Dao, Dat D
2006-01-01
DNA is the most accessible biologic material for obtaining information from the human genome because of its molecular stability and its presence in every nucleated cell. Currently, single nucleotide polymorphism genotyping and DNA methylation are the main DNA-based approaches to deriving genomic and epigenomic disease biomarkers. Upon the discontinuation of the Schleicher & Schuell IsoCode product (Dassel, Germany), which was a treated paper system to elute DNA from several biologic sources for polymerase chain reaction (PCR) analysis, a high-yielding DNA elution method was imperative. We describe here an improved procedure of the not fully validated Whatman pH-based elution protocol. Our DNA elution procedure from buccal cells collected in Whatman FTA cards (Whatman Inc., Florham Park, NJ) yielded approximately 4 microg of DNA from a 6-mm FTA card punch and was successfully applied for HLA-DQB1 genotyping. The genotypes showed complete concordance with data obtained from blood of the same subjects. The achieved high DNA yield from buccal cells suggests a potential cost-effective tool for genomic and epigenomic disease biomarkers development.
Fu, Yong; Lei, Peng; Han, Yu-mei; Yan, Dan
2010-02-01
To study the technological parameters of the purification process of saponins with macroporous adsorption resin. The adsorptive characteristics and elutive parameters of the process were studied by taking the elutive and purified ratio of saponins as markers. Bacteriostasis activity of each parts eluted was evaluated by the mean of cup-plate method. 13.6 mL of the extraction of sapindus saponin (crude drugs 0.01 g/mL) was purified with a column of macroporous adsorption resin (phi15 mm x H90 mm, dry weight 2.5 g) and washed with 3BV of distilled water, then eluted with 3BV of 30% ethanol and 3BV of 70% ethanol, most of saponins were collected in the 70% ethanol. With macroporous adsorption resin adsorbing and purifying, the elutive ratio of saponins was 93.8% and the purity reached 250.1%. So this process of applying macroporous adsorption resin to adsorb and purify saponins is feasible, and supplies reference to the purification of other types of saponin.
Enhanced performance of magnesium alloy for drug-eluting vascular scaffold application
NASA Astrophysics Data System (ADS)
Dong, Hongzhou; Li, Daikun; Mao, Daoyong; Bai, Ningning; Chen, Yashi; Li, Qing
2018-03-01
Bio-absorbable magnesium alloys drug-eluting vascular scaffold was developed to resolve the defect of permanent metal and drug-eluting stents, most notably a chronic vessel wall inflammation and the risk of stent thrombosis. Nevertheless, violent chemical reaction and rapid degradation under physiological conditions limits their application. Furthermore, multifunctional drug-eluting stents which could reduce the formation of thrombus and repair the damaged vessels need more attention to fundamentally cure the coronary artery disease. Herein, a drug delivery system (Mg/MgO/PLA-FA) which can realize sustainable release of ferulaic acid was designed via anodic oxidation process and dip coating process. Electrochemical tests and immersion experiments showed that the superior anticorrosion behavior, it is due to the dense MgO-PLA composite layer. The released ferulaic acid can effectively decrease platelets adhesion and aggregation during the early stage of implantation. Besides, hemolysis tests showed that the composite coatings endowed the Mg alloy with a low hemolysis ratio. The Mg/MgO/PLA-FA composite materials may be appropriate for applications on biodegradable Mg alloys drug-eluting stents.
A Raman and UV-Vis study of catecholamines oxidized with Mn(III)
NASA Astrophysics Data System (ADS)
Barreto, W. J.; Ponzoni, S.; Sassi, P.
1998-12-01
A UV-Vis and Raman spectroscopy study of three aminochromes generated through Mn 3+ oxidation of the dopamine, L-dopa and adrenaline molecules at physiological pH was performed. The UV-Vis spectra of the catecholamines oxidized using Mn 3+ in buffer solution at pH 7.2 show a band at ca. 300 nm, formed by two transitions at 280 nm and 300 nm assigned to an La and Lb transition respectively, and other at ca. 470 nm assigned to an n- π* transition localized in the carbonyl group. This assignment is suggested by the UV-Vis and Raman spectra of ortho-aminoquinone generated by MnO 2 oxidation of a dopamine aqueous acidic solution. The resonance Raman spectra of the three chromes at buffer pH 7.2 show a very similar feature and the most intense bands are observed in the spectral range 1100-1800 cm -1. The band around 1680 cm -1 for the three compounds is assigned to a ν(CO) stretching vibration, 1630 cm -1 to the ν(CC) ring mode, two bands at 1423, 1439 cm -1; 1427, 1438 cm -1 and 1456, 1475 cm -1 are assigned to a ν(CN +) vibration, for aminochrome, dopachrome and adrenochrome, respectively. The excitation profiles for the most intense bands for aminochrome and adrenochrome were obtained. The band assigned to the ν(CN +) present a red shift with respect to the visible band peak, however the band in adrenochrome at 1475 cm -1 shows a profile similar to ν(CO) and ν(CC) modes that reflects the methyl group effect on mixing this mode more effectively with the ν(CC) ring mode.
Xiao, Meng; Kong, Fanrong; Jin, Ping; Wang, Qinning; Xiao, Kelin; Jeoffreys, Neisha; James, Gregory
2012-01-01
PCR ribotyping is the most commonly used Clostridium difficile genotyping method, but its utility is limited by lack of standardization. In this study, we analyzed four published whole genomes and tested an international collection of 21 well-characterized C. difficile ribotype 027 isolates as the basis for comparison of two capillary gel electrophoresis (CGE)-based ribotyping methods. There were unexpected differences between the 16S-23S rRNA intergenic spacer region (ISR) allelic profiles of the four ribotype 027 genomes, but six bands were identified in all four and a seventh in three genomes. All seven bands and another, not identified in any of the whole genomes, were found in all 21 isolates. We compared sequencer-based CGE (SCGE) with three different primer pairs to the Qiagen QIAxcel CGE (QCGE) platform. Deviations from individual reference/consensus band sizes were smaller for SCGE (0 to 0.2 bp) than for QCGE (4.2 to 9.5 bp). Compared with QCGE, SCGE more readily distinguished bands of similar length (more discriminatory), detected bands of larger size and lower intensity (more sensitive), and assigned band sizes more accurately and reproducibly, making it more suitable for standardization. Specifically, QCGE failed to identify the largest ISR amplicon. Based on several criteria, we recommend the primer set 16S-USA/23S-USA for use in a proposed standard SCGE method. Similar differences between SCGE and QCGE were found on testing of 14 isolates of four other C. difficile ribotypes. Based on our results, ISR profiles based on accurate sequencer-based band lengths would be preferable to agarose gel-based banding patterns for the assignment of ribotypes. PMID:22692737
Bechtel, Peter J; Oliveira, Alexandra CM; Demir, Necla; Smiley, Scott
2013-01-01
Giant red sea cucumbers, Parastichopus californicus, are commercially harvested in the U.S. Pacific Northwest; however, the nutritional and chemical properties of its edible muscle bands and body wall have not been fully elucidated. In particular are the fatty acid profiles of P. californicus tissues, which have not been documented. Sea cucumbers were delivered live and muscle bands and body wall freeze dried, vacuum packed, and stored at –30°C until analyzed. Proximate composition of freeze-dried tissues varied greatly with muscle bands being composed of 68% protein, 12% ash, 9% carbohydrate, and 5% lipids, while the body wall was composed of 47% protein, 26% ash, 15% carbohydrate, and 8% lipids. The hydroxyproline, proline, and glycine contents of the body wall were much higher than those in muscle bands, consistent with the larger amount of connective tissue. Calcium, magnesium, sodium, and iron contents were higher in the body wall than those in muscle bands, whereas the opposite was observed for zinc content. Total long-chain n-3 fatty acid contents were 19% and 32% of total fatty acids in body wall and muscle bands, respectively. Muscle bands had higher content of eicosapentaenoic acid (20:5n-3) than body wall at 22.6% and 12.3%, respectively. High content of arachidonic acid (20:4n-6) was recorded in both body wall (7.1%) and muscle bands (9.9%). Overall, the fatty acid profiles of body wall and muscle bands of P. californicus resemble those described for other species; however, the distribution and occurrence of certain fatty acids is unique to P. californicus, being representative of the fatty acid composition of temperate-polar marine organisms. The chemical characterization of freeze-dried edible tissues from P. californicus demonstrated that these products have valuable nutritional properties. The body wall, a food product of lower market value than muscle bands, could be better utilized for nutraceutical and pharmaceutical applications. PMID:24804015
Resist development status for immersion lithography
NASA Astrophysics Data System (ADS)
Tsuji, Hiromitsu; Yoshida, Masaaki; Ishizuka, Keita; Hirano, Tomoyuki; Endo, Kotaro; Sato, Mitsuru
2005-05-01
Immersion lithography has already demonstrated superior performance for next generation semiconductor manufacturing, while some challenges with contact immersion fluids and resist still remain. There are many interactions to be considered with regards to the solid and liquid interface. Resist elusion in particular requires very careful attention since the impact on the lens and fluid supply system in exposure tool could pose a significant risk at the manufacturing stage. TOK developed a screening procedure to detect resist elution of ion species down to ppb levels during non and post exposure steps. It was found that the PAG cation elution is affected by molecular weight and structure while the PAG anion elution was dependent on the molecular structure and mobility. In this paper, lithographic performance is also discussed with the low elution type resist.
Controversies in the use & implementation of drug-eluting stent technology
Itagaki, Brandon K.; Brar, Somjot S.
2012-01-01
The introduction of drug eluting stents has resulted in dramatic reductions in the rates of restenosis and the need for repeat revascularization. In the last several years, concern has been raised regarding the long-term safety of this technology, particularly in the area of late restenosis and stent thrombosis. The development of newer anti-restenotic drug coatings, biodegradable polymers and even completely bioabsorbable stents offer the potential to address these limitations. Additional questions that have recently come to the forefront include the optimal duration of dual antiplatelet therapy, the use of platelet reactivity assays and genetic testing and drug eluting stent use in the treatment of acute myocardial infarction. This article will attempt to address these and other areas of controversy in the use and implementation of drug eluting stents. PMID:23391788
1978-01-01
This laboratory has previously isolated a fraction from rat liver nuclei consisting of nuclear pore complexes associated with the proteinaceous lamina which underlies the inner nuclear membrane. Using protein eluted from sodium dodecyl sulfate (SDS) gels, we have prepared antibodies in chickens to each of the three predominant pore complex- lamina bands. Ouchterlony double diffusion analysis shows that each of these individual bands cross-reacts strongly with all three antisera. In immunofluorescence localization performed on tissue culture cells with these antibodies, we obtain a pattern of intense staining at the periphery of the interphase nucleus, with little or no cytoplasmic reaction. Electron microscope immunoperoxidase staining of rat liver nuclei with these antibodies labels exclusively the nuclear periphery. Furthermore, reaction occurs in areas which contain the lamina, but not at the pore complexes. While our isolation procedure extracts the internal contents of nuclei completely, semiquantitative Ouchterlony analysis shows that it releases negligible amounts of these lamina antigens. Considered together, our results indicate that these three bands represent major components of a peripheral nuclear lamina, and are not structural elements of an internal "nuclear protein matrix." Fluorescence microscopy shows that the perinuclear interphase localization of these lamina proteins undergoes dramatic changes during mitosis. Concomitant with nuclear envelope disassembly in prophase, these antigens assume a diffuse localization throughout the cell. This distribution persists until telophase, when the antigens become progressively and completely localized at the surface of the daughter chromosome masses. We propose that the lamina is a biological polymer which can undergo reversible disassembly during mitosis. PMID:102651
Caswell, Clayton C; Han, Runlin; Hovis, Kelley M; Ciborowski, Pawel; Keene, Douglas R; Marconi, Richard T; Lukomski, Slawomir
2008-02-01
Non-specific activation of the complement system is regulated by the plasma glycoprotein factor H (FH). Bacteria can avoid complement-mediated opsonization and phagocytosis through acquiring FH to the cell surface. Here, we characterize an interaction between the streptococcal collagen-like protein Scl1.6 of M6-type group A Streptococcus (GAS) and FH. Using affinity chromatography with immobilized recombinant Scl1.6 protein, we co-eluted human plasma proteins with molecular weight of 155 kDa, 43 kDa and 38 kDa. Mass spectrometry identified the 155 kDa band as FH and two other bands as isoforms of the FH-related protein-1. The identities of all three bands were confirmed by Western immunoblotting with specific antibodies. Structure-function relation studies determined that the globular domain of the Scl1.6 variant specifically binds FH while fused to collagenous tails of various lengths. This binding is not restricted to Scl1.6 as the phylogenetically linked Scl1.55 variant also binds FH. Functional analyses demonstrated the cofactor activity of the rScl1.6-bound FH for factor I-mediated cleavage of C3b. Finally, purified FH bound to the Scl1.6 protein present in the cell wall material obtained from M6-type GAS. In conclusion, we have identified a functional interaction between Scl1 and plasma FH, which may contribute to GAS evasion of complement-mediated opsonization and phagocytosis.
Walsh, L J; Lander, P E; Seymour, G J; Powell, R N
1987-01-01
Recent studies have described the presence of an interleukin 1 (IL-1) inhibitor (ILS) in supernatants from human gingival organ cultures. This report describes the isolation and purification of ILS. ILS was produced in serum-free medium and purified to apparent homogeneity by ion exchange chromatography and high pressure liquid chromatography. IL-1 and ILS eluted as discrete proteins using this system, with ILS appearing as a single protein band of 97,400 molecular weight on SDS-PAGE. ILS inhibited the effects of both murine IL-1 and IL-2 on thymocyte proliferation, and was heat resistant, moderately resistant to freeze-thawing and stable for 2 years at 0-4 degrees C or -20 degrees C. Production of ILS by gingival epithelial cell cultures was not affected by depletion of Langerhans cells, implying that ILS is primarily a keratinocyte product. Images Fig. 5 PMID:3498574
Non-planar microfabricated gas chromatography column
Lewis, Patrick R.; Wheeler, David R.
2007-09-25
A non-planar microfabricated gas chromatography column comprises a planar substrate having a plurality of through holes, a top lid and a bottom lid bonded to opposite surfaces of the planar substrate, and inlet and outlet ports for injection of a sample gas and elution of separated analytes. A plurality of such planar substrates can be aligned and stacked to provide a longer column length having a small footprint. Furthermore, two or more separate channels can enable multi-channel or multi-dimensional gas chromatography. The through holes preferably have a circular cross section and can be coated with a stationary phase material or packed with a porous packing material. Importantly, uniform stationary phase coatings can be obtained and band broadening can be minimized with the circular channels. A heating or cooling element can be disposed on at least one of the lids to enable temperature programming of the column.
Allergic reaction to latex: a risk factor for unsuspected anaphylaxis.
Warpinski, J R; Folgert, J; Cohen, M; Bush, R K
1991-01-01
Allergic reactions to latex, including anaphylaxis may be a problem in certain individuals exposed to latex. Four atopic patients with symptoms of rhinitis, asthma, anaphylaxis, and/or urticaria upon contact with latex products were studied. The patients showed IgE binding to latex RAST disks ranging from 1.0 to 27.3 times the negative control. Latex products (gloves, balloons, and condoms) directly bound IgE from all four patients. Eluted proteins from the latex products inhibited IgE binding to commercial latex RAST disks. SDS-PAGE demonstrated multiple latex protein bands by Coomassie Blue staining between 14 and 66 kD. Immunoblotting showed specific IgE binding to latex proteins at 30 and 66 kD. These results indicate that latex-allergic patients have IgE directed against specific latex proteins. Allergy to latex can pose a substantial health risk to susceptible individuals.
Muramatsu, Takashi; Onuma, Yoshinobu; van Geuns, Robert-Jan; Chevalier, Bernard; Patel, Tejas M; Seth, Ashok; Diletti, Roberto; García-García, Hector M; Dorange, Cécile C; Veldhof, Susan; Cheong, Wai-Fung; Ozaki, Yukio; Whitbourn, Robert; Bartorelli, Antonio; Stone, Gregg W; Abizaid, Alexandre; Serruys, Patrick W
2014-05-01
The aim of this study was to evaluate 1-year clinical outcomes of diabetic patients treated with the Absorb bioresorbable vascular scaffold (BVS). Clinical outcomes of diabetic patients after BVS implantation have been unreported. This study included 101 patients in the ABSORB Cohort B trial and the first consecutive 450 patients with 1 year of follow-up in the ABSORB EXTEND trial. A total of 136 diabetic patients were compared with 415 nondiabetic patients. In addition, 882 diabetic patients treated with everolimus-eluting metal stents (EES) in pooled data from the SPIRIT trials (SPIRIT FIRST [Clinical Trial of the Abbott Vascular XIENCE V Everolimus Eluting Coronary Stent System], SPIRIT II [A Clinical Evaluation of the XIENCE V Everolimus Eluting Coronary Stent System], SPIRIT III [Clinical Trial of the XIENCE V Everolimus Eluting Coronary Stent System (EECSS)], SPIRIT IV Clinical Trial [Clinical Evaluation of the XIENCE V Everolimus Eluting Coronary Stent System]) were used for the comparison by applying propensity score matching. The primary endpoint was a device-oriented composite endpoint (DoCE), including cardiac death, target vessel myocardial infarction, and target lesion revascularization at 1-year follow-up. The cumulative incidence of DoCE did not differ between diabetic and nondiabetic patients treated with the BVS (3.7% vs. 5.1%, p = 0.64). Diabetic patients treated with the BVS had a similar incidence of the DoCE compared with diabetic patients treated with EES in the matched study group (3.9% for the BVS vs. 6.4% for EES, p = 0.38). There were no differences in the incidence of definite or probable scaffold/stent thrombosis (0.7% for both diabetic and nondiabetic patients with the BVS; 1.0% for diabetic patients with the BVS vs. 1.7% for diabetic patients with EES in the matched study group). In the present analyses, diabetic patients treated with the BVS showed similar rates of DoCEs compared with nondiabetic patients treated with the BVS and diabetic patients treated with EES at 1-year follow-up. (ABSORB Clinical Investigation, Cohort B; NCT00856856; ABSORB EXTEND Clinical Investigation; NCT01023789; Clinical Trial of the Abbott Vascular XIENCE V Everolimus Eluting Coronary Stent System [SPIRIT FIRST]; NCT00180453; A Clinical Evaluation of the XIENCE V Everolimus Eluting Coronary Stent System [SPIRIT II]; NCT00180310; Clinical Trial of the XIENCE V Everolimus Eluting Coronary Stent System [EECSS] [SPIRIT III]; NCT00180479; Clinical Evaluation of the XIENCE V Everolimus Eluting Coronary Stent System [SPIRIT IV Clinical Trial]; NCT00307047). Copyright © 2014 American College of Cardiology Foundation. Published by Elsevier Inc. All rights reserved.
Shan, Yi-chu; Zhang, Yu-kui; Zhao, Rui-huan
2002-07-01
In high performance liquid chromatography, it is necessary to apply multi-composition gradient elution for the separation of complex samples such as environmental and biological samples. Multivariate stepwise gradient elution is one of the most efficient elution modes, because it combines the high selectivity of multi-composition mobile phase and shorter analysis time of gradient elution. In practical separations, the separation selectivity of samples can be effectively adjusted by using ternary mobile phase. For the optimization of these parameters, the retention equation of samples must be obtained at first. Traditionally, several isocratic experiments are used to get the retention equation of solute. However, it is time consuming especially for the separation of complex samples with a wide range of polarity. A new method for the fast optimization of ternary stepwise gradient elution was proposed based on the migration rule of solute in column. First, the coefficients of retention equation of solute are obtained by running several linear gradient experiments, then the optimal separation conditions are searched according to the hierarchical chromatography response function which acts as the optimization criterion. For each kind of organic modifier, two initial linear gradient experiments are used to obtain the primary coefficients of retention equation of each solute. For ternary mobile phase, only four linear gradient runs are needed to get the coefficients of retention equation. Then the retention times of solutes under arbitrary mobile phase composition can be predicted. The initial optimal mobile phase composition is obtained by resolution mapping for all of the solutes. A hierarchical chromatography response function is used to evaluate the separation efficiencies and search the optimal elution conditions. In subsequent optimization, the migrating distance of solute in the column is considered to decide the mobile phase composition and sustaining time of the latter steps until all the solutes are eluted out. Thus the first stepwise gradient elution conditions are predicted. If the resolution of samples under the predicted optimal separation conditions is satisfactory, the optimization procedure is stopped; otherwise, the coefficients of retention equation are adjusted according to the experimental results under the previously predicted elution conditions. Then the new stepwise gradient elution conditions are predicted repeatedly until satisfactory resolution is obtained. Normally, the satisfactory separation conditions can be found only after six experiments by using the proposed method. In comparison with the traditional optimization method, the time needed to finish the optimization procedure can be greatly reduced. The method has been validated by its application to the separation of several samples such as amino acid derivatives, aromatic amines, in which satisfactory separations were obtained with predicted resolution.
ERIC Educational Resources Information Center
Rickels, David A.; Brewer, Wesley D.
2017-01-01
The purpose of this study was to investigate participation in a Facebook social media community known as Band Director's Group (BDG) through examination of members' demographic profiles, self-reported usage behaviors, and perceptions about how group activity satisfies their professional development needs. Respondents to an online survey (n = 336)…
Ooi, Tze C; Thompson, Dennis; Anderson, David R; Fisher, Ray
2018-01-01
It has been previously shown that the isomer profile of PCDF emissions from iron ore sinter plant only varies within limits even when suppressants or alternative fuels are added, to the extent that it can be said to have a 'fingerprint'. The isomer profiles of PCDD from tetra- to hexacholrodibenzo-p-dioxin from the same samples examined for PCDF emissions have been obtained, and show the same tendency for a 'fingerprint ' isomer distribution to occur. Occasional exceptionally high isomer abundances are observed, but these are uncommon. The potential for comparison of the abundances of PCDF and PCDD isomers with similar chlorination patterns to determine whether the same formation process is involved has been examined. It is found that co-elutions prevent extensive comparisons irrespective of whether the SP2331 or DB5ms column is used in the analyses for separation of isomers to provide the results used for comparisons, although they allow limited results to be obtained. It is suggested that analyses using the two chromatography columns to analyse the same sample in parallel could provide more resolution of the isomer profiles for use in comparisons. A pilot study using samples analysed using each column is limited because of detailed differences in the emissions profiles, but demonstrates that greater resolution is possible if the two columns are used to analyse one sample. Copyright © 2017 Elsevier Ltd. All rights reserved.
Cho, Yuko; Tsuchiya, Shigeki; Yoshioka, Renpei; Omura, Takuo; Konoki, Keiichi; Oshima, Yasukatsu; Yotsu-Yamashita, Mari
2016-11-25
Hydrophilic-interaction chromatography (HILIC) is reportedly useful for the analysis of saxitoxin (STX) analogues, collectively known as paralytic shellfish toxins. Column switching and two-step gradient elution using HILIC combined with mass spectrometry enabled the simultaneous analysis of the 15 primary STX analogues and their biosynthetic intermediates, arginine, Int-A', and Int-C'2, and the shunt product, Cyclic-C'. Crude extracts of toxin-producing dinoflagellates can be injected without any treatment except filtration. Enrichment of the compounds using this method was highly reproducible with respect to retention times (% RSD was under 1%) and highly sensitive (limits of detection (LODs) were in the range 0.9 (Int-C'2) - 116 (C3) μM) in terms of avoiding matrix effects associated with co-eluting substances. Validation studies demonstrated acceptable performance of this method for specificity, repeatability, linearity and recovery. A comparison of the quantitative results for STX analogues in Alexandrium tamarense using HPLC with post-column fluorescent derivatization and the column-switching HILIC-MS method revealed good agreement. The presence of Int-A', Int-C'2, and Cyclic-C' in toxic dinoflagellate species with different toxin profiles was confirmed using this method. Our data support the hypothesis that the early stages of the STX biosynthesis and shunt pathways are the same in dinoflagellates and cyanobacteria. Copyright © 2016 Elsevier B.V. All rights reserved.
Integrated multidimensional and comprehensive 2D GC analysis of fatty acid methyl esters.
Zeng, Annie Xu; Chin, Sung-Tong; Marriott, Philip J
2013-03-01
Fatty acid methyl ester (FAME) profiling in complex fish oil and milk fat samples was studied using integrated comprehensive 2D GC (GC × GC) and multidimensional GC (MDGC). Using GC × GC, FAME compounds--cis- and trans-isomers, and essential fatty acid isomers--ranging from C18 to C22 in fish oil and C18 in milk fat were clearly displayed in contour plot format according to structural properties and patterns, further identified based on authentic standards. Incompletely resolved regions were subjected to MDGC, with Cn (n = 18, 20) zones transferred to a (2)D column. Elution behavior of C18 FAME on various (2)D column phases (ionic liquids IL111, IL100, IL76, and modified PEG) was evaluated. Individual isolated Cn zones demonstrated about four-fold increased peak capacities. The IL100 provided superior separation, good peak shape, and utilization of elution space. For milk fat-derived FAME, the (2)D chromatogram revealed at least three peaks corresponding to C18:1, more than six peaks for cis/trans-C18:2 isomers, and two peaks for C18:3. More than 17 peaks were obtained for the C20 region of fish oil-derived FAMEs using MDGC, compared with ten peaks using GC × GC. The MDGC strategy is useful for improved FAME isomer separation and confirmation. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Chaudhary, Nisha; Dangi, Priya; Khatkar, B S
2017-02-01
The size distribution assessment of unreduced wheat gluten proteins of commercial Indian wheat varieties was examined using Size-Exclusion Fast Protein Liquid Chromatography. Elution profiles were fractionated into five peaks, with the molecular weights of eluting peaks as 130-30, 55-20, 28-10 and <10 kDa (IV and V), respectively. Peak I (glutenins) and II (gliadins) exhibited contrary results with AWRC (r = 0.928** and r = -0.831**), R/E ratio (r = 0.745** and r = -0.869**), gluten index (r = 0.959** and r = -0.994**), gliadin/glutenin ratio (r = -0.952** and r = 0.948**), dough development time (r = 0.830** and r = -0.930**), dough stability (r = 0.901** and r = -0.979**) and dough weakening (r = -0.969** and r = 0.986**). Significant statistical correlation was also observed for peak I and II with cookie hardness (r = 0.948** and r = -0.924**) and cookie spread (r = -0.837** and r = -0.743**) respectively. Peak III, IV and V occupied a minor fraction of whole and did not exhibit a statistically significant correlation with any of the quality parameters.
Li, Qiang; Tong, Zichuan; Wang, Lefeng; Zhang, Jianjun; Ge, Yonggui; Wang, Hongshi; Li, Weiming; Xu, Li; Ni, Zhuhua
2013-01-01
Introduction With long-term follow-up, whether biodegradable polymer drug-eluting stents (DES) is efficient and safe in primary percutaneous coronary intervention (PCI) remains a controversial issue. This study aims to assess the long-term efficacy and safety of DES in PCI for ST-segment elevation myocardial infarction (STEMI). Material and methods A prospective, randomized single-blind study with 3-year follow-up was performed to compare biodegradable polymer DES with durable polymer DES in 332 STEMI patients treated with primary PCI. The primary end point was major adverse cardiac events (MACE) at 3 years after the procedure, defined as the composite of cardiac death, recurrent infarction, and target vessel revascularization. The secondary end points included in-segment late luminal loss (LLL) and binary restenosis at 9 months and cumulative stent thrombosis (ST) event rates up to 3 years. Results The rate of the primary end points and the secondary end points including major adverse cardiac events, in-segment late luminal loss, binary restenosis, and cumulative thrombotic event rates were comparable between biodegradable polymer DES and durable polymer DES in these 332 STEMI patients treated with primary PCI at 3 years. Conclusions Biodegradable polymer DES has similar efficacy and safety profiles at 3 years compared with durable polymer DES in STEMI patients treated with primary PCI. PMID:24482648
Accelerated in vitro release testing of implantable PLGA microsphere/PVA hydrogel composite coatings
Shen, Jie; Burgess, Diane J.
2011-01-01
Dexamethasone loaded poly(lactic-co-glycolic acid) (PLGA) microsphere/PVA hydrogel composites have been investigated as an outer drug-eluting coating for implantable devices such as glucose sensors to counter negative tissue responses to implants. The objective of this study was to develop a discriminatory, accelerated in vitro release testing method for this drug-eluting coating using United States Pharmacopeia (USP) apparatus 4. Polymer degradation and drug release kinetics were investigated under “real-time” and accelerated conditions (i.e. extreme pH, hydro-alcoholic solutions and elevated temperatures). Compared to “real-time” conditions, the initial burst and lag phases were similar using hydro-alcoholic solutions and extreme pH conditions, while the secondary apparent zero-order release phase was slightly accelerated. Elevated temperatures resulted in a significant acceleration of dexamethasone release. The accelerated release data were able to predict “real-time” release when applying the Arrhenius equation. Microsphere batches with faster and slower release profiles were investigated under “real-time” and elevated temperature (60°C) conditions to determine the discriminatory ability of the method. The results demonstrated both the feasibility and the discriminatory ability of this USP apparatus 4 method for in vitro release testing of drug loaded PLGA microsphere/PVA hydrogel composites. This method may be appropriate for similar drug/device combination products and drug delivery systems. PMID:22016033
Shen, Jie; Burgess, Diane J
2012-01-17
Dexamethasone loaded poly(lactic-co-glycolic acid) (PLGA) microsphere/PVA hydrogel composites have been investigated as an outer drug-eluting coating for implantable devices such as glucose sensors to counter negative tissue responses to implants. The objective of this study was to develop a discriminatory, accelerated in vitro release testing method for this drug-eluting coating using United States Pharmacopeia (USP) apparatus 4. Polymer degradation and drug release kinetics were investigated under "real-time" and accelerated conditions (i.e. extreme pH, hydro-alcoholic solutions and elevated temperatures). Compared to "real-time" conditions, the initial burst and lag phases were similar using hydro-alcoholic solutions and extreme pH conditions, while the secondary apparent zero-order release phase was slightly accelerated. Elevated temperatures resulted in a significant acceleration of dexamethasone release. The accelerated release data were able to predict "real-time" release when applying the Arrhenius equation. Microsphere batches with faster and slower release profiles were investigated under "real-time" and elevated temperature (60°C) conditions to determine the discriminatory ability of the method. The results demonstrated both the feasibility and the discriminatory ability of this USP apparatus 4 method for in vitro release testing of drug loaded PLGA microsphere/PVA hydrogel composites. This method may be appropriate for similar drug/device combination products and drug delivery systems. Copyright © 2011 Elsevier B.V. All rights reserved.
Latriano, L; Goldstein, B D; Witz, G
1986-01-01
It has been proposed that a ring-opened form may be responsible for the toxicity of benzene. The present studies demonstrate that incubation of [14C]benzene with liver microsomes (obtained from male CD-1 mice treated with benzene) in the presence of NADPH results in the formation of a ring-opened product. Evidence for the identity of this product was obtained by derivatizing with 2-thiobarbituric acid (TBA), which resulted in the formation of an adduct with a 490-nm absorbance maximum. This maximum is identical to that observed after authentic trans,trans-muconaldehyde has reacted with TBA. Separation of muconaldehyde, both with and without trapping with TBA, from other benzene metabolites in the incubation mixture was accomplished by HPLC. The radioactivity profile of fractions collected during HPLC analysis contained peaks that eluted with muconaldehyde and the muconaldehyde-TBA adduct. The structure of the ring-opened product was confirmed by mass spectrometry, studies in which the HPLC peak from the microsomal incubation mixture that eluted at the retention time of authentic muconaldehyde was collected and derivatized with 2,4-dinitrophenylhydrazine. The high-resolution mass spectrum of this sample contained an ion with an m/z of 291.0729, corresponding to muconaldehyde mono-dinitrophenylhydrazone. These results indicate that benzene is metabolized in vitro to a ring-opened product identified as muconaldehyde. PMID:3464956
Clustering and Filtering Tandem Mass Spectra Acquired in Data-Independent Mode
NASA Astrophysics Data System (ADS)
Pak, Huisong; Nikitin, Frederic; Gluck, Florent; Lisacek, Frederique; Scherl, Alexander; Muller, Markus
2013-12-01
Data-independent mass spectrometry activates all ion species isolated within a given mass-to-charge window ( m/z) regardless of their abundance. This acquisition strategy overcomes the traditional data-dependent ion selection boosting data reproducibility and sensitivity. However, several tandem mass (MS/MS) spectra of the same precursor ion are acquired during chromatographic elution resulting in large data redundancy. Also, the significant number of chimeric spectra and the absence of accurate precursor ion masses hamper peptide identification. Here, we describe an algorithm to preprocess data-independent MS/MS spectra by filtering out noise peaks and clustering the spectra according to both the chromatographic elution profiles and the spectral similarity. In addition, we developed an approach to estimate the m/z value of precursor ions from clustered MS/MS spectra in order to improve database search performance. Data acquired using a small 3 m/z units precursor mass window and multiple injections to cover a m/z range of 400-1400 was processed with our algorithm. It showed an improvement in the number of both peptide and protein identifications by 8 % while reducing the number of submitted spectra by 18 % and the number of peaks by 55 %. We conclude that our clustering method is a valid approach for data analysis of these data-independent fragmentation spectra. The software including the source code is available for the scientific community.
Alexander, Anthony J; Ma, Lianjia
2009-02-27
This paper focuses on the application of RPLC x RPLC to pharmaceutical analysis and addresses the specific problem of separating co-eluting impurities/degradation products that maybe "hidden" within the peak envelope of the active pharmaceutical ingredient (API) and thus may escape detection by conventional methods. A comprehensive two-dimensional liquid chromatograph (LC x LC) was constructed from commercially available HPLC equipment. This system utilizes two independently configurable 2nd dimension binary pumping systems to deliver independent flow rates, gradient profiles and mobile phase compositions to dual Fused-Core secondary columns. Very fast gradient separations (30s total cycle time) were achieved at ambient temperature without excessive backpressure and without compromising optimal 1st dimension sampling rates. The operation of the interface is demonstrated for the analysis of a 1mg/ml standard mixture containing 0.05% of a minor component. The practicality of using RPLC x RPLC for the analysis of actual co-eluting pharmaceutical degradation products, by exploiting pH-induced changes in selectivity, is also demonstrated using a three component mixture. This mixture (an API, an oxidation product of the API at 1.0%, w/w, and a photo degradant of the API at 0.5%, w/w) was used to assess the stability indicating nature of an established LC method for analysis of the API.
Wu, Jinglan; Peng, Qijun; Arlt, Wolfgang; Minceva, Mirjana
2009-12-11
One of the conventional processes used for the recovery of citric acid from its fermentation broth is environmentally harmful and cost intensive. In this work an innovative benign process, which comprises simulated moving bed (SMB) technology and use of a tailor-made tertiary poly(4-vinylpyridine) (PVP) resin as a stationary phase is proposed. This paper focuses on a model-based design of the operation conditions for an existing pilot-scale SMB plant. The SMB unit is modeled on the basis of experimentally determined hydrodynamics, thermodynamics and mass transfer characteristics in a single chromatographic column. Three mathematical models are applied and validated for the prediction of the experimentally attained breakthrough and elution profiles of citric acid and the main impurity component (glucose). The transport dispersive model was selected for the SMB simulation and design studies, since it gives a satisfactory prediction of the elution profiles within acceptable computational time. The equivalent true moving bed (TMB) and SMB models give a good prediction of the experimentally attained SMB separation performances, obtained with a real clarified and concentrated fermentation broth as a feed mixture. The SMB separation requirements are set to at least 99.8% citric acid purity and 90% citric acid recovery in the extract stream. The complete regeneration in sections 1 and 4 is unnecessary. Therefore the net flow rates in all four SMB sections have been considered in the unit design. The influences of the operating conditions (the flow rate in each section, switching time and unit configuration) on the SMB performances were investigated systematically. The resulting SMB design provides 99.8% citric acid purity and 97.2% citric acid recovery in the extract. In addition the citric acid concentration in the extract is a half of its concentration in the pretreated fermentation broth (feed).
Hynninen, P H; Räisänen, R
2001-01-01
Preparative-scale separation of substituted anthraquinones by multiple liquid-liquid partition was studied using isopropylmethyl ketone (IMK)/aqueous phosphate buffer (aq.) as the solvent system and the Hietala apparatus with 100 partition units as the partition equipment. The lower (aq.) phase was chosen as mobile, while the upper (IMK) phase remained stationary. Hence, the principle of stepwise pH-gradient elution could be utilized to separate the components in two complex mixtures of hydroxyanthraquinones and hydroxyanthraquinone carboxylic acids, isolated from the fungus Dermocybe sanguinea. In spite of the nonlinearity of the partition isotherms for these anthraquinones, implying deviations from the Nernst partition law, remarkable separations were achieved for the components in each mixture. Every anthraquinone carboxylic acid showed markedly irregular partition behavior, appearing in the effluent as two more or less resolved concentration zones. Such splitting was attributed to the formation of relatively stable sandwich-dimers, which were in a slow equilibrium with the monomers in the more nonpolar organic phase. At lower pH-values, only the polar monomers were distributed into the mobile aqueous phase and moved forward, whereas the nonpolar sandwich-dimers remained almost entirely in the stationary organic phase and lagged behind. When the pH of the mobile aqueous phase was raised high enough, the firmly linked dimers were monomerized and emerged from the apparatus as a second concentration profile. Intermolecular hydrogen bonding and pi-pi interaction between the pi-systems of two anthraquinone molecules in a parallel orientation were considered responsible for the nonlinear and markedly irregular partition behavior of the natural anthraquinones studied. The nonlinearity of the partition behavior of the hydroxyanthraquinones lacking the carboxyl group, appeared merely as excessive broadening of the experimental concentration profile, which impaired the resolution between the components only insignificantly. Thus, e.g. the main components, dermocybin and emodin, could both be obtained from Separation 1 in a purity of at least 99%.
Romaguera, Rafael; Gómez-Hospital, Joan A; Gomez-Lara, Josep; Brugaletta, Salvatore; Pinar, Eduardo; Jiménez-Quevedo, Pilar; Gracida, Montserrat; Roura, Gerard; Ferreiro, Jose L; Teruel, Luis; Montanya, Eduard; Fernandez-Ortiz, Antonio; Alfonso, Fernando; Valgimigli, Marco; Sabate, Manel; Cequier, Angel
2016-01-11
The aim of this study was to compare the efficacy of amphilimus-eluting stents (AES) with that of everolimus-eluting stents (EES) in patients with diabetes mellitus (DM). The AES is a polymer-free drug-eluting stent that elutes sirolimus formulated with an amphiphilic carrier from laser-dug wells. This technology could be associated with a high efficacy in patients with DM. This was a multicenter, randomized, noninferiority trial. Patients with DM medically treated with oral glucose-lowering agents or insulin and de novo coronary lesions were randomized in a 1:1 fashion to AES or EES. The primary endpoint was the neointimal (NI) volume obstruction assessed by optical coherence tomography at 9-month follow-up. A total of 116 lesions in 112 patients were randomized. Overall, 40% were insulin-treated patients, with a median HbA1c of 7.3% (interquartile range: 6.7% to 8.0%). The primary endpoint, NI volume obstruction, was 11.97 ± 5.94% for AES versus 16.11 ± 18.18% for EES, meeting the noninferiority criteria (p = 0.0003). Pre-specified subgroup analyses showed a significant interaction between stent type and glycemic control (p = 0.02), with a significant reduction in NI hyperplasia in the AES group in patients with the higher HbA1c (p = 0.03). By quantitative coronary angiography, in-stent late loss was 0.14 ± 0.24 for AES versus 0.24 ± 0.57 mm for EES (p = 0.27), with a larger minimal lumen diameter at follow-up for AES (p = 0.02), mainly driven by 2 cases of occlusive restenosis in the EES group. AES are noninferior to EES for the coronary revascularization of patients with DM. These results suggest a high efficacy of the AES and may support the potential benefit of this stent in patients with DM. (A Randomized Comparison of Reservoir-Based Polymer-Free Amphilimus-Eluting Stents Versus Everolimus-Eluting Stents With Durable Polymer in Patients With Diabetes Mellitus [RESERVOIR]; NCT01710748). Copyright © 2016 American College of Cardiology Foundation. Published by Elsevier Inc. All rights reserved.
Kandzari, David E; Smits, Pieter C; Love, Michael P; Ben-Yehuda, Ori; Banai, Shmuel; Robinson, Simon D; Jonas, Michael; Kornowski, Ran; Bagur, Rodrigo; Iniguez, Andres; Danenberg, Haim; Feldman, Robert; Jauhar, Rajiv; Chandna, Harish; Parikh, Manish; Perlman, Gidon Y; Balcells, Mercedes; Markham, Peter; Ozan, Melek Ozgu; Genereux, Philippe; Edelman, Elazer R; Leon, Martin B; Stone, Gregg W
2017-10-03
The safety and efficacy of a novel cobalt alloy-based coronary stent with a durable elastomeric polymer eluting the antiproliferative agent ridaforolimus for treatment of patients with coronary artery disease is undetermined. A prospective, international 1:1 randomized trial was conducted to evaluate in a noninferiority design the relative safety and efficacy of ridaforolimus-eluting stents (RESs) and slow-release zotarolimus-eluting stents among 1919 patients undergoing percutaneous coronary intervention at 76 centers. Inclusion criteria allowed enrollment of patients with recent myocardial infarction, total occlusions, bifurcations lesions, and other complex conditions. Baseline clinical and angiographic characteristics were similar between the groups. Overall, mean age was 63.4 years, 32.5% had diabetes mellitus, and 39.7% presented with acute coronary syndromes. At 12 months, the primary end point of target lesion failure (composite of cardiac death, target vessel-related myocardial infarction, and target lesion revascularization) was 5.4% for both devices (upper bound of 1-sided 95% confidence interval 1.8%, P noninferiority =0.001). Definite/probable stent thrombosis rates were low in both groups (0.4% RES versus 0.6% zotarolimus-eluting stent, P =0.75); 13-month angiographic in-stent late lumen loss was 0.22±0.41 mm and 0.23±0.39 mm ( P noninferiority =0.004) for the RES and zotarolimus-eluting stent groups, respectively, and intravascular ultrasound percent neointimal hyperplasia was 8.10±5.81 and 8.85±7.77, respectively ( P noninferiority =0.01). In the present trial, which allowed broad inclusion criteria, the novel RESs met the prespecified criteria for noninferiority compared with zotarolimus-eluting stents for the primary end point of target lesion failure at 12 months and had similar measures of late lumen loss. These findings support the safety and efficacy of RESs in patients who are representative of clinical practice. URL: http://www.clinicaltrials.gov. Unique identifier: NCT01995487. © 2017 American Heart Association, Inc.
Protein microspheres for controlled drug delivery and related analysis of biopolymers
NASA Astrophysics Data System (ADS)
Kirk, James Forrest
Rheumatoid arthritis (RA) is a systemic disorder which manifests itself most notably in the synovial joints. In recent years, methotrexate (MTX), a foliate antagonist, has been used with some success for treatment of RA. MTX has a maximum cumulative dose beyond which it becomes dangerous to administer due primarily to liver toxicity. This unfortunate side effect has prompted research into means of delivering MTX to the synovial joint in hopes of making more efficient use of the drug. Both MTX and its sodium salt (Na-MTX) were loaded into microspheres (MS) composed of bovine serum albumin (BSA) stabilized by cross linking with dialdehydes or ferric ion. MS were prepared with two levels of drug loading at two different levels of cross linking. MTX loading densities as high as 46.8% w/w were achieved in the aldehyde cross linking system and as high as 46.3% w/w were achieved with ferric ion cross linking. Using Na-MTX, the values were 37.2% w/w and 31.7% w/w respectively. Both MTX and Na-MTX were elutable from the MS into phosphate buffered saline at 37sp°C. MTX elution from aldehyde cross linked microspheres was load dependent with ca. 60% eluted by 9 hours at low loading and ca. 60% eluted by 24 hours at high loading. In the ferric ion cross link system, the elution was independent of loading with 50% elution occurring between 20 and 48 hours. Na-MTX elution was independent of drug loading or cross link system with 50% elution occurring in less than two hours in all cases. Other investigations included the loading of mitoxantrone (NOV) and of enzyme. NOV was loaded onto BSA microspheres to a concentration of 19.3% w/w and was used successfully in the treatment of murine ovarian tumors. Acid phosphatase was successfully loaded onto and into BSA microspheres. This enzyme retained its initial activity up to four months on post-loaded spheres. The enzyme also remained active inside the microsphere as demonstrated by a substrate cleavage assay.
Waseda, Katsuhisa; Ako, Junya; Yamasaki, Masao; Koizumi, Tomomi; Sakurai, Ryota; Hongo, Yoichiro; Koo, Bon-Kwon; Ormiston, John; Worthley, Stephen G; Whitbourn, Robert J; Walters, Darren L; Meredith, Ian T; Fitzgerald, Peter J; Honda, Yasuhiro
2011-06-01
Polymer formulation may affect the efficacy of drug-eluting stents. Resolute, Endeavor, and ZoMaxx are zotarolimus-eluting stents with different stent platforms and different polymer coatings and have been tested in clinical trials. The aim of this analysis was to compare the efficacy of zotarolimus-eluting stents with different polymers. Data were obtained from the first-in man trial or first randomized trials of each stent, The Clinical RESpOnse EvaLUation of the MedTronic Endeavor CR ABT-578 Eluting Coronary Stent System in De Novo Native Coronary Artery Lesions (RESOLUTE), Randomized Controlled Trial to Evaluate the Safety and Efficacy of the Medtronic AVE ABT-578 Eluting Driver Coronary Stent in De Novo Native Coronary Artery Lesions (ENDEAVOR II), and ZoMaxx I trials. Follow-up intravascular ultrasound analyses (8 to 9 months of follow-up) were possible in 353 patients (Resolute: 88, Endeavor: 98, ZoMaxx: 82, Driver: 85). Volume index (volume/stent length) was obtained for vessel, stent, lumen, peristent plaque, and neointima. Cross-sectional narrowing was defined as neointimal area divided by stent area (%). Neointima-free frame ratio was calculated as the number of frames without intravascular ultrasound-detectable neointima divided by the total number of frames within the stent. At baseline, vessel, lumen, and peristent plaque volume index were not significantly different among the 4 stent groups. At follow-up, percent neointimal obstruction was significantly lower in Resolute compared with Endeavor, ZoMaxx, and Driver (Resolute: 3.7±4.0, Endeavor: 17.5±10.1, ZoMaxx: 14.6±8.1, Driver: 29.4±17.2%; P<0.001). Greater maximum cross-sectional narrowing and higher neointima-free frame ratio, suggesting less neointimal coverage, were observed in Resolute compared with other stent groups. Multiple regression analysis confirmed that the biodurable polymer used in Resolute independently correlated with neointimal suppression among 3 zotarolimus-eluting stents. The different polymer formulations significantly affect the relative amount of neointima for zotarolimus-eluting stents. URL: http://www.clinicaltrials.gov. Unique identifier: NCT00248079.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Repins, Ingrid; Mansfield, Lorelle; Kanevce, Ana
Band-edge effects -- including grading, electrostatic fluctuations, bandgap fluctuations, and band tails -- affect chalcogenide device efficiency. These effects now require more careful consideration as efficiencies increase beyond 20%. Several aspects of the relationships between band-edge phenomena and device performance for NREL absorbers are examined. For Cu(In,Ga)Se2 devices, recent increases in diffusion length imply changes to optimum bandgap profile. The origin, impact, and modification of electrostatic and bandgap fluctuations are also discussed. The application of the same principles to devices based on CdTe, kesterites, and emerging absorbers (Cu2SnS3, CuSbS2), considering differences in materials properties and defect formation energies, is examined.
Raman-based noninvasive metabolic profile evaluation of in vitro bovine embryos
NASA Astrophysics Data System (ADS)
dos Santos, Érika Cristina; Martinho, Herculano; Annes, Kelly; da Silva, Thais; Soares, Carlos Alexandre; Leite, Roberta Ferreira; Milazzotto, Marcella Pecora
2016-07-01
The timing of the first embryonic cell divisions may predict the ability of an embryo to establish pregnancy. Similarly, metabolic profiles may be markers of embryonic viability. However, in bovine, data about the metabolomics profile of these embryos are still not available. In the present work, we describe Raman-based metabolomic profiles of culture media of bovine embryos with different developmental kinetics (fast x slow) throughout the in vitro culture. The principal component analysis enabled us to classify embryos with different developmental kinetics since they presented specific spectroscopic profiles for each evaluated time point. We noticed that bands at 1076 cm-1 (lipids), 1300 cm-1 (Amide III), and 2719 cm-1 (DNA nitrogen bases) gave the most relevant spectral features, enabling the separation between fast and slow groups. Bands at 1001 cm-1 (phenylalanine) and 2892 cm-1 (methylene group of the polymethylene chain) presented specific patterns related to embryonic stage and can be considered as biomarkers of embryonic development by Raman spectroscopy. The culture media analysis by Raman spectroscopy proved to be a simple and sensitive technique that can be applied with high efficiency to characterize the profiles of in vitro produced bovine embryos with different development kinetics and different stages of development.
NASA Astrophysics Data System (ADS)
Pokharel, Binod; Geerts, Bart
2016-12-01
The AgI Seeding Cloud Impact Investigation (ASCII) campaign was conducted in early 2012 and 2013 over two mountain ranges in southern Wyoming to examine the impact of ground-based glaciogenic seeding on snow growth in winter orographic clouds. The campaign was supported by a network of ground-based instruments, including microwave radiometers, two profiling Ka-band Micro-Rain Radars (MRRs), a Doppler on Wheels (DOW) X-band radar, and a Parsivel disdrometer. The University of Wyoming King Air operated the profiling Wyoming Cloud Radar, the Wyoming Cloud Lidar, and in situ cloud and precipitation particle probes. The characteristics of the orographic clouds, flow field, and upstream stability profiles in 27 intensive observation periods (IOPs) are described here. A composite analysis of the impact of seeding on snow growth is presented in Part II of this study (Pokharel et al., 2017).
Wide forbidden band induced by the interference of different transverse acoustic standing-wave modes
NASA Astrophysics Data System (ADS)
Tao, Zhiyong; He, Weiyu; Xiao, Yumeng; Wang, Xinlong
2008-03-01
A non-Bragg nature forbidden band is experimentally observed in an axially symmetric hard-walled duct with a periodically varying cross section. Unlike the familiar Bragg ones, the observed bandgap is found to result from the interference of sound wave modes having different transverse standing-wave profiles, the so-called non-Bragg resonance. The experiments also show that the non-Bragg band can be comparably wider than the Bragg one; furthermore, the sound transmission loss within the band can be much more effective, exhibiting the great significance of the non-Bragg resonance in wave propagation in periodic waveguides.
Mesospheric dynamics and chemistry from SME data
NASA Technical Reports Server (NTRS)
Strobel, Darrell F.
1987-01-01
A fast Curtis matrix calculation of cooling rates due to the 15 micron band of CO2 is modified to parameterize the detailed calculations by Dickinson (1984) of infrared cooling by CO2 in the mesosphere and lower thermosphere. The calculations included separate NLTE treatment of the different 15 micron bands likely to be important for cooling. The goal was to compress the detailed properties of the different bands into a modified Curtis matrix, which represents one composite band with appropriate averaged radiative properties to allow for a simple and quick calculation of cooling rates given a temperature profile. Vertical constituent transport in the mesosphere was also studied.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Lee, W.M.G.; Chen, J.C.
1995-12-31
In this study, solid-gas partitioning coefficients of PAHs on fly ash in stack gas from a municipal incinerator were determined according to elution analysis with gas-solid chromatography. The fly ash from the electrostatic precipitator was sieved and packed into a 1/4 inch (6.3 mm) pyrex column. Elution analysis with gas-solid chromatography was conducted for three PAEs, Napthalene, Anthracene, and Pyrene. The temperature for elution analysis was in the range of 100{degrees}C to 300{degrees}C. Vg, specific retention volume obtained from elution analysis, and S, specific surface area of fly ash measured by a surface area measurement instrument were used to estimatemore » the solid-gas partitioning coefficient KR. In addition, the relationships between KR and temperature and KR and PAH concentrations were investigated.« less
Establishing conditions for the storage and elution of rabies virus RNA using FTA® cards
SAKAI, Takeo; ISHII, Ayako; SEGAWA, Takao; TAKAGI, Yukihiko; KOBAYASHI, Yuki; ITOU, Takuya
2014-01-01
The Flinders Technology Associates filter paper cards (FTA® cards) can be used to store nucleic acid from various samples and are easily portable. However, RNA is physicochemically unstable compared with DNA, and appropriate methods have not been established for storage and extraction of RNA from FTA® cards. The present study investigated the optimum conditions for storage and elution of viral RNA (vRNA) using rabies virus (RABV) applied to FTA® cards. When TE buffer was used, the elution rates of vRNA increased with the length of the elution time. When the cards were stored at −80°C or −20°C, vRNA was stable over 3 months. Degradation of vRNAs occurred following storage at 4°C and room temperature, suggesting that RNA should be extracted from cards as soon as possible if no freezer is available. When we tried to amplify vRNA from RABV-infected animal brains applied to FTA® cards and stored at −80°C for 6 months, we did not detect any amplified products with the primer set for 964 bp of RABV N gene. However, we were able to detect amplified products by increasing the elution time of vRNA from FTA® cards from 30 min to 24 hr or by changing the primer sets to amplify 290 bp of N gene. Thus, we recommend extending the elution time for damaged or low concentration samples in FTA® cards. PMID:25648208
Establishing conditions for the storage and elution of rabies virus RNA using FTA(®) cards.
Sakai, Takeo; Ishii, Ayako; Segawa, Takao; Takagi, Yukihiko; Kobayashi, Yuki; Itou, Takuya
2015-04-01
The Flinders Technology Associates filter paper cards (FTA(®) cards) can be used to store nucleic acid from various samples and are easily portable. However, RNA is physicochemically unstable compared with DNA, and appropriate methods have not been established for storage and extraction of RNA from FTA(®) cards. The present study investigated the optimum conditions for storage and elution of viral RNA (vRNA) using rabies virus (RABV) applied to FTA(®) cards. When TE buffer was used, the elution rates of vRNA increased with the length of the elution time. When the cards were stored at -80 °C or -20 °C, vRNA was stable over 3 months. Degradation of vRNAs occurred following storage at 4 °C and room temperature, suggesting that RNA should be extracted from cards as soon as possible if no freezer is available. When we tried to amplify vRNA from RABV-infected animal brains applied to FTA(®) cards and stored at -80 °C for 6 months, we did not detect any amplified products with the primer set for 964 bp of RABV N gene. However, we were able to detect amplified products by increasing the elution time of vRNA from FTA(®) cards from 30 min to 24 hr or by changing the primer sets to amplify 290 bp of N gene. Thus, we recommend extending the elution time for damaged or low concentration samples in FTA(®) cards.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Arguello, M.D.
1977-12-01
Modifications to the forced-flow chromatograph include a flow-through pH monitor to continuously monitor the pH of the final effluent and an active low-pass filter to eliminate noise in the spectrophotometric detector. All separations are performed using partially sulfonated XAD-2 as the ion exchanger. Elution of calcium and magnesium is accomplished using ammonium chloride and ethylenediammonium chloride solutions. Calcium and magnesium are detected by means of Arsenazo I and PAR-ZnEDTA color-forming reagents. Other metal ions are detected by means of PAR and Chromazurol S color-forming reagents. Calcium and magnesium distribution coefficients on partially sulfonated XAD-2 as functions of ammonium chloride andmore » ethylenediammonium chloride concentration are given together with distribution coefficients of other metal ions. Methods for the selective elution of interfering metal ions prior to the elution of calcium and magnesium are described. Beryllium and aluminum are selectively eluted with sulfosalicylic acid. Those elements forming anionic chloride complexes are selectively eluted with HCl-acetone. Nickel is selectively eluted with HCl-acetone-dimethylglyoxime. Synthetic samples containing calcium and magnesium, both alone and in combination with alkali metals, strontium, barium, beryllium, aluminum, transition metals, and rare earths, are analyzed. Hard water samples are analyzed for calcium and magnesium and the results compared to those obtained by EDTA titration, atomic absorption spectroscopy, and plasma emission spectroscopy. Several clinical serum samples are analyzed for calcium and magnesium and the results compared to those obtained by atomic absorption spectroscopy.« less
DNA Adsorption to and Elution from Silica Surfaces: Influence of Amino Acid Buffers
Vandeventer, Peter E.; Mejia, Jorge; Nadim, Ali; Johal, Malkiat S.; Niemz, Angelika
2014-01-01
Solid phase extraction and purification of DNA from complex samples typically requires chaotropic salts that can inhibit downstream polymerase amplification if carried into the elution buffer. Amino acid buffers may serve as a more compatible alternative for modulating the interaction between DNA and silica surfaces. We characterized DNA binding to silica surfaces, facilitated by representative amino acid buffers, and the subsequent elution of DNA from the silica surfaces. Through bulk depletion experiments, we found that more DNA adsorbs to silica particles out of positively compared to negatively charged amino acid buffers. Additionally, the type of the silica surface greatly influences the amount of DNA adsorbed, and the final elution yield. Quartz crystal microbalance experiments with dissipation monitoring (QCM-D) revealed multiphasic DNA adsorption out of stronger adsorbing conditions such as arginine, glycine, and glutamine, with DNA more rigidly bound during the early stages of the adsorption process. The DNA film adsorbed out of glutamate was more flexible and uniform throughout the adsorption process. QCM-D characterization of DNA elution from the silica surface indicates an uptake in water mass during the initial stage of DNA elution for the stronger adsorbing conditions, which suggests that for these conditions the DNA film is partly dehydrated during the prior adsorption process. Overall, several positively charged and polar neutral amino acid buffers show promise as an alternative to methods based on chaotropic salts for solid phase DNA extraction. PMID:23931415
Efficiency of beef extract for the recovery of poliovirus from wastewater effluents
DOE Office of Scientific and Technical Information (OSTI.GOV)
Landry, E.F.; Vaughn, J.M.; Thomas, M.Z.
1978-10-01
The efficiency of poliovirus elution from fiber glass cartridge filters (K27), epoxy-fiber glass-asbestos filters (M780), and pleated cartridge filters was assessed by using 3% beef extract (pH 9.0) or 0.1 M glycine (pH 11.5). Poliovirus type I, strain LSc, was seeded into 20 to 25 gallon (ca. 75.6 to 95.6 liter) samples of treated sewage effluent and concentrated by using a filter adsorption-elution technique. Virus elution was accomplished by using either two 600-ml portions of 3% beef extract (pH 9.0), or two 1 liter portions of 0.1 M glycine (pH 11.5). In all experiments, beef extract elution followed by organicmore » flocculation was found to be superior, yielding a mean recovery efficiency of 85%, with recoveries ranging from 68 to 100%. Elution with 0.1 M glycine (pH 11.5) followed by inorganic flocculation resulted in a mean recovery efficiency of 36%. The variable range of recoveries with beef extract could not be significantly improved by varying the type of beef extract or by extending the elution time to 30 min. Second-step reconcentration of 1 liter seeded sewage effluent and renovated wastewater samples indicated that organic flocculation was a more efficient method for virus recovery than inorganic flocculation. Beef extract concentrations of less than 3% were found to be efficient in the recovery of poliovirus from renovated wastewater.« less
Direct comparison of the short-term clinical performance of Z Guidant and Taxus stents.
Guildford, Anna; Colombo, Paola; Bruschi, Giuseppe; Bonacina, Edgardo; Klugmann, Silvio; Santin, Matteo
2010-12-03
The recent introduction of drug-eluting stents in angioplasty of atherosclerotic blood vessels has significantly reduced the risks of in-stent restenosis (ISR) [1]. Indeed, it is known that in conventional stents ISR takes place in over 20% of the cases and up to 60% when implanted in diabetic patients. Conversely, clinical trials have shown that drug-eluting stents have significantly reduced ISR. Among the drug-eluting stents available on the market, Taxus stents (Tax, Boston Scientific, USA) are among the most used devices [2]. Tax are stainless-steel stents coated with Translute, a poly(styrene-b-isobutylene-b-styrene) polymer (PSIBS) eluting Placlitaxel, an anti-mitotic drug. Clinical trials on this type of drug-eluting stents have shown an incidence of restenosis of approximately 4%. The majority of these trials were randomized studies where conventional stents and drug-eluting devices have been implanted in separate patients' cohorts. Such a randomized design, although fundamental to collect statistically-relevant data, does not allow a direct histological comparison of different stent types when implanted in the same patient and do not show the individual susceptibility to the host response especially at short-term implantation times. Here, an interesting case study is presented where two chrome-cobalt stents (Z Guidant, ZG, Guidant Corp.) and a Tax have been simultaneously implanted in the same patient in three separate coronary arteries, retrieved after only 8 weeks and histologically analysed. Copyright © 2009 Elsevier Ireland Ltd. All rights reserved.
Creasy, Arch; Lomino, Joseph; Barker, Gregory; Khetan, Anurag; Carta, Giorgio
2018-04-27
Protein retention in hydrophobic interaction chromatography is described by the solvophobic theory as a function of the kosmostropic salt concentration. In general, an increase in salt concentration drives protein partitioning to the hydrophobic surface while a decrease reduces it. In some cases, however, protein retention also increases at low salt concentrations resulting in a U-shaped retention factor curve. During gradient elution the salt concentration is gradually decreased from a high value thereby reducing the retention factor and increasing the protein chromatographic velocity. For these conditions, a steep gradient can overtake the protein in the column, causing it to rebind. Two dynamic models, one based on the local equilibrium theory and the other based on the linear driving force approximation, are presented. We show that the normalized gradient slope determines whether the protein elutes in the gradient, partially elutes, or is trapped in the column. Experimental results are presented for two different monoclonal antibodies and for lysozyme on Capto Phenyl (High Sub) resin. One of the mAbs and lysozyme exhibit U-shaped retention factor curves and for each, we determine the critical gradient slope beyond which 100% recovery is no longer possible. Elution with a reverse gradient is also demonstrated at low salt concentrations for these proteins. Understanding this behavior has implications in the design of gradient elution since the gradient slope impacts protein recovery. Copyright © 2018 Elsevier B.V. All rights reserved.
Park, Duk-Woo; Park, Seung-Jung
2017-06-01
For nearly half a century, coronary artery bypass grafting has been the standard treatment for patients with obstructive left main coronary artery (LMCA) disease. However, there has been considerable evolution in the field of percutaneous coronary intervention, and especially, percutaneous coronary intervention for LMCA disease has been rapidly expanded with adoption of drug-eluting stents. Some, but not all randomized trials, have shown that percutaneous coronary intervention with drug-eluting stents might be a suitable alternative for selected patients with LMCA disease instead of bypass surgery. However, none of previous trials involving early-generation drug-eluting stents was sufficiently powered and comparative trials using contemporary drug-eluting stents were limited. Recently, primary results of 2 new trials of EXCEL (Evaluation of XIENCE Everolimus Eluting Stent Versus Coronary Artery Bypass Surgery for Effectiveness of Left Main Revascularization) and NOBLE (Nordic-Baltic-British Left Main Revascularization Study) were reported. However, these trials showed conflicting results, which might pose uncertainty on the optimal revascularization strategy for LMCA disease. In this article, with the incorporation of a key review on evolution of LMCA treatment, we summarize the similarity or disparity of the EXCEL and NOBLE trials, focus on how they relate to previous trials in the field, and finally speculate on how the treatment strategy may be changed or recommended for LMCA treatment. © 2017 American Heart Association, Inc.
Surface correlation effects in two-band strongly correlated slabs.
Esfahani, D Nasr; Covaci, L; Peeters, F M
2014-02-19
Using an extension of the Gutzwiller approximation for an inhomogeneous system, we study the two-band Hubbard model with unequal band widths for a slab geometry. The aim is to investigate the mutual effect of individual bands on the spatial distribution of quasi-particle weight and charge density, especially near the surface of the slab. The main effect of the difference in band width is the presence of two different length scales corresponding to the quasi-particle profile of each band. This is enhanced in the vicinity of the critical interaction of the narrow band where an orbitally selective Mott transition occurs and a surface dead layer forms for the narrow band. For the doped case, two different regimes of charge transfer between the surface and the bulk of the slab are revealed. The charge transfer from surface/center to center/surface depends on both the doping level and the average relative charge accumulated in each band. Such effects could also be of importance when describing the accumulation of charges at the interface between structures made of multi-band strongly correlated materials.
Data-Rate Performance and Coverage of the Sub-Band Vectoring for VDSL 35b Profile
NASA Astrophysics Data System (ADS)
Giuliano, Romeo; Mazzenga, Franco; Vatalaro, Francesco
2017-05-01
Vectoring, used in VDSL2 to counteract FEXT, becomes less effective, or even ineffective, when users belong to different vectoring groups. This situation is common when the Regulator imposes sub-loop unbundling and users of uncoordinated service providers cause alien-FEXT. The sub-band vectoring (SBV) technique introduced here, avoids this situation and retains the vectoring benefits. We show SBV allows achieving up to 150 Mbit/s per user in downstream at 200 m from cabinet for VDSL2 profile-35b, with two concurrent service providers. We also introduce the concept of data-rate coverage representing the users' percentage served at a given data-rate in the area.
Energy Conservation in Optical Fibers With Distributed Brick-Walls Filters
NASA Astrophysics Data System (ADS)
Garcia, Javier; Ghozlan, Hassan; Kramer, Gerhard
2018-05-01
A band-pass filtering scheme is proposed to mitigate spectral broadening and channel coupling in the Nonlinear Schr\\"odinger (NLS) fiber optic channel. The scheme is modeled by modifying the NLS Equation to include an attenuation profile with multiple brick-wall filters centered at different frequencies. It is shown that this brick-walls profile conserves the total in-band energy of the launch signal. Furthermore, energy fluctuations between the filtered channels are characterized, and conditions on the channel spacings are derived that ensure energy conservation in each channel. The maximum spectral efficiency of such a system is derived, and a constructive rule for achieving it using Sidon sequences is provided.
NASA Astrophysics Data System (ADS)
Ito, S.; Feng, B.; Arita, M.; Someya, T.; Chen, W.-C.; Takayama, A.; Iimori, T.; Namatame, H.; Taniguchi, M.; Cheng, C.-M.; Tang, S.-J.; Komori, F.; Matsuda, I.
2018-04-01
Alkali-metal adsorption on the surface of materials is widely used for in situ surface electron doping, particularly for observing unoccupied band structures by angle-resolved photoemission spectroscopy (ARPES). However, the effects of alkali-metal atoms on the resulting band structures have yet to be fully investigated, owing to difficulties in both experiments and calculations. Here, we combine ARPES measurements on cesium-adsorbed ultrathin bismuth films with first-principles calculations of the electronic charge densities and demonstrate a simple method to evaluate alkali-metal induced band deformation. We reveal that deformation of bismuth surface bands is directly correlated with vertical charge-density profiles at each electronic state of bismuth. In contrast, a change in the quantized bulk bands is well described by a conventional rigid-band-shift picture. We discuss these two aspects of the band deformation holistically, considering spatial distributions of the electronic states and cesium-bismuth hybridization, and provide a prescription for applying alkali-metal adsorption to a wide range of materials.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Zheng, Zheng; Thilker, David A.; Heckman, Timothy M.
2015-02-20
We present the results of an analysis of Pan-STARRS1 Medium Deep Survey multi-band (grizy) images of a sample of 698 low-redshift disk galaxies that span broad ranges in stellar mass, star-formation rate, and bulge/disk ratio. We use population synthesis spectral energy distribution fitting techniques to explore the radial distribution of the light, color, surface mass density, mass/light ratio, and age of the stellar populations. We characterize the structure and stellar content of the galaxy disks out to radii of about twice Petrosian r {sub 90}, beyond which the halo light becomes significant. We measure normalized radial profiles for sub-samples ofmore » galaxies in three bins each of stellar mass and concentration. We also fit radial profiles to each galaxy. The majority of galaxies have down-bending radial surface brightness profiles in the bluer bands with a break radius at roughly r {sub 90}. However, they typically show single unbroken exponentials in the reddest bands and in the stellar surface mass density. We find that the mass/light ratio and stellar age radial profiles have a characteristic 'U' shape. There is a good correlation between the amplitude of the down-bend in the surface brightness profile and the rate of the increase in the M/L ratio in the outer disk. As we move from late- to early-type galaxies, the amplitude of the down-bend and the radial gradient in M/L both decrease. Our results imply a combination of stellar radial migration and suppression of recent star formation can account for the stellar populations of the outer disk.« less
Retrievals of heavy ozone with MIPAS
NASA Astrophysics Data System (ADS)
Jonkheid, Bastiaan; Röckmann, Thomas; Glatthor, Norbert; Janssen, Christof; Stiller, Gabriele; von Clarmann, Thomas
2016-12-01
A method for retrieval of 18O-substituted isotopomers of O3 in the stratosphere with the Michelson Interferometer for Passive Atmospheric Sounding (MIPAS) is presented. Using a smoothing regularisation constraint, volume mixing ratio profiles are retrieved for the main isotopologue and the symmetric and asymmetric isotopomers of singly substituted O3. For the retrieval of the heavy isotopologues, two microwindows in the MIPAS A band (685-970 cm-1) and six in the AB band (1020-1170 cm-1) are used. As the retrievals are performed as perturbations on the previously retrieved a priori profiles, the vertical resolution of the individual isotopomer profiles is very similar, which is important when calculating the ratio between two isotopomers. The performance of the method is evaluated using 1044 vertical profiles recorded with MIPAS on 1 July 2003. The mean values are separated by latitude bands, along with estimates of their uncertainties. The asymmetric isotopomer shows a mean enrichment of ˜ 8 %, with a vertical profile that increases up to 33 km and decreases at higher altitudes. This decrease with altitude is a robust result that does not depend on retrieval settings, and it has not been reported clearly in previously published datasets. The symmetric isotopomer is considerably less enriched, with mean values around 3 % and with a large spread. In individual retrievals the uncertainty of the enrichment is dominated by the measurement noise (2-4 %), which can be reduced by averaging multiple retrievals; systematic uncertainties linked to the retrieval are generally small at ˜ 0.5 %, but this is likely underestimated because the uncertainties in key spectroscopic parameters are unknown. The variabilities in the retrieval results are largest for the Southern Hemisphere.
Berggrund, Malin; Ekman, Daniel; Gustavsson, Inger; Sundfeldt, Karin; Olovsson, Matts; Enroth, Stefan; Gyllensten, Ulf
2016-01-01
The indicating FTA elute micro card™ has been developed to collect and stabilize the nucleic acid in biological samples and is widely used in human and veterinary medicine and other disciplines. This card is not recommended for protein analyses, since surface treatment may denature proteins. We studied the ability to analyse proteins in human plasma and vaginal fluid as applied to the indicating FTA elute micro card™ using the sensitive proximity extension assay (PEA). Among 92 proteins in the Proseek Multiplex Oncology Iv2 panel, 87 were above the limit of detection (LOD) in liquid plasma and 56 among 92 above LOD in plasma applied to FTA cards. Washing and protein elution protocols were compared to identify an optimal method. Liquid-based cytology samples showed a lower number of proteins above LOD than FTA cards with vaginal fluid samples applied. Our results demonstrate that samples applied to the indicating FTA elute micro card™ are amendable to protein analyses, given that a sensitive protein detection assay is used. The results imply that biological samples applied to FTA cards can be used for DNA, RNA and protein detection. PMID:28936257
Berggrund, Malin; Ekman, Daniel; Gustavsson, Inger; Sundfeldt, Karin; Olovsson, Matts; Enroth, Stefan; Gyllensten, Ulf
2016-01-01
The indicating FTA elute micro card™ has been developed to collect and stabilize the nucleic acid in biological samples and is widely used in human and veterinary medicine and other disciplines. This card is not recommended for protein analyses, since surface treatment may denature proteins. We studied the ability to analyse proteins in human plasma and vaginal fluid as applied to the indicating FTA elute micro card™ using the sensitive proximity extension assay (PEA). Among 92 proteins in the Proseek Multiplex Oncology Iv2 panel, 87 were above the limit of detection (LOD) in liquid plasma and 56 among 92 above LOD in plasma applied to FTA cards. Washing and protein elution protocols were compared to identify an optimal method. Liquid-based cytology samples showed a lower number of proteins above LOD than FTA cards with vaginal fluid samples applied. Our results demonstrate that samples applied to the indicating FTA elute micro card™ are amendable to protein analyses, given that a sensitive protein detection assay is used. The results imply that biological samples applied to FTA cards can be used for DNA, RNA and protein detection.
The elution of colistimethate sodium from polymethylmethacrylate and calcium phosphate cement beads.
Waterman, Paige; Barber, Melissa; Weintrob, Amy C; VanBrakle, Regina; Howard, Robin; Kozar, Michael P; Andersen, Romney; Wortmann, Glenn
2012-06-01
Gram-negative bacilli resistance to all antibiotics, except for colistimethate sodium (CMS), is an emerging healthcare concern. Incorporating CMS into orthopedic cement to treat bone and soft-tissue infections due to these bacteria is attractive, but the data regarding the elution of CMS from cement are conflicting. The in vitro analysis of the elution of CMS from polymethylmethacrylate (PMMA) and calcium phosphate (CP) cement beads is reported. PMMA and CP beads containing CMS were incubated in phosphate-buffered saline and the eluate sampled at sequential time points. The inhibition of the growth of a strain of Acinetobacter baumannii complex by the eluate was measured by disk diffusion and microbroth dilution assays, and the presence of CMS in the eluate was measured by mass spectroscopy. Bacterial growth was inhibited by the eluate from both PMMA and CP beads. Mass spectroscopy demonstrated greater elution of CMS from CP beads than PMMA beads. The dose of CMS in PMMA beads was limited by failure of bead integrity. CMS elutes from both CP and PMMA beads in amounts sufficient to inhibit bacterial growth in vitro. The clinical implications of these findings require further study.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Seo, Seong-Heon; Wi, H. M.; Lee, W. R.
2013-08-15
Frequency modulation reflectometer has been developed to measure the plasma density profile of the Korea Superconducting Tokamak Advanced Research tokamak. Three reflectometers are operating in extraordinary polarization mode in the frequency range of Q band (33.6–54 GHz), V band (48–72 GHz), and W band (72–108 GHz) to measure the density up to 7 × 10{sup 19} m{sup −3} when the toroidal magnetic field is 2 T on axis. The antenna is installed inside of the vacuum vessel. A new vacuum window is developed by using 50 μm thick mica film and 0.1 mm thick gold gasket. The filter bank ofmore » low pass filter, notch filter, and Faraday isolator is used to reject the electron cyclotron heating high power at attenuation of 60 dB. The full frequency band is swept in 20 μs. The mixer output is directly digitized with sampling rate of 100 MSamples/s. The phase is obtained by using wavelet transform. The whole hardware and software system is described in detail and the measured density profile is presented as a result.« less
Jimsphere wind and turbulence exceedance statistic
NASA Technical Reports Server (NTRS)
Adelfang, S. I.; Court, A.
1972-01-01
Exceedance statistics of winds and gusts observed over Cape Kennedy with Jimsphere balloon sensors are described. Gust profiles containing positive and negative departures, from smoothed profiles, in the wavelength ranges 100-2500, 100-1900, 100-860, and 100-460 meters were computed from 1578 profiles with four 41 weight digital high pass filters. Extreme values of the square root of gust speed are normally distributed. Monthly and annual exceedance probability distributions of normalized rms gust speeds in three altitude bands (2-7, 6-11, and 9-14 km) are log-normal. The rms gust speeds are largest in the 100-2500 wavelength band between 9 and 14 km in late winter and early spring. A study of monthly and annual exceedance probabilities and the number of occurrences per kilometer of level crossings with positive slope indicates significant variability with season, altitude, and filter configuration. A decile sampling scheme is tested and an optimum approach is suggested for drawing a relatively small random sample that represents the characteristic extreme wind speeds and shears of a large parent population of Jimsphere wind profiles.
Kingsley, I.S.
1987-01-06
A process and apparatus are disclosed for the separation of complex mixtures of carbonaceous material by sequential elution with successively stronger solvents. In the process, a column containing glass beads is maintained in a fluidized state by a rapidly flowing stream of a weak solvent, and the sample is injected into this flowing stream such that a portion of the sample is dissolved therein and the remainder of the sample is precipitated therein and collected as a uniform deposit on the glass beads. Successively stronger solvents are then passed through the column to sequentially elute less soluble materials. 1 fig.
Drug-eluting coronary stents – focus on improved patient outcomes
Jaffery, Zehra; Prasad, Amit; Lee, John H; White, Christopher J
2011-01-01
The development of stent has been a major advance in the treatment of obstructive coronary artery disease since the introduction of balloon angioplasty. Subsequently, neointimal hyperplasia within the stent leading to in-stent restenosis emerged as a major obstacle in long-term success of percutaneous coronary intervention. Recent introduction of drug-eluting stents is a major breakthrough to tackle this problem. This review article summarizes stent technology, reviews progress of drug-eluting stents and discusses quality of life, patient satisfaction, and acceptability of percutaneous coronary intervention. PMID:22915977
Chemical Modification of the Olfactory Receptor Epithelium of Vertebrate Species
1990-06-28
Pre-column Derivatization Procedure: 1.0 mL of the Jeffamine solution was mixed with 1.0 mL of NaCN, 5.0 mL of phosphate buffer pH 9.5 followed by 1.0...running buffer. All the unprotonated components elute at the same time because their rate of elution is controlled only by the rate of electroosmotic ...elecarosomotic mobility under our experimental conditions. Using an average elution time of 22.2 min the measured electroosmotic mobility is 1.3 x 10-4 cm2
Purification of the Alpha Glycerophosphate Oxidase from African Trypanosomes
1988-02-02
remo~val of all unattached enzymes , the GPO would be eluted with a buffer containing the substrate a- GP. Cyancqen bromide activated Sepharose 4B was...released upon eluticn with a buffer cm-xtaining 100 rm of a-GP. Unfortunately, in these experiments, trypan blue was eluted from the colmn and the enzyme ...borate buffer (pH 8.0), there was no leakage of the ligand but the GPO was not released fram the colun when eluted with 10aM c-GP. Enzyme assays of the
Bailey-Shaw, Y A; Golden, K D; Pearson, A G M; Porter, R B R
2012-09-01
This paper describes the determination of fatty acid composition of coffee, citrus and rum distillery wastes using reversed-phase high-performance liquid chromatography (RP-HPLC). Lipid extracts of the waste samples are derivatized with phenacyl bromide and their phenacyl esters are separated on a C8 reversed-phase column by using continuous gradient elution with water and acetonitrile. The presence of saturated and unsaturated fatty acids in quantifiable amounts in the examined wastes, as well as the high percentage recoveries, are clear indications that these wastes have potential value as inexpensive sources of lipids. The HPLC procedures described here could be adopted for further analysis of materials of this nature.
Boutaoui, Nassima; Zaiter, Lahcene; Benayache, Fadila; Benayache, Samir; Carradori, Simone; Cesa, Stefania; Giusti, Anna Maria; Campestre, Cristina; Menghini, Luigi; Innosa, Denise; Locatelli, Marcello
2018-02-20
This study was performed to evaluate the metabolite recovery from different extraction methods applied to Thymus algeriensis aerial parts. A high-performance liquid chromatographic method using photodiode array detector with gradient elution has been developed and validated for the simultaneous estimation of different phenolic compounds in the extracts and in their corresponding purified fractions. The experimental results show that microwave-assisted aqueous extraction for 15 min at 100 °C gave the most phenolics-enriched extract, reducing extraction time without degradation effects on bioactives. Sixteen compounds were identified in this extract, 11 phenolic compounds and five flavonoids, all known for their biological activities. Color analysis and determination of chlorophylls and carotenoids implemented the knowledge of the chemical profile of this plant.
Technology optimization techniques for multicomponent optical band-pass filter manufacturing
NASA Astrophysics Data System (ADS)
Baranov, Yuri P.; Gryaznov, Georgiy M.; Rodionov, Andrey Y.; Obrezkov, Andrey V.; Medvedev, Roman V.; Chivanov, Alexey N.
2016-04-01
Narrowband optical devices (like IR-sensing devices, celestial navigation systems, solar-blind UV-systems and many others) are one of the most fast-growing areas in optical manufacturing. However, signal strength in this type of applications is quite low and performance of devices depends on attenuation level of wavelengths out of operating range. Modern detectors (photodiodes, matrix detectors, photomultiplier tubes and others) usually do not have required selectivity or have higher sensitivity to background spectrum at worst. Manufacturing of a single component band-pass filter with high attenuation level of wavelength is resource-intensive task. Sometimes it's not possible to find solution for this problem using existing technologies. Different types of filters have technology variations of transmittance profile shape due to various production factors. At the same time there are multiple tasks with strict requirements for background spectrum attenuation in narrowband optical devices. For example, in solar-blind UV-system wavelengths above 290-300 nm must be attenuated by 180dB. In this paper techniques of multi-component optical band-pass filters assembly from multiple single elements with technology variations of transmittance profile shape for optimal signal-tonoise ratio (SNR) were proposed. Relationships between signal-to-noise ratio and different characteristics of transmittance profile shape were shown. Obtained practical results were in rather good agreement with our calculations.
Kandzari, David E.; Smits, Pieter C.; Love, Michael P.; Ben-Yehuda, Ori; Banai, Shmuel; Rob-inson, Simon D.; Jonas, Michael; Kornowski, Ran; Bagur, Rodrigo; Iniguez, Andres; Danenberg, Haim; Feldman, Robert; Jauhar, Rajiv; Chandna, Harish; Parikh, Manish; Perlman, Gidon Y.; Balcells, Mer-cedes; Markham, Peter; Ozan, Melek Ozgu; Genereux, Philippe; Edelman, Elazer R.; Leon, Martin B.; Stone, Gregg W.
2018-01-01
BACKGROUND The safety and efficacy of a novel cobalt alloy-based coronary stent with a durable elastomeric polymer eluting the antiproliferative agent ridaforolimus for treatment of patients with coronary artery disease is undetermined. METHODS A prospective, international 1:1 randomized trial was conducted to evaluate in a noninferiority design the relative safety and efficacy of ridaforolimus-eluting stents (RESs) and slow-release zotarolimus-eluting stents among 1919 patients undergoing percutaneous coronary intervention at 76 centers. Inclusion criteria allowed enrollment of patients with recent myocardial infarction, total occlusions, bifurcations lesions, and other complex conditions. RESULTS Baseline clinical and angiographic characteristics were similar between the groups. Overall, mean age was 63.4 years, 32.5% had diabetes mellitus, and 39.7% presented with acute coronary syndromes. At 12 months, the primary end point of target lesion failure (composite of cardiac death, target vessel-related myocardial infarction, and target lesion revascularization) was 5.4% for both devices (upper bound of 1-sided 95% confidence interval 1.8%, Pnoninferiority=0.001). Definite/probable stent thrombosis rates were low in both groups (0.4% RES versus 0.6% zotarolimus-eluting stent, P=0.75); 13-month angiographic in-stent late lumen loss was 0.22±0.41 mm and 0.23±0.39 mm (Pnoninferiority=0.004) for the RES and zotarolimus-eluting stent groups, respectively, and intravascular ultrasound percent neointimal hyperplasia was 8.10±5.81 and 8.85±7.77, respectively (Pnoninferiority=0.01). CONCLUSIONS In the present trial, which allowed broad inclusion criteria, the novel RESs met the prespecified criteria for noninferiority compared with zotarolimus-eluting stents for the primary end point of target lesion failure at 12 months and had similar measures of late lumen loss. These findings support the safety and efficacy of RESs in patients who are representative of clinical practice. CLINICAL TRIAL REGISTRATION URL: http://www.clinicaltrials.gov. Unique identifier: NCT01995487. PMID:28794001
Degree of conversion and monomer elution of CQ/amine and TPO adhesives.
Pongprueksa, Pong; Miletic, Vesna; Janssens, Henriette; Van Landuyt, Kirsten L; De Munck, Jan; Godderis, Lode; Van Meerbeek, Bart
2014-06-01
To evaluate the effect of photo-initiator on the degree of conversion (DC) and elution of Bis-GMA and HEMA for 8 one-step adhesive formulations. We used Scotchbond Universal ('SBU-CQ/amine_4.0', 3M ESPE), containing about 2wt% camphorquinone (CQ) and 2wt% ethyl-4-dimethylamino benzoate (EDMAB), an experimental 'SBU-TPO_2.1' version, containing 2.1wt% diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide (TPO), and 6 experimental LUB adhesives (Kuraray Noritake), namely 'LUB-CQ/amine_0.7', 'LUB-CQ/amine_1.4', 'LUB-CQ/amine_4.0', 'LUB-TPO_0.35', 'LUB-TPO_0.7' and 'LUB-TPO_2.0', respectively containing 0.35wt% CQ and 0.35wt% EDMAB, 0.7wt% CQ and 0.7wt% EDMAB, 2.0wt% CQ and 2.0wt% EDMAB, 0.35wt% TPO, 0.7wt% TPO, and 2.0wt% TPO. DC was measured using micro-Raman spectroscopy. Additional specimens were immersed in ethanol for 24h to determine the elution of Bis-GMA and HEMA using HPLC. DC of the respective SBU and LUB adhesives was alike at high photo-initiator concentration. At low concentration, TPO was significantly more efficient than CQ/amine (LUB adhesives only). A statistically significant positive photo-initiator concentration effect on DC was noted for both CQ/amine and TPO (LUB adhesives only). A statistically significant inverse photo-initiator concentration effect on HEMA elution was noted for both the CQ/amine- and TPO-containing LUB adhesives. A significantly strong correlation was found between DC and Bis-GMA elution (R(2)=0.744, p=0.026), and between DC and HEMA elution (R(2)=0.913, p=0.002) for the LUB adhesives. The photo-initiator kind and concentration affect DC and the Bis-GMA/HEMA elution. TPO can be used as an alternative photo-initiator for CQ/amine. Copyright © 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
NASA Technical Reports Server (NTRS)
Usry, J. W.
1983-01-01
Wind shear statistics were calculated for a simulated set of wind profiles based on a proposed standard wind field data base. Wind shears were grouped in altitude in altitude bands of 100 ft between 100 and 1400 ft and in wind shear increments of 0.025 knot/ft. Frequency distributions, means, and standard deviations for each altitude band were derived for the total sample were derived for both sets. It was found that frequency distributions in each altitude band for the simulated data set were more dispersed below 800 ft and less dispersed above 900 ft than those for the measured data set. Total sample frequency of occurrence for the two data sets was about equal for wind shear values between +0.075 knot/ft, but the simulated data set had significantly larger values for all wind shears outside these boundaries. It is shown that normal distribution in both data sets neither data set was normally distributed; similar results are observed from the cumulative frequency distributions.
NASA Astrophysics Data System (ADS)
Tomar, Ruchi; Wadehra, Neha; Budhiraja, Vaishali; Prakash, Bhanu; Chakraverty, S.
2018-01-01
To characterize the physical properties of thin films without ambiguity and design interface with new functionalities, it is essential to have detailed knowledge of physical properties and appropriate estimation of the band profile of perovskite oxide substrates. We have developed and demonstrated a chemical free unified framework to realize single terminated surface of KTaO3, (LaAlO3)0.3 (Sr2AlTaO6)0.7 and SrTiO3 (001) oriented single crystals. The electronic band line-up of these single crystal substrates, using a combination of optical spectroscopy and Kelvin Probe Force Microscopy, has been constructed. A polar-polar interface of KTaO3 and LaBO3 (B-Transition metal ion) before and after the possible surface/electronic reconstruction has also been schematically presented.
Tattawasart, U; Maillard, J Y; Furr, J R; Russell, A D
2000-11-01
Changes in outer membrane proteins (OMP) and lipopolysaccharide (LPS) in cells of strains of Pseudomonas stutzeri sensitive and resistant to chlorhexidine diacetate (CHA) or cetylpyridinium chloride (CPC) have been examined. Four of five CHA-resistant strains had alterations in OMP profiles, including the expression of two additional protein bands. All the CPC-resistant strains had altered OMP profiles but the changes varied from strain to strain. Loss of the fastest-migrating bands was observed in the LPS from CHX-resistant strains. In strain JM 302R with high-level CHX resistance (minimal inhibitory concentration 100 mg/l as opposed to 2.5 mg/l in the parent-strain, JM 302), all the fast-migrating bands were lost and the strain showed 'cross-resistance' to polymyxin, gentamicin and ethylenediamine tetraacetic acid. It is however, possible that the altered LPS patterns reflect a response to alterations in other components rather than being directly associated per se with the enhanced resistance.
GOSAT TIR radiometric validation toward simultaneous GHG column and profile observation
NASA Astrophysics Data System (ADS)
Kataoka, F.; Knuteson, R. O.; Kuze, A.; Shiomi, K.; Suto, H.; Saitoh, N.
2015-12-01
The Greenhouse gases Observing SATellite (GOSAT) was launched on January 2009 and continues its operation for more than six years. The thermal and near infrared sensor for carbon observation Fourier-Transform Spectrometer (TANSO-FTS) onboard GOSAT measures greenhouse gases (GHG), such as CO2 and CH4, with wide and high resolution spectra from shortwave infrared (SWIR) to thermal infrared (TIR). This instrument has the advantage of being able to measure simultaneously the same field of view in different spectral ranges. The combination of column-GHG form SWIR band and vertical profile-GHG from TIR band provide better understanding and distribution of GHG, especially in troposphere. This work describes the radiometric validation and sensitivity analysis of TANSO-FTS TIR spectra, especially CO2, atmospheric window and CH4 channels with forward calculation. In this evaluation, we used accurate in-situ dataset of the HIPPO (HIAPER Pole-to-Pole Observation) airplane observation data and GOSAT vicarious calibration and validation campaign data in Railroad Valley, NV. The HIPPO aircraft campaign had taken accurate atmospheric vertical profile dataset (T, RH, O3, CO2, CH4, N2O, CO) approximately pole-to-pole from the surface to the tropopause over the ocean. We implemented these dataset for forward calculation and made the spectral correction model with respect to wavenumber and internal calibration blackbody temperature The GOSAT vicarious calibration campaign have conducted every year since 2009 near summer solstice in Railroad Valley, where high-temperature desert site. In this campaign, we have measured temperature and humidity by a radiosonde and CO2, CH4 and O3 profile by the AJAX airplane at the time of the GOSAT overpass. Sometimes, the GHG profiles over the Railroad Valley show the air mass advection in mid-troposphere depending on upper wind. These advections bring the different concentration of GHG in lower and upper troposphere. Using these cases, we made sensitivity analysis of TANSO-FTS TIR band in troposphere changing in-situ GHG profiles.
[Studies on the process of Herba Clinopodii saponins purified with macroporous adsorption resin].
Zhang, Yi; Yan, Dan; Han, Yumei
2005-10-01
To study the technological parameters of the purification process of saponins with macroporous adsorption resin. The adsorptive characteristics and elutive parameters of the process were studied by taking the elutive and purified ratio of saponins as markers. 11.4 ml of the extraction of Herba Clinopodii (crude drugs 0.2 g/ml) was purified with a column of macroporous adsorption resin (phi15 mm x H90 mm, dry weight 2.5 g) and washed with 3BV of distilled water, then eluted with 3BV of 30% ethanol and 3BV of 70% ethanol. Most of saponins were collected in the 70% ethanol. With macroporous adsorption resin adsorbing and purifying,the elutive ratio of saponins is 86.8% and the purity reaches 153.2%. So this process of applying macroporous adsorption resin to adsorb and purify Saponins is feasible.
[Hemapheresis using vesicular plant separation materials].
Mavrina, L; Ehwald, R; Matthes, G; Stamminger, G
1990-01-01
The present paper deals with the separation of cells from soluble compounds of blood by means of exclusion chromatography using a recently described vesicular packing material made from the cell wall framework of the small duckweed Wolffia arrhiza. The cells of the periphere blood are hardly retarded in passing through a packing of the vesicular material and eluted as sharp peak at an elution volume which is near to 30% of the column volume. The behavior of cells is similar to that of the excluded high molecular weight plasma proteins (e.g. serumalbumin). Low molecular weight solutes (e.g. salts, glucose, urea, kreatinin), but also substances of considerable molecular weight (e.g. myoglobin and Vitamin B12) which are usually difficult to separate by dialysis from serum, are eluted at nearly 100% of the packing volume and may be separated completely from cells and high molecular weight proteins. In vitro-Tests did not show a reduced vitality of eluted blood cells.
Painting blood vessels and atherosclerotic plaques with an adhesive drug depot
Kastrup, Christian J.; Nahrendorf, Matthias; Figueiredo, Jose Luiz; Lee, Haeshin; Kambhampati, Swetha; Lee, Timothy; Cho, Seung-Woo; Gorbatov, Rostic; Iwamoto, Yoshiko; Dang, Tram T.; Dutta, Partha; Yeon, Ju Hun; Cheng, Hao; Pritchard, Christopher D.; Vegas, Arturo J.; Siegel, Cory D.; MacDougall, Samantha; Okonkwo, Michael; Thai, Anh; Stone, James R.; Coury, Arthur J.; Weissleder, Ralph; Langer, Robert; Anderson, Daniel G.
2012-01-01
The treatment of diseased vasculature remains challenging, in part because of the difficulty in implanting drug-eluting devices without subjecting vessels to damaging mechanical forces. Implanting materials using adhesive forces could overcome this challenge, but materials have previously not been shown to durably adhere to intact endothelium under blood flow. Marine mussels secrete strong underwater adhesives that have been mimicked in synthetic systems. Here we develop a drug-eluting bioadhesive gel that can be locally and durably glued onto the inside surface of blood vessels. In a mouse model of atherosclerosis, inflamed plaques treated with steroid-eluting adhesive gels had reduced macrophage content and developed protective fibrous caps covering the plaque core. Treatment also lowered plasma cytokine levels and biomarkers of inflammation in the plaque. The drug-eluting devices developed here provide a general strategy for implanting therapeutics in the vasculature using adhesive forces and could potentially be used to stabilize rupture-prone plaques. PMID:23236189
Fast "hyperlayer" separation development in sedimentation field flow fractionation.
Kassab, James R; Cardot, Philippe J P; Zahoransky, Richard A; Battu, Serge
2005-11-05
Specific prototypes of sedimentation field flow fractionation devices (SdFFF) have been developed with relative success for cell sorting. However, no data are available to compare these apparatus with commercial ones. In order to compare with other devices mainly used for non-biological species, biocompatible systems were used for standard particle (latex: 3-10 microm of different size dispersities) separation development. In order to enhance size dependent separations, channels of reduced thickness were used (80 and 100 microm) and channel/carrier-phase equilibration procedures were necessary. For sample injection, the use of inlet tubing linked to the FFF accumulation wall, common for cell sorting, can be extended to latex species when they are eluted in the Steric Hyperlayer elution mode. It avoids any primary relaxation steps (stop flow injection procedure) simplifying series of elution processing. Mixtures composed of four different monodispersed latex beads can be eluted in 6 min with 100 microm channel thickness.
Enhancing Stent Effectiveness with Nanofeatures
Bassous, Nicole; Cooke, John P.; Webster, Thomas J.
2016-01-01
Drug-eluting stents are an effective therapy for symptomatic arterial obstructions, substantially reducing the incidence of restenosis by suppressing the migration and proliferation of vascular smooth muscle cells into the intima. However, current drug-eluting stents also inhibit the growth of endothelial cells, which are required to cover the vascular stent to reduce an excessive inflammatory response. As a result, the endothelial lining of the lumen is not regenerated. Since the loss of this homeostatic monolayer increases the risk of thrombosis, patients with drug-eluting stents require long-term antithrombotic therapy. Thus, there is a need for improved devices with enhanced effectiveness and physiological compatibility towards endothelial cells. Current developments in nanomaterials may enhance the function of commercially available vascular devices. In particular, modified design schemes might incorporate nanopatterns or nanoparticle-eluting features that reduce restenosis and enhance re-endothelialization. The intent of this review is to discuss emerging nanotechnologies that will improve the performance of vascular stents. PMID:27826371
NASA Astrophysics Data System (ADS)
Tanaka, Takahisa; Uchida, Ken
2018-06-01
Band tails in heavily doped semiconductors are one of the important parameters that determine transfer characteristics of tunneling field-effect transistors. In this study, doping concentration and doing profile dependences of band tails in heavily doped Si nanowires were analyzed by a nonequilibrium Green function method. From the calculated band tails, transfer characteristics of nanowire tunnel field-effect transistors were numerically analyzed by Wentzel–Kramer–Brillouin approximation with exponential barriers. The calculated transfer characteristics demonstrate that the band tails induced by dopants degrade the subthreshold slopes of Si nanowires from 5 to 56 mV/dec in the worst case. On the other hand, surface doping leads to a high drain current while maintaining a small subthreshold slope.
Band gap in tubular pillar phononic crystal plate.
Shu, Fengfeng; Liu, Yongshun; Wu, Junfeng; Wu, Yihui
2016-09-01
In this paper, a phononic crystal (PC) plate with tubular pillars is presented and investigated. The band structures and mode displacement profiles are calculated by using finite element method. The result shows that a complete band gap opens when the ratio of the pillar height to the plate thickness is about 1.6. However, for classic cylinder pillar structures, a band gap opens when the ratio is equal or greater than 3. A tubular pillar design with a void room in it enhances acoustic multiple scattering and gives rise to the opening of the band gap. In order to verify it, a PC structure with double tubular pillars different in size (one within the other) is introduced and a more than 2times band gap enlargement is observed. Furthermore, the coupling between the resonant mode and the plate mode around the band gap is characterized, as well as the effect of the geometrical parameters on the band gap. The behavior of such structure could be utilized to design a pillar PC with stronger structural stability and to enlarge band gaps. Copyright © 2016 Elsevier B.V. All rights reserved.
A synthetic aperture microwave radiometer to measure soil moisture and ocean salinity from space
NASA Technical Reports Server (NTRS)
Le Vine, D. M.; Hilliard, L. M.; Swift, C. T.; Ruf, C. S.; Garrett, L. B.
1991-01-01
A concept is presented for a microwave radiometer in space to measure soil moisture and ocean salinity as part of an 'Earth Probe' mission. The measurements could be made using an array of stick antennas. The L-band channel (1.4 GHz) would be the primary channel for determining soil moisture, with the S-band (2.65-GHz) and C-band (5.0-GHz) channels providing ancillary information to help correct for the effects of the vegetation canopy and possibly to estimate a moisture profile. A preliminary study indicates that an orbit at 450 km would provide coverage of better than 95 percent of the earth every 3 days. A 10-km resolution cell (at nadir) requires stick antennas about 9.5-m long at L-band. The S-band and C-band sticks would be substantially shorter (5 m and 2.7 m, respectively).
NASA Astrophysics Data System (ADS)
Noll, S.; Kausch, W.; Kimeswenger, S.; Unterguggenberger, S.; Jones, A. M.
2015-11-01
Rotational temperatures Trot derived from lines of the same OH band are an important method to study the dynamics and long-term trends in the mesopause region near 87 km. To measure realistic temperatures, a corresponding Boltzmann distribution of the rotational level populations has to be achieved. However, this might not be fulfilled, especially at high emission altitudes. In order to quantify possible non-local thermodynamic equilibrium (non-LTE) contributions to the OH Trot as a function of the upper vibrational level v', we studied a sample of 343 echelle spectra taken with the X-shooter spectrograph at the Very Large Telescope at Cerro Paranal in Chile. These data allowed us to analyse 25 OH bands in each spectrum. Moreover, we could measure lines of O2b(0-1), which peaks at about 94 to 95 km, and O2a(0-0) with an emission peak at about 90 km. The latter altitude is reached in the second half of the night after a rise of several km because of the decay of a daytime population of excited O2. Since the radiative lifetimes for the upper levels of the two O2 bands are relatively long, the derived Trot are not significantly affected by non-LTE contributions. These bands are well suited for a comparison with OH if the differences in the emission profiles are corrected. For different sample averages, we made these corrections by using OH emission, O2a(0-0) emission, and CO2-based temperature profile data from the multi-channel radiometer SABER on the TIMED satellite. The procedure relies on differences of profile-weighted SABER temperatures. For an O2a(0-0)-based reference profile at 90 km, we found a good agreement of the O2 with the SABER-related temperatures, whereas the OH temperatures, especially for the high and even v', showed significant excesses with a maximum of more than 10 K for v' = 8. The exact value depends on the selected lines and molecular parameters. We could also find a nocturnal trend towards higher non-LTE effects, particularly for high v'. The amplitude of these variations can be about 2 K or less, which tends to be significantly smaller than the total amount of the non-LTE contributions. The found variations can be critical for dynamical studies based on Trot derived from OH bands with high v'.
Crock, J.G.; Lichte, F.E.; Wildeman, T.R.
1984-01-01
Demand is increasing for the determination of the rare-earth elements (REE) and yttrium in geologic materials. Due to their low natural abundance in many materials and the interferences that occur in many methods of determination, a separation procedure utilizing gradient strong-acid cation-exchange chromatography is often used to preconcentrate and isolate these elements from the host-rock matrix. Two separate gradient strong-acid cation-exchange procedures were characterized and the major elements as well as those elements thought to provide the greatest interference for the determination of the REE in geologic materials were tested for separation from the REE. Simultaneous inductively coupled argon plasma-atomic emission spectroscopy (ICAP-AES) measurements were used to construct the chromatograms for the elution studies, allowing the elution patterns of all the elements of interest to be determined in a single fraction of eluent. As a rock matrix, U.S. Geological Survey standard reference BCR-1 basalt was digested using both an acid decomposition procedure and a lithium metaborate fusion. Hydrochloric and nitric acids were tested as eluents and chromatograms were plotted using the ICAP-AES data; and we observed substantial differences in the elution patterns of the REE and as well as in the solution patterns of Ba, Ca, Fe and Sr. The nitric acid elution required substantially less eluent to elute the REE and Y as a group when compared to the hydrochloric acid elution, and provided a clearer separation of the REE from interfering and matrix elements. ?? 1984.
Luo, Haibin; Lee, Nacole; Wang, Xiangyang; Li, Yuling; Schmelzer, Albert; Hunter, Alan K; Pabst, Timothy; Wang, William K
2017-03-10
Turbid elution pools and high column back pressure are common during elution of monoclonal antibodies (mAbs) by acidic pH in Protein A chromatography. This phenomenon has been historically attributed to acid-induced precipitation of incorrectly folded or pH-sensitive mAbs and host cell proteins (HCPs). In this work, we propose a new mechanism that may account for some observations of elution turbidity in Protein A chromatography. We report several examples of turbidity and high column back pressure occurring transiently under a short course of neutral conditions during Protein A elution. A systematic study of three mAbs displaying this behavior revealed phase separation characterized by liquid drops under certain conditions including neutral pH, low ionic strength, and high protein concentration. These liquid droplets caused solution turbidity and exhibited extremely high viscosity, resulting in high column back pressure. We found out that the droplets were formed through liquid-liquid phase separation (LLPS) as a result of protein self-association. We also found multiple factors, including pH, temperature, ionic strength, and protein concentration can affect LLPS behaviors. Careful selection of process parameters during protein A elution, including temperature, flow rate, buffer, and salt can inhibit formation of a dense liquid phase, reducing both turbidity (by 90%) and column back pressure (below 20 pounds per square inch). These findings provide both mechanistic insight and practical mitigation strategies for Protein A chromatography induced LLPS. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.
Elution of monomer from different bulk fill dental composite resins.
Cebe, Mehmet Ata; Cebe, Fatma; Cengiz, Mehmet Fatih; Cetin, Ali Rıza; Arpag, Osman Fatih; Ozturk, Bora
2015-07-01
The purpose of this study was to evaluate the elution of Bis-GMA, TEGDMA, HEMA, and Bis-EMA monomers from six bulk fill composite resins over four different time periods, using HPLC. Six different composite resin materials were used in the present study: Tetric Evo Ceram Bulk Fill (Ivoclar Vivadent, Amherst, NY), X-tra Fill (VOCO, Cuxhaven, Germany), Sonic Fill (Kerr, Orange, CA, USA), Filtek Bulk Fill (3M ESPE Dental Product, St. Paul, MN), SDR (Dentsply, Konstanz, Germany), EQUIA (GC America INC, Alsip, IL). The samples (4mm thickness, 5mm diameter) were prepared and polymerized for 20s with a light emitted diode unit. After fabrication, each sample was immediately immersed in 75wt% ethanol/water solution used as extraction fluid and stored in the amber colored bottles at room temperature. Ethanol/water samples were taken (0.5mL) at predefined time intervals:10m (T1), 1h (T2), 24h (T3) and 30 days (T4). These samples were analyzed by HPLC. The obtained data were analyzed with one-way ANOVA and Tukey HSD at significance level of p<0.05. Amount of eluted Bis-EMA and Bis-GMA from Tetric Evo Ceram Bulk Fill and amount of eluted TEGDMA and HEMA from X-tra Fill higher than others composites (p<0.05). Residual monomers were eluted from bulk fill composite resins in all time periods and the amount of eluted monomers was increased with time. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Engineering a laser remote sensor for atmospheric pressure and temperature
NASA Technical Reports Server (NTRS)
Kalshoven, J. E., Jr.; Korb, C. L.
1978-01-01
A system for the remote sensing of atmospheric pressure and temperature is described. Resonant lines in the 7600 Angstrom oxygen A band region are used and an organic dye laser beam is tuned to measure line absorption changes with temperature or pressure. A reference beam outside this band is also transmitted for calibration. Using lidar techniques, profiling of these parameters with altitude can be accomplished.
Neutral gas and diffuse interstellar bands in the LMC
NASA Technical Reports Server (NTRS)
Danks, Anthony C.; Penprase, Brian
1994-01-01
Tracing the dynamics of the neutral gas and observing diffuse interstellar bands in the LMC (Large Magellanic Cloud) was the focus of this study. The S/N values, a Quartz lamp exposure, a T horium Argon Comparision lamp exposure, and spectral plots for each star observed were taken. The stars observed were selected to sample the 30 Dor vicinty. NaI absorption profiles are included.
Fitz, Brian D; Mannion, Brandyn C; To, Khang; Hoac, Trinh; Synovec, Robert E
2015-05-01
Low thermal mass gas chromatography (LTM-GC) was evaluated for rapid, high peak capacity separations with three injection methods: liquid, headspace solid phase micro-extraction (HS-SPME), and direct vapor. An Agilent LTM equipped with a short microbore capillary column was operated at a column heating rate of 250 °C/min to produce a 60s separation. Two sets of experiments were conducted in parallel to characterize the instrumental platform. First, the three injection methods were performed in conjunction with in-house built high-speed cryo-focusing injection (HSCFI) to cryogenically trap and re-inject the analytes onto the LTM-GC column in a narrower band. Next, the three injection methods were performed natively with LTM-GC. Using HSCFI, the peak capacity of a separation of 50 nl of a 73 component liquid test mixture was 270, which was 23% higher than without HSCFI. Similar peak capacity gains were obtained when using the HSCFI with HS-SPME (25%), and even greater with vapor injection (56%). For the 100 μl vapor sample injected without HSCFI, the preconcentration factor, defined as the ratio of the maximum concentration of the detected analyte peak relative to the analyte concentration injected with the syringe, was determined to be 11 for the earliest eluting peak (most volatile analyte). In contrast, the preconcentration factor for the earliest eluting peak using HSCFI was 103. Therefore, LTM-GC is demonstrated to natively provide in situ analyte trapping, although not to as great an extent as with HSCFI. We also report the use of LTM-GC applied with time-of-flight mass spectrometry (TOFMS) detection for rapid, high peak capacity separations from SPME sampled banana peel headspace. Copyright © 2015 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Bo, Zhang; Jinjiang, Zhang; Shuyu, Yan; Jiang, Liu; Jinhai, Zhang; Zhongpei, Zhang
2010-05-01
The phenomenon of Kink banding is well known throughout the engineering and geophysical sciences. Associated with layered structures compressed in a layer-parallel direction, it arises for example in stratified geological systems under tectonic compression. Our work documented it is also possible to develop super large-scale kink-bands in sedimentary sequences. We interpret the Bachu fold uplift belt of the central Tarim basin in western China to be composed of detachment folds flanked by megascopic-scale kink-bands. Those previous principal fold models for the Bachu uplift belt incorporated components of large-scale thrust faulting, such as the imbricate fault-related fold model and the high-angle, reverse-faulted detachment fold model. Based on our observations in the outcrops and on the two-dimension seismic profiles, we interpret that first-order structures in the region are kink-band style detachment folds to accommodate regional shortening, and thrust faulting can be a second-order deformation style occurring on the limb of the detachment folds or at the cores of some folds to accommodate the further strain of these folds. The belt mainly consists of detachment folds overlying a ductile decollement layer. The crests of the detachment folds are bounded by large-scale kink-bands, which are zones of angularly folded strata. These low-signal-tonoise, low-reflectivity zones observed on seismic profiles across the Bachu belt are poorly imaged sections, which resulted from steeply dipping bedding in the kink-bands. The substantial width (beyond 200m) of these low-reflectivity zones, their sub-parallel edges in cross section, and their orientations at a high angle to layering between 50 and 60 degrees, as well as their conjugate geometry, support a kink-band interpretation. The kink-band interpretation model is based on the Maximum Effective Moment Criteria for continuous deformation, rather than Mohr-Column Criteria for brittle fracture. Seismic modeling is done to identify the characteristics and natures of seismic waves within the kink-band and its fold structure, which supplies the further evidences for the kink-band interpretation in the region.
Carbon Dioxide Line Shapes for Atmospheric Remote Sensing
NASA Astrophysics Data System (ADS)
Predoi-Cross, Adriana; Ibrahim, Amr; Wismath, Alice; Teillet, Philippe M.; Devi, V. Malathy; Benner, D. Chris; Billinghurst, Brant
2010-02-01
We present a detailed spectroscopic study of carbon dioxide in support of atmospheric remote sensing. We have studied two weak absorption bands near the strong ν2 band that is used to derive atmospheric temperature profiles. We have analyzed our laboratory spectra recorded with the synchrotron and globar sources with spectral line profiles that reproduce the absorption features with high accuracy. The Q-branch transitions exhibited asymmetric line shape due to weak line-mixing. For these weak transitions, we have retrieved accurate experimental line strengths, self- and air-broadening, self- and air-induced shift coefficients and weak line mixing parameters. The experimental precision is sufficient to reveal inherent variations of the width and shift coefficients according to transition quantum numbers.
Use of FTA® classic cards for epigenetic analysis of sperm DNA.
Serra, Olga; Frazzi, Raffaele; Perotti, Alessio; Barusi, Lorenzo; Buschini, Annamaria
2018-02-01
FTA® technologies provide the most reliable method for DNA extraction. Although FTA technologies have been widely used for genetic analysis, there is no literature on their use for epigenetic analysis yet. We present for the first time, a simple method for quantitative methylation assessment based on sperm cells stored on Whatman FTA classic cards. Specifically, elution of seminal DNA from FTA classic cards was successfully tested with an elution buffer and an incubation step in a thermocycler. The eluted DNA was bisulfite converted, amplified by PCR, and a region of interest was pyrosequenced.
Gas chromatographic separation of fatty acid methyl esters on weakly polar capillary columns.
Yamamoto, Kouhei; Kinoshita, Akemi; Shibahara, Akira
2008-02-22
It was found that weakly polar columns, routinely used in capillary GC for analyzing sterols, food additives, etc., can also be used for separating fatty acid methyl esters (FAMEs). On these columns, FAMEs elute in the order of their unsaturation. The equivalent chain-length value of methyl 22:6 is below 23.00. This means FAMEs within a carbon chain length, having up to six double bonds, elute before the next (one carbon longer) saturated FAME elutes. Peak identification is easy. Weakly polar columns are compatible in both GC and GC/MS systems.
Investigations into Alternative Desorption Agents for Amidoxime-Based Polymeric Uranium Adsorbents
DOE Office of Scientific and Technical Information (OSTI.GOV)
Gill, Gary A.; Kuo, Li-Jung; Strivens, Jonathan E.
2015-06-01
Amidoxime-based polymeric braid adsorbents that can extract uranium (U) from seawater are being developed to provide a sustainable supply of fuel for nuclear reactors. A critical step in the development of the technology is to develop elution procedures to selectively remove U from the adsorbents and to do so in a manner that allows the adsorbent material to be reused. This study investigates use of high concentrations of bicarbonate along with targeted chelating agents as an alternative means to the mild acid elution procedures currently in use for selectively eluting uranium from amidoxime-based polymeric adsorbents.
Electrophoretic separation of proteins in space
NASA Technical Reports Server (NTRS)
Brown, R. K.
1976-01-01
Commercially available and synthetic wide range and short range ampholytes used in the isoelectric focusing of proteins was analyzed by ion exchange chromatography. A pH gradient over the pH range 3.8 to 11.0 was used to elute the ampholytes from a column of a sulfonated polystyrene resin. The wide range ampholytes were resolved into some 60 to 70 ninhydrin positive components. The recovery obtained with the method was quantitative. Acid short range ampholytes have approximately 35 components which elute readily from the ion exchange resin. Basic short range ampholytes gave about 50 components, most of which eluted at alkaline pH.
Release of TEGDMA from composite during the chewing situation.
Durner, J; Glasl, B; Zaspel, J; Kunzelmann, K H; Hickel, R; Reichl, F X
2010-07-01
The aim of this study was to investigate the triethylene glycol (TEGDMA) elution kinetics from light-cured composite with and without chewing simulation over a time period of 86 h. An experimental composite with TEGDMA labeled with a tracer dose of 14C-TEGDMA was used. The material parameters were in the range of commercially available composites. The mastification was simulated with the Fatigue-machine and the MUC-3 chewing simulator. 14C was eluted to 2.55% of the applied 14C-TEGDMA dose within 86 h after chewing simulation with the Fatigue-machine and to 2.60% after chewing simulation with the MUC-3. Similar 14C-kinetic data were found for 14C-elution with and without chewing simulation with the Fatigue-machine and with MUC-3. During the first 26 h after the beginning of the experiments a linear 14C-elution kinetic was observed, followed by a second linear 14C-elution kinetic with a lower slope up to 86 h in both apparatus. It could be shown that chewing simulation has no significant (p<0.05) effect on the release of 14C-TEGDMA (and/or 14C-degradation products) from polymerized composites. Copyright 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Desneux, Jérémy; Pourcher, Anne-Marie
2014-01-01
Four commercial DNA extraction kits and a minor modification in the DNA elution procedure were evaluated for the quantitation of bacteria in pig manure samples. The PowerSoil®, PowerFecal®, NucleoSpin® Soil kits and QIAamp® DNA Stool Mini kit were tested on raw manure samples and on lagoon effluents for their ability to quantify total bacteria and a subdominant bacteria specific of pig manure contamination: Lactobacillus amylovorus. The NucleoSpin® Soil kit (NS kit), and to a lesser extent the PowerFecal® kit were the most efficient methods. Regardless of the kit utilized, the modified elution procedure increased DNA yield in the lagoon effluent by a factor of 1.4 to 1.8. When tested on 10 piggery effluent samples, compared to the QIAamp kit, the NS kit combined with the modified elution step, increased by a factor up to 1.7 log10 the values of the concentration of L. amylovorus. Regardless of the type of manure, the best DNA quality and the highest concentrations of bacteria were obtained using the NS kit combined with the modification of the elution procedure. The method recommended here significantly improved quantitation of subdominant bacteria in manure. PMID:24838631
Dahling, Daniel R
2002-01-01
Large-scale virus studies of groundwater systems require practical and sensitive procedures for both sample processing and viral assay. Filter adsorption-elution procedures have traditionally been used to process large-volume water samples for viruses. In this study, five filter elution procedures using cartridge filters were evaluated for their effectiveness in processing samples. Of the five procedures tested, the third method, which incorporated two separate beef extract elutions (one being an overnight filter immersion in beef extract), recovered 95% of seeded poliovirus compared with recoveries of 36 to 70% for the other methods. For viral enumeration, an expanded roller bottle quantal assay was evaluated using seeded poliovirus. This cytopathic-based method was considerably more sensitive than the standard plaque assay method. The roller bottle system was more economical than the plaque assay for the evaluation of comparable samples. Using roller bottles required less time and manipulation than the plaque procedure and greatly facilitated the examination of large numbers of samples. The combination of the improved filter elution procedure and the roller bottle assay for viral analysis makes large-scale virus studies of groundwater systems practical. This procedure was subsequently field tested during a groundwater study in which large-volume samples (exceeding 800 L) were processed through the filters.
Hsu, Yung-Heng; Chen, Dave Wei-Chih; Tai, Chun-Der; Chou, Ying-Chao; Liu, Shih-Jung; Ueng, Steve Wen-Neng; Chan, Err-Cheng
2014-01-01
We developed biodegradable drug-eluting nanofiber-enveloped implants that provided sustained release of vancomycin and ceftazidime. To prepare the biodegradable nanofibrous membranes, poly(D,L)-lactide-co-glycolide and the antibiotics were first dissolved in 1,1,1,3,3,3-hexafluoro-2-propanol. They were electrospun into biodegradable drug-eluting membranes, which were then enveloped on the surface of stainless plates. An elution method and a high-performance liquid chromatography assay were employed to characterize the in vivo and in vitro release rates of the antibiotics from the nanofiber-enveloped plates. The results showed that the biodegradable nanofiber-enveloped plates released high concentrations of vancomycin and ceftazidime (well above the minimum inhibitory concentration) for more than 3 and 8 weeks in vitro and in vivo, respectively. A bacterial inhibition test was carried out to determine the relative activity of the released antibiotics. The bioactivity ranged from 25% to 100%. In addition, the serum creatinine level remained within the normal range, suggesting that the high vancomycin concentration did not affect renal function. By adopting the electrospinning technique, we will be able to manufacture biodegradable drug-eluting implants for the long-term drug delivery of different antibiotics. PMID:25246790
DOE Office of Scientific and Technical Information (OSTI.GOV)
Peter W. Carr; K.M. Fuller; D.R. Stoll
A new approach has been developed by modifying a conventional gradient elution liquid chromatograph for the high throughput screening of biological samples to detect the presence of regulated intoxicants. The goal of this work was to improve the speed of a gradient elution screening method over current approaches by optimizing the operational parameters of both the column and the instrument without compromising the reproducibility of the retention times, which are the basis for the identification. Most importantly, the novel instrument configuration substantially reduces the time needed to re-equilibrate the column between gradient runs, thereby reducing the total time for eachmore » analysis. The total analysis time for each gradient elution run is only 2.8 minutes, including 0.3 minutes for column reequilibration between analyses. Retention times standard calibration solutes are reproducible to better than 0.002 minutes in consecutive runs. A corrected retention index was adopted to account for day-to-day and column-to-column variations in retention time. The discriminating power and mean list length were calculated for a library of 47 intoxicants and compared with previous work from other laboratories to evaluate fast gradient elution HPLC as a screening tool.« less
NASA Astrophysics Data System (ADS)
Hilpert, Markus; Johnson, William P.
2018-01-01
We used a recently developed simple mathematical network model to upscale pore-scale colloid transport information determined under unfavorable attachment conditions. Classical log-linear and nonmonotonic retention profiles, both well-reported under favorable and unfavorable attachment conditions, respectively, emerged from our upscaling. The primary attribute of the network is colloid transfer between bulk pore fluid, the near-surface fluid domain (NSFD), and attachment (treated as irreversible). The network model accounts for colloid transfer to the NSFD of downgradient grains and for reentrainment to bulk pore fluid via diffusion or via expulsion at rear flow stagnation zones (RFSZs). The model describes colloid transport by a sequence of random trials in a one-dimensional (1-D) network of Happel cells, which contain a grain and a pore. Using combinatorial analysis that capitalizes on the binomial coefficient, we derived from the pore-scale information the theoretical residence time distribution of colloids in the network. The transition from log-linear to nonmonotonic retention profiles occurs when the conditions underlying classical filtration theory are not fulfilled, i.e., when an NSFD colloid population is maintained. Then, nonmonotonic retention profiles result potentially both for attached and NSFD colloids. The concentration maxima shift downgradient depending on specific parameter choice. The concentration maxima were also shown to shift downgradient temporally (with continued elution) under conditions where attachment is negligible, explaining experimentally observed downgradient transport of retained concentration maxima of adhesion-deficient bacteria. For the case of zero reentrainment, we develop closed-form, analytical expressions for the shape, and the maximum of the colloid retention profile.
Ground-Based Icing Condition Remote Sensing System Definition
NASA Technical Reports Server (NTRS)
Reehorst, Andrew L.; Koenig, George G.
2001-01-01
This report documents the NASA Glenn Research Center activities to assess and down select remote sensing technologies for the purpose of developing a system capable of measuring icing condition hazards aloft. The information generated by such a remote sensing system is intended for use by the entire aviation community, including flight crews. air traffic controllers. airline dispatchers, and aviation weather forecasters. The remote sensing system must be capable of remotely measuring temperature and liquid water content (LWC), and indicating the presence of super-cooled large droplets (SLD). Technologies examined include Profiling Microwave Radiometer, Dual-Band Radar, Multi-Band Radar, Ka-Band Radar. Polarized Ka-Band Radar, and Multiple Field of View (MFOV) Lidar. The assessment of these systems took place primarily during the Mt. Washington Icing Sensors Project (MWISP) in April 1999 and the Alliance Icing Research Study (AIRS) from November 1999 to February 2000. A discussion of the various sensing technologies is included. The result of the assessment is that no one sensing technology can satisfy all of the stated project goals. Therefore a proposed system includes radiometry and Ka-band radar. A multilevel approach is proposed to allow the future selection of the fielded system based upon required capability and available funding. The most basic level system would be the least capable and least expensive. The next level would increase capability and cost, and the highest level would be the most capable and most expensive to field. The Level 1 system would consist of a Profiling Microwave Radiometer. The Level 2 system would add a Ka-Band Radar. The Level 3 system would add polarization to the Ka-Band Radar. All levels of the system would utilize hardware that is already under development by the U.S. Government. However, to meet the needs of the aviation community, all levels of the system will require further development. In addition to the proposed system, it is also recommended that NASA continue to foster the development of Multi-Band Radar and airborne microwave radiometer technologies.
VizieR Online Data Catalog: Surface photometry of GHASP galaxies (Barbosa+, 2015)
NASA Astrophysics Data System (ADS)
Barbosa, C. E.; Mendes de Oliveira, C.; Amram, P.; Ferrari, F.; Russeil, D.; Epinat, B.; Perret, V.; Adami, C.; Marcelin, M.
2016-04-01
Our data set is constructed using new Rc-band observations taken at the Observatoire de Haute-Provence, supplemented with Sloan Digital Sky Survey archival data, obtained with the purpose of deriving homogeneous photometric profiles and parameters. Our results include Rc-band surface brightness profiles for 170 galaxies and ugriz profiles for 108 of these objects. We catalogue several parameters of general interest for further reference, such as total magnitude, effective radius and isophotal parameters (magnitude, position angle, ellipticity and inclination). We also perform a structural decomposition of the surface brightness profiles using a multi-component method to separate discs from bulges and bars, and to observe the main scaling relations involving luminosities, sizes and maximum velocities. We determine the Rc-band Tully-Fisher relation using maximum velocities derived solely from Hα rotation curves for a sample of 80 galaxies, resulting in a slope of -8.1+/-0.5, zero-point of -3.0+/-1.0 and an estimated intrinsic scatter of 0.28+/-0.07. We note that, unlike the Tully-Fisher relation in the near-infrared derived for the same sample, no change in the slope of the relation is seen at the low-mass end (for galaxies with Vmax<125km/s). We suggest that this different behaviour of the Tully-Fisher relation (with the optical relation being described by a single power law while the near-infrared has two), may be caused by differences in the stellar mass-to-light ratio for galaxies with Vmax<125km/s. (4 data files).
Gas chromatography-vacuum ultraviolet spectroscopy for analysis of fatty acid methyl esters.
Fan, Hui; Smuts, Jonathan; Bai, Ling; Walsh, Phillip; Armstrong, Daniel W; Schug, Kevin A
2016-03-01
A new vacuum ultraviolet (VUV) detector for gas chromatography was recently developed and applied to fatty acid methyl ester (FAME) analysis. VUV detection features full spectral acquisition in a wavelength range of 115-240nm, where virtually all chemical species absorb. VUV absorption spectra of 37 FAMEs, including saturated, monounsaturated, and polyunsaturated types were recorded. Unsaturated FAMEs show significantly different gas phase absorption profiles than saturated ones, and these classes can be easily distinguished with the VUV detector. Another advantage includes differentiating cis/trans-isomeric FAMEs (e.g. oleic acid methyl ester and linoleic acid methyl ester isomers) and the ability to use VUV data analysis software for deconvolution of co-eluting signals. As a universal detector, VUV also provides high specificity, sensitivity, and a fast data acquisition rate, making it a powerful tool for fatty acid screening when combined with gas chromatography. The fatty acid profile of several food oil samples (olive, canola, vegetable, corn, sunflower and peanut oils) were analyzed in this study to demonstrate applicability to real world samples. Copyright © 2015 Elsevier Ltd. All rights reserved.